WO2020133961A1 - Functional polyester production method and production system, and functional polyester fiber - Google Patents

Functional polyester production method and production system, and functional polyester fiber Download PDF

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Publication number
WO2020133961A1
WO2020133961A1 PCT/CN2019/092058 CN2019092058W WO2020133961A1 WO 2020133961 A1 WO2020133961 A1 WO 2020133961A1 CN 2019092058 W CN2019092058 W CN 2019092058W WO 2020133961 A1 WO2020133961 A1 WO 2020133961A1
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Prior art keywords
functional
polyester
functional powder
slurry
reactor
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PCT/CN2019/092058
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French (fr)
Chinese (zh)
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李鑫
邱志成
张厚羽
金剑
李志勇
刘玉来
王雪
马肖
刘建立
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中国纺织科学研究院有限公司
中纺院（天津）科技发展有限公司
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Publication of WO2020133961A1 publication Critical patent/WO2020133961A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/183—Terephthalic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/04—Pigments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters

Definitions

  • the invention belongs to the technical field of polymer material synthesis, and specifically relates to a production method and production system of functional polyester and functional polyester fiber.
  • the preparation method of the functional polyester fiber mainly adopts the masterbatch method.
  • the functional powder and the carrier resin are melted and mixed to obtain the functional masterbatch with high functional powder content, and then the functional masterbatch melt and the spinning polymer are used.
  • the ester melt is uniformly mixed to obtain functional polyester fibers through the spinning process.
  • the dispersion of the functional powder in the high-viscosity polyester melt mainly depends on the mechanical shear force provided by the mixing equipment, the functional powder is difficult to be uniform in the polyester melt Dispersed, the prepared functional polyester melt has poor spinning performance, and it is not easy to spin functional polyester fibers with fine denier or ultrafine denier.
  • the technical problem to be solved by the present invention is to overcome the shortcomings of the prior art, and to provide a production method and production system of functional polyester to realize the continuous and stable preparation of functional polyester with highly uniformly dispersed functional powder and improve the spinning of functional polyester Silk performance.
  • a functional polyester production system including a polyester main production system and a functional powder slurry concentrate preparation system.
  • the polyester main production system includes an esterification system, a pre-condensation system and a final polycondensation system connected in sequence.
  • the powder slurry concentrate preparation system includes an online addition device connected to the esterification system or/and between the esterification system and the pre-condensation system.
  • the functional powder slurry concentrate preparation system includes a slurry preparation unit, a slurry concentration unit and an online addition device connected in sequence, and the discharge port of the online addition device and the esterification system or/and The connection between the esterification system and the pre-condensation system.
  • the functional powder slurry preparation unit includes a carrier preparation unit, a functional powder dispersion preparation unit, and a mixing unit.
  • the carrier preparation unit is connected to the functional powder dispersion preparation unit via a metering and conveying device.
  • the functional powder is connected to the mixing unit via a metering and conveying device.
  • Mixing units include but are not limited to shear pumps, screw extruders, grinders, planetary gear dynamic mixers, dynamic and static ring gear type dynamic mixers or ball and socket type dynamic mixers.
  • the slurry concentration unit has a reaction kettle with a flashing function, and no stirring structure is provided.
  • the functional powder slurry enters the reaction kettle with flashing function, on the one hand, under negative pressure conditions, the water or excess alcohol present in the functional powder slurry will be flashed off to prepare a low pressure with highly uniformly dispersed functional powder Filter value of functional powder slurry concentrate.
  • the flashing of water or excess alcohol in the functional powder slurry will cause the material to boil violently and replace the mechanical stirrer to achieve the stirring effect. Therefore, it can improve the operation reliability of the reactor and facilitate The cleaning of the reactor reduces the energy consumption of the reactor.
  • the online addition device includes a metering delivery device and/or a mixing device
  • the metering delivery device includes a delivery pump and a flow meter or a delivery pump with a metering function
  • the mixing device includes a static mixer or/and dynamic mixing Device.
  • Static mixers include but are not limited to SMX type mixers, SMXL type mixers, SMV type mixers; dynamic mixers include but not limited to shear pumps, screw extruders, planetary gear dynamic mixers, dynamic and static ring gear type dynamic mixing , Ball and socket dynamic mixer.
  • the polyester main production system further includes a liquid-phase tackifying reaction kettle, the outlet of the final polycondensation system is connected to the inlet of the liquid-phase tackifying reaction kettle, and the outlet of the liquid-phase tackifying reaction kettle is Spinning equipment connection.
  • the esterification system, the pre-condensation system and the final polycondensation system of the polyester main production system are connected via an online addition device, and more preferably, the polyester main production system includes an esterification reaction kettle or Esterification alcoholysis reactor, pre-condensation reactor, final polycondensation reactor and liquid-phase thickening reactor.
  • One or more esterification reactors, esterification alcoholysis reactors, pre-condensation reactors, final polycondensation reactors and liquid-phase viscosity-increasing reactors in the polyester main production system can be provided.
  • Another object of the present invention is to provide a method for producing functional polyester, including the following steps:
  • the functional powder dispersion is prepared by the following method: the functional powder and water and/or glycol are used as raw materials to configure the functional powder dispersion.
  • Glycols include but are not limited to ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, methyl propylene glycol, neopentyl glycol, diethylene glycol or triethylene glycol.
  • the functional powder is a powder having functions of coloring, antibacterial, radiation protection, antibacterial, conductive, thermal conductivity, far infrared, flame retardant, negative ion, fluorescent or magnetic;
  • the carrier is selected from Polyester polyol, polyether or polyester oligomer.
  • the functional powder can be selected from one or more of the following substances: carbon black, pigment brown 3, pigment blue 5, pigment blue 15, pigment blue 15:1, pigment blue 15:3, pigment blue 15:4, pigment Blue 15:6, Pigment Blue 16, Pigment Blue 28, Pigment Blue 29, Pigment Blue 60, Pigment Violet 19, Pigment Violet 23, Pigment Violet 29, Pigment Red 101, Pigment Red 102, Pigment Red 108, Pigment Red 112, Pigment Red 122, Pigment Red 146, Pigment Red 149, Pigment Red 170, Pigment Red 171, Pigment Red 172, Pigment Red 175, Pigment Red 176, Pigment Red 177, Pigment Red 178, Pigment Red 179, Pigment Red 185, Pigment Red 202 , Pigment Red 207, Pigment Red 208, Pigment Red 214, Pigment Red 241, Pigment Red 242, Pigment Red 254, Pigment Red 255, Pigment Red 263, Pigment Red 264, Pigment Red 272, Pigment Yellow 6, Pigment Yellow 13, Pigment Yellow 14, Pigment Yellow 17, Pigment Yellow 21, Pigment Yellow 37
  • the average particle diameter of the functional powder in the functional powder slurry is controlled to be not higher than 1000 nm, preferably not higher than 500 nm, and more preferably not higher than 300 nm;
  • the average particle diameter of the functional powder in the functional powder slurry is controlled within the above range, which can ensure that the functional powder is highly uniformly dispersed in the subsequent preparation of the functional powder slurry concentrate, so that the functional powder slurry concentrate has Low pressure filter value.
  • the content of the functional powder in the functional powder slurry concentrate is 3% to 95%, preferably 5% to 60%, and more preferably 10% to 50%;
  • a functional powder concentrate in which the functional powder is highly uniformly dispersed can be prepared.
  • the hydroxyl value of the functional powder slurry concentrate is not higher than 175 mgKOH/g, and the filter press value DFMS is not higher than 30 kPa ⁇ cm 2 /g.
  • the hydroxyl value of the functional powder concentrate is controlled within the above range.
  • the amount of by-product diol generated during the polycondensation reaction is small, to avoid stable production operation due to the significant increase in the amount of diol evaporation when injected into the polyester production system. Sexual decline.
  • the pressure filtration value of the functional powder slurry concentrate is controlled within the above range.
  • the functional powder When the functional powder slurry concentrate is introduced into the polyester production system, the functional powder has better dispersibility, so that the functional powder Highly evenly dispersed in the ester.
  • raw materials for preparing polyester oligomers include terephthalic acid slurry, copolymer modified monomer slurry or polyester waste.
  • the terephthalic acid slurry is composed of glycol and Terephthalic acid is prepared according to a molar ratio of 1.05 to 2.0.
  • Copolymer modified monomer slurry is prepared from copolymer modified monomer and/or glycol as raw materials.
  • the polyester waste is waste from polyester bottles and production. Materials, polyester film waste and production scrap, polyester textile waste and production scrap and/or polyester fiber production scrap.
  • terephthalic acid has good slurryability
  • the terephthalic acid slurry in the range of the molar ratio of alkyd acid is input into the esterification system
  • the air lift of the esterification system is in a suitable range, which is conducive to the smooth progress of the esterification reaction, and the small condensate return flow of ethylene glycol during the esterification reaction is conducive to saving the reaction energy consumption.
  • Co-modified monomers include but are not limited to the following substances: isophthalic acid, adipic acid, neopentyl glycol, diethylene glycol, polyethylene glycol, sorbitol, polyamide, polyethylene adipate, Diethylene glycol isophthalate-5-sulfonate sodium, diethylene glycol isophthalate-5-sulfonate lithium, diethylene glycol isophthalate-5-sulfonate potassium, 2- Diethylene glycol carboxyethylphenyl hypophosphite, [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)methyl]butanedi Diethylene glycol acid, dipropylene isophthalate-5-sulfonate sodium, dipropylene isophthalate-5-sulfonate lithium, dipropylene isophthalate-5-sulfonate potassium, 2 -Dipropylene glycol carboxyethylphenyl hypo
  • copolymer modified monomer slurry can endow functional powder modified polyester cationic dye dyeing, disperse dye atmospheric dyeing, antibacterial, hydrophilic, low melting point, high shrinkage, cotton imitation and other composite functions.
  • the nature of the body, the copolymer modified monomer slurry can be added in different reaction stages of the esterification system.
  • the intrinsic viscosity of the functional polyester prepolymer is 0.1 to 0.5 dL/g
  • the intrinsic viscosity of the functional polyester is 0.5 to 1.2 dL/g
  • the filter press value DFFP is not higher than 0.8 kPa ⁇ cm 2 /g.
  • the functional powder can be highly uniformly dispersed in the polyester matrix.
  • the prepared functional polyester is suitable for preparing high-quality films and fibers.
  • the reaction temperature of the esterification system is 230-280°C
  • the reaction temperature of the pre-condensation system is 230-290°C
  • the reaction temperature of the final polycondensation system is 240-300°C.
  • Still another object of the present invention is to provide a functional polyester fiber obtained from the functional polyester production system described in any one of the foregoing, and the function obtained by the functional polyester production method described in any one of the above Made of polyester.
  • the functional polyester fibers include one or more of functional polyester fibers in the colors of undiluted solution, antibacterial, anti-radiation, antistatic, fluorescent, far infrared, thermally conductive, or negative ions.
  • the functional polyester molecule is polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate; more preferably, the functional polyester molecule has a cationic dye Dyeable, hydrophilic, cotton-like, flame retardant, low melting point or high shrinkage copolyester.
  • the present invention has the following beneficial effects compared with the prior art:
  • the invention introduces a functional powder slurry concentrate preparation system into the main polyester production system, which can continuously prepare functional powder slurry concentrates with low hydroxyl value and low pressure filtration value, and concentrate the prepared functional powder slurry concentrate After the material and polyester oligomer are mixed uniformly, the polycondensation reaction is carried out to obtain the functional polyester with highly uniformly dispersed functional powder, which is conducive to improving the spinning performance of the functional polyester and is suitable for the production of high-quality fibers and films.
  • the production method of functional polyester according to the present invention is easy to implement industrially, can realize large-scale industrialization of functional polyester and continuously produce functional polyester with highly uniformly dispersed functional powder, improve the spinning performance of functional polyester, and improve the functional polymerization Ester production efficiency and cost reduction.
  • 1 is a schematic process flow diagram of the production method of functional polyester according to the present invention.
  • FIG. 2 is a schematic structural diagram of a functional polyester production system according to the present invention.
  • FIG. 3 is a schematic diagram of a second structure of the functional polyester production system according to the present invention.
  • FIG. 4 is a schematic diagram of a third structure of the functional polyester production system according to the present invention.
  • FIG. 5 is a fourth structural schematic diagram of the functional polyester production system according to the present invention.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 265°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
  • the raw material slurry prepared by mixing terephthalic acid and ethylene glycol into a carrier with an alkyd molar ratio of 1.3 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 293.7 kg/h, with a concentration of 3 wt
  • the flow rate of the% catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 2.9 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 255 kg/h through a carrier metering and conveying unit composed of a conveying pump and a flow meter.
  • the pigment blue 15:3 concentration of 40wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered at a flow rate of 244.6kg/h to a functional powder dispersion preparation unit made up of 3 grinders in series,
  • the pigment powder 15:3 prepared by grinding and the functional powder dispersion with an average particle size of 143nm enters the functional powder dispersion supply tank, and is transported to a measuring unit of 244.6kg through the functional powder dispersion composed of a delivery pump and a flow meter
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a pigment blue 15:3 functional powder slurry with an average particle size of 154 nm, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 499.6 kg/h.
  • the temperature of the evaporation unit is 275°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 326.1 kg/h Extracted from the feed concentration unit, the content of the pigment blue 15:3 in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 6.1 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit
  • the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the stock solution whose base is polyethylene terephthalate is colored blue.
  • the monofilament fineness of this dope-colored blue polyester fiber was 0.77 dtex, the breaking strength was 3.4 cN/dtex, and the elongation at break was 33%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 265°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 375 kg/h, concentration
  • the flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.2 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 326.2 kg/h by the carrier metering and conveying unit composed of a conveying pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20% by weight is continuously and uniformly delivered at a flow rate of 625 kg/h to a functional powder dispersion preparation unit formed by three grinding machines connected in series, and prepared by grinding
  • the functional powder dispersion with an average particle size of carbon black of 96nm enters the functional powder dispersion supply tank, and is continuously and stably transferred from the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter at a flow rate of 625kg/h Produced in the functional powder dispersion tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 110 nm, and then the functional powder slurry
  • the flow rate of 951.2kg/h is continuously and uniformly transported to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 416.7 kg/h Extracted from the feed concentration unit, the content of carbon black in the functional powder slurry concentrate is 30 wt%, and the pressure filtration value DFMS is 2.3 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit
  • the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw material colored polyethylene terephthalate base black colored polymer is prepared.
  • the monofilament fineness of this dope-colored black polyester fiber was 0.77 dtex, the breaking strength was 3.6 cN/dtex, and the breaking elongation was 32%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 265°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
  • the acid value of the carrier reaches 25 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 342.3 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with an antibacterial agent cuprous oxide concentration of 15% by weight is continuously and uniformly delivered at a flow rate of 494.5 kg/h to a functional powder dispersion preparation unit formed by three grinding machines connected in series,
  • the functional powder dispersion liquid with an average particle size of 84 nm of the antibacterial agent cuprous oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 494.5 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an antibacterial agent cuprous oxide functional particle size of 92nm, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 836.8 kg/h.
  • the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 371 kg/h.
  • the content of the antibacterial agent cuprous oxide in the functional powder slurry concentrate is 20 wt%
  • the filter press value DFMS is 4.8 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 280°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antibacterial polyester fiber with a polyethylene terephthalate matrix is obtained Among them, the press filter value DFFP of the functional polyester is 0.12 kPa ⁇ cm 2 /g.
  • the antibacterial polyester fiber has a monofilament fineness of 1.16 dtex, a breaking strength of 4.2 cN/dtex, and an elongation at break of 33%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and butylene glycol with an alkyd molar ratio of 1.12 is continuously and uniformly conveyed to the vertical type by the flow rate of 4546kg/h.
  • An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 240°C.
  • the catalyst tetrabutyl titanate solution with a concentration of 20 wt% was continuously and uniformly injected into the vertical esterification reactor at a flow rate of 53.6 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and a oligomer flow meter continuously and stably withdraws from the esterification reactor at a flow rate of 3949 kg/h.
  • the terephthalic acid and butylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 1.1.
  • the raw material carrier of the carrier is continuously and uniformly delivered to the carrier preparation unit composed of the carrier preparation reactor at a flow rate of 144.1 kg/h, the concentration is
  • the flow rate of the 20 wt% catalyst tetrabutyl titanate solution injected into the carrier preparation reactor was 1.6 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C.
  • the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 126.9 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the butadiene glycol-based functional powder pre-dispersion with a thermal conductivity aluminum nitride concentration of 60wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 187.5kg/h.
  • the functional powder dispersion liquid with an average particle size of 147 nm of the thermally conductive aluminum nitride prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 187.5 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit and are mixed uniformly to obtain a functional powder slurry with an average particle size of 163 nm as the thermal conductive agent aluminum nitride, and then the function
  • the powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 314.4 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h
  • the content of the thermal conductive agent aluminum nitride in the functional powder slurry concentrate is 50 wt%
  • the filter press value DFMS is 8.4 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 250°C.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 260°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to obtain a thermally conductive polyester fiber with a matrix of polybutylene terephthalate Among them, the press filter value DFFP of the functional polyester is 0.28 kPa ⁇ cm 2 /g.
  • the monofilament fineness of this thermally conductive fiber was 1.54 dtex, the breaking strength was 3.3 cN/dtex, and the elongation at break was 30%.
  • the terephthalic acid and propylene glycol are formulated into a polyester oligomer slurry with an alkyd molar ratio of 1.4.
  • the raw material slurry of the polyester oligomer is continuously and uniformly delivered to the vertical first ester at a flow rate of 4958 kg/h.
  • the esterification reaction system composed of a chemical reaction kettle and a horizontal second esterification reaction kettle performs an esterification reaction.
  • the reaction temperature of the first esterification reaction kettle is 235°C
  • the reaction temperature of the second esterification reaction kettle is 240°C.
  • the catalyst tetraisopropyl titanate solution with a concentration of 10 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 18.8 kg/h.
  • the acid value of the polyester oligomer reaches 10 mgKOH/g
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4326 kg/h Out.
  • the terephthalic acid and propylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 2.0.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 667.8 kg/h, with a concentration of 10 wt%
  • the flow rate of the catalyst tetraisopropyl titanate solution into the carrier preparation reactor was 2.2 kg/h, and the reaction temperature of the carrier preparation reactor was 230°C.
  • the acid value of the carrier reaches 7 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 595.2 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
  • Propylene glycol-based functional powder pre-dispersion with a concentration of 10wt% of fluorescent agent yellow-green luminous powder (ZnS:Cu) was continuously and uniformly delivered to a functional powder dispersion composed of 1 grinder at a flow rate of 478.8kg/h Unit, the fluorescent powder yellow-green luminous powder (ZnS:Cu) prepared by grinding and the functional powder dispersion with an average particle size of 460nm enters the functional powder dispersion supply tank, through the functional powder composed of the supply pump and the flow meter The slurry conveying and metering unit continuously and stably withdraws from the functional powder dispersion liquid supply tank at a flow rate of 478.8 kg/h.
  • the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit, and the phosphor yellow-green luminous powder (ZnS:Cu) with an average particle size of 500 nm is obtained after mixing uniformly The slurry, and then the functional powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1074 kg/h.
  • the temperature of the evaporation unit is 245°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 478.8 kg/h
  • the content of the yellow-green luminous powder (ZnS:Cu) in the functional powder slurry concentrate is 10 wt%
  • the filter press value DFMS is 19.8 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 255°C. When the intrinsic viscosity of the prepolymer reaches 0.5dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 260°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the fluorescent polyester fiber with the matrix of polytrimethylene terephthalate is prepared.
  • the filter press value DFFP of the functional polyester is 0.66 kPa ⁇ cm 2 /g.
  • This fluorescent polyester fiber has a monofilament fineness of 3.47 dtex, a breaking strength of 2.8 cN/dtex, and an elongation at break of 27%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 2.0 is continuously and uniformly conveyed to the vertical type at a rate of 5667kg/h.
  • An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 255°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter is continuously and stably extracted from the esterification reactor at a flow rate of 5021 kg/h.
  • the terephthalic acid and ethylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 2.0.
  • the raw material slurry of the carrier is continuously and uniformly delivered to the carrier preparation unit composed of the carrier preparation reactor at a flow rate of 617.7 kg/h, the concentration is
  • the flow rate of the 3 wt% catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 5.9 kg/h
  • the reaction temperature of the carrier preparation reactor was 250°C.
  • the carrier delivery metering unit composed of a delivery pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 548.5 kg/h.
  • the ethylene glycol-based functional powder pre-dispersion with a far-infrared agent zirconium carbide concentration of 20 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by two grinding machines in series at a flow rate of 511.4 kg/h.
  • the far-infrared agent zirconium carbide prepared by grinding the functional powder dispersion with an average particle size of 112nm enters the functional powder dispersion supply tank, and the functional powder dispersion consisting of a delivery pump and a flow meter is transported to a metering unit of 511.4kg
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit and are mixed uniformly to obtain a far-infrared agent zirconium carbide functional powder slurry with an average particle size of 129 nm, and then the function
  • the powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1059.9 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 511.4 kg/h.
  • the content of the far-infrared agent zirconium carbide in the functional powder slurry concentrate is 20 wt%
  • the filter press value DFMS is 5.4 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the reactant temperature of the pre-condensation reactor is 290°C. When the intrinsic viscosity of the prepolymer reaches 0.30dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 285°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the far-infrared polyester whose base is polyethylene terephthalate is prepared.
  • This far infrared polyester fiber has a monofilament fineness of 2.31 dtex, a breaking strength of 3.2 cN/dtex, and an elongation at break of 31%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.05 is continuously and uniformly conveyed to the vertical type by the flow rate of 4516 kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 270°C
  • the reaction temperature of the second esterification reactor is 280°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3841 kg/h. Out.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 1004.6 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 11.3 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 875.3 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with an anti-ultraviolet radiation agent zinc oxide concentration of 10 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by two grinding machines in series at a flow rate of 411.5 kg/h
  • the functional powder dispersion liquid with an average particle size of 340 nm of zinc oxide, an anti-ultraviolet radiation agent prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to the metering unit by the functional powder dispersion liquid composed of a delivery pump and a flow meter.
  • the flow rate of 411.5kg/h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 362 nm of the anti-UV radiation agent zinc oxide, and then the functional powder
  • the bulk slurry is continuously and uniformly delivered to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1286.8 kg/h.
  • the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 823 kg/h
  • the content of the functional powder slurry concentrate, which was extracted from the concentration unit, was 5 wt% of the anti-ultraviolet radiation agent zinc oxide, and the filter press value DFMS was 10.2 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 275°C and the reactant temperature of the second precondensation reaction kettle is 280°C.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 285°C.
  • Polyester fiber where the functional polyester has a filter value DFFP of 0.25 kPa ⁇ cm 2 /g.
  • the monofilament fineness of this radiation-proof polyester fiber was 2.31 dtex, the breaking strength was 3.0 cN/dtex, and the elongation at break was 31%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.05 is continuously and uniformly conveyed to the vertical type by the flow rate of 4516 kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 270°C
  • the reaction temperature of the second esterification reactor is 280°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3848 kg/h. Out.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 731.8 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 7.7 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C.
  • the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 643.2 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a concentration of tin oxide and antimony oxide of 20 wt% is continuously and uniformly delivered to the functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 661.8 kg/h.
  • the functional powder dispersion liquid with an average particle diameter of 68 nm of the conductive agent tin antimony oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and the functional powder dispersion liquid composed of a delivery pump and a flow meter is transported to a metering unit of 661.8 kg
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 80 nm of the anti-UV radiation agent zinc oxide, and then the functional powder
  • the bulk slurry is continuously and uniformly delivered to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1305 kg/h.
  • the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 661.8 kg/h. It was collected in the material concentration unit, and the content of the conductive agent tin antimony oxide in the functional powder slurry concentrate was 20 wt%, and the filter press value DFMS was 2.2 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 280°C and the reactant temperature of the second precondensation reaction kettle is 285°C.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 300°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antistatic polyester whose base is polyethylene terephthalate is obtained.
  • the press-filtration value DFFP of the functional polyester is 0.07 kPa ⁇ cm 2 /g.
  • the antistatic polyester fiber had a monofilament fineness of 1.16 dtex, a breaking strength of 6.2 cN/dtex, and an elongation at break of 28%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and butylene glycol with an alkyd molar ratio of 1.12 is continuously and uniformly conveyed to the vertical type by the flow rate of 4546kg/h.
  • An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 240°C.
  • the catalyst tetrabutyl titanate solution with a concentration of 20 wt% was continuously and uniformly injected into the vertical esterification reactor at a flow rate of 53.6 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and a oligomer flow meter continuously and stably withdraws from the esterification reactor at a flow rate of 3949 kg/h.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 233.5 kg/h.
  • the flow rate of the catalyst tetrabutyl titanate solution with a concentration of 20 wt% injected into the carrier preparation reactor was 2.7 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C.
  • the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reaction kettle at a flow rate of 206.1 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the butanediol-based functional powder pre-dispersion with a concentration of 30% by weight of anion generator tourmaline is continuously and uniformly delivered to the functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 267.9 kg/h.
  • the functional powder dispersion liquid with an average particle size of 189 nm, which is an anion generator tourmaline prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 267.9 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit and are uniformly mixed to obtain a functional powder slurry with an average particle size of 194 nm, an anion generator tourmaline, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 474 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 267.9 kg/h
  • the content of the negative ion generator tourmaline in the functional powder slurry concentrate is 30 wt% and the filter press value DFMS is 15.5 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 250°C.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 250°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the negative ion polyester fiber whose base is polybutylene terephthalate is prepared.
  • the press filter value DFFP of the functional polyester is 0.51 kPa ⁇ cm 2 /g.
  • the monofilament fineness of this negative ion fiber was 2.31 dtex, the breaking strength was 3.1 cN/dtex, and the breaking elongation was 26%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and low melting point copolymer modified monomer isophthalic acid slurry, wherein the terephthalic acid slurry is composed of p-benzene
  • the dicarboxylic acid and ethylene glycol are formulated with an alkyd molar ratio of 1.12, and the low melting point copolymer modified monomer isophthalic acid slurry is prepared from isophthalic acid and ethylene glycol with an alkyd molar ratio of 1.12.
  • the terephthalic acid slurry with a flow rate of 2760kg/h and the low melting point copolymer modified monomer isophthalic acid slurry with a flow rate of 1841kg/h are continuously and uniformly delivered to the vertical first esterification reactor and the vertical
  • the esterification reaction system of the esterification reaction system composed of the second esterification reaction kettle performs an esterification reaction in the vertical first esterification reaction kettle.
  • the reaction temperature of the first esterification reaction kettle is 260°C
  • the reaction temperature of the second esterification reaction kettle is 265°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer delivery and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3919 kg/h Out.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 119.3 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 1.1 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 106 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a pigment red 254 concentration of 60% by weight is continuously and uniformly delivered at a flow rate of 197.4 kg/h to a functional powder dispersion preparation unit composed of two grinding machines connected in series, after grinding
  • the prepared functional powder dispersion with an average particle size of 294 nm in Pigment Red 254 enters the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 197.4 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with a pigment red 254 average particle size of 300 nm, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 303.4 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 197.4 kg/h
  • the content of pigment red 254 in the functional powder slurry concentrate is 60 wt%
  • the filter press value DFMS is 9.3 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, where the reactant temperature of the first precondensation reaction kettle is 265°C and the reactant temperature of the second precondensation reaction kettle is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw liquid colored low-melting polyester fiber whose matrix is a low-melting point copolyester is prepared.
  • the press filter value DFFP of the functional polyester is 0.23 kPa ⁇ cm 2 /g.
  • the stock solution colored red low-melting polyester fiber monofilament fineness was 1.54 dtex, breaking strength was 2.8 cN/dtex, and breaking elongation was 36%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and high shrink copolymerization modified monomer neopentyl glycol slurry, wherein the terephthalic acid slurry is composed of p-benzene
  • the dicarboxylic acid and ethylene glycol are formulated with an alkyd molar ratio of 1.05, and the high shrinkage copolymer modified monomer neopentyl glycol slurry is formulated with neopentyl glycol and ethylene glycol at a weight ratio of 8:2.
  • the terephthalic acid slurry with a flow rate of 4516kg/h and the high shrinkage copolymerization modified monomer neopentyl glycol slurry with a flow rate of 152.5kg/h are continuously and uniformly delivered to the vertical first esterification reactor and the vertical
  • the esterification reaction system of the esterification reaction system composed of the second esterification reaction kettle performs esterification reaction in the vertical first esterification reaction kettle, the reaction temperature of the first esterification reaction kettle is 260°C, and the reaction temperature of the second esterification reaction kettle is 265°C .
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the acid value of the polyester oligomer reaches 15mgKOH/g
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3987kg/h Out.
  • the pigment blue 15:3 concentration 40wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered at a flow rate of 239.4kg/h to a functional powder dispersion preparation unit made up of 3 grinders in series, After preparation, the functional powder dispersion liquid with pigment blue 15:3 with an average particle size of 143 nm is fed into the functional powder dispersion liquid supply tank, and the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter is 239.4 kg/ The flow rate of h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a pigment blue 15:3 functional powder slurry with an average particle size of 154 nm, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 404.9 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h Extracted from the feed concentration unit, the content of the pigment blue 15:3 in the functional powder slurry concentrate is 40 wt%, and the filter press value DFMS is 7.8 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, where the reactant temperature of the first precondensation reaction kettle is 265°C and the reactant temperature of the second precondensation reaction kettle is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw liquid colored blue high-shrink polyester with the matrix of high-shrink copolyester is obtained
  • the stock solution colored blue high shrinkage polyester fiber monofilament fineness was 1.16 dtex, the breaking strength was 3.6 cN/dtex, and the breaking elongation was 34%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and cationic dye-dyeable copolymerizable modified monomer diethylene glycol isophthalate-5-sulfonate sodium slurry
  • the composition is composed of terephthalic acid slurry made from terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.15.
  • the cationic dye can be dyed and copolymerized to modify the monomer diethylene glycol isophthalate-5-
  • the sodium sulfonate slurry is prepared from diethylene glycol isophthalate-5-sodium sulfonate and ethylene glycol at a weight ratio of 4:6.
  • the esterification reaction system is composed of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor.
  • the terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4637kg/h
  • Chemical reactor cationic dye-dyeable copolymerized modified monomer diethylene glycol isophthalate-5-sulfonate sodium slurry was continuously and uniformly injected into the bedroom horizontal second esterification reactor at a flow rate of 260.7 kg/h
  • the second chamber and the catalyst ethylene glycol antimony solution with a concentration of 3% by weight are continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 54.8 kg/h.
  • the ethylene glycol-based functional powder pre-dispersion with a matting agent titanium dioxide concentration of 40% by weight is continuously and uniformly delivered at a flow rate of 312.5 kg/h to a functional powder dispersion preparation unit composed of three grinding machines connected in series, after grinding
  • the prepared functional powder dispersion with an average particle size of 62 nm of the matting agent titanium dioxide enters the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 312.5 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 68 nm of the matting agent titanium dioxide, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 639.2 kg/h.
  • the temperature of the evaporation unit is 280°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder at a flow rate of 416.7 kg/h
  • the bulk slurry concentration unit extracts directly to the third chamber of the horizontal second esterification reactor, the content of the matting agent titanium dioxide in the functional powder slurry concentrate is 30wt%, and the filter press value DFMS is 1.2kPa ⁇ cm 2 /g.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 250°C.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the fully extinct cationic dyeable dyeable copolyester whose matrix is the cationic dyeable dyeable is prepared.
  • Polyester fiber wherein the functional polyester has a filter value DFFP of 0.04 kPa ⁇ cm 2 /g.
  • the total extinction cationic dyeable polyester fiber monofilament fineness is 1.16 dtex, breaking strength is 3.3 cN/dtex, and breaking elongation is 35%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and disperse dye at atmospheric pressure copolymerizable modified monomer diethylene glycol adipate slurry, of which Phthalic acid slurry is prepared from terephthalic acid and ethylene glycol at an alkyd molar ratio of 1.08. Disperse dyes can be dyed at atmospheric pressure. Copolymerized modified monomer diethylene glycol adipate slurry is made from diethyl adipate Glycol ester and ethylene glycol are formulated at a weight ratio of 6:4.
  • the esterification reaction system consists of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor.
  • the terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4098kg/h Chemical reactor, disperse dyes, atmospheric pressure dyeable copolymerization modified monomer diethylene glycol adipate slurry was continuously and uniformly injected into the second chamber of the bedroom horizontal second esterification reactor at a flow rate of 761.5 kg/h,
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 54.8 kg/h.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 250°C.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 450.6 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 5.1 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 392.6 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the anti-ultraviolet radiation agent-doped aluminum oxide-based zinc oxide functional powder pre-dispersion with a concentration of 15wt% was continuously and uniformly delivered to the functional powder dispersion formed by 4 grinding machines in series at a flow rate of 412.5kg/h
  • the functional powder dispersion liquid with an average particle diameter of 82 nm of the aluminum oxide-doped zinc oxide prepared by grinding and entering the functional powder dispersion liquid supply tank passes through the functional powder dispersion liquid composed of a delivery pump and a flowmeter
  • the conveying and metering unit continuously and stably withdraws from the functional powder dispersion liquid supply tank at a flow rate of 412.5 kg/h.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an anti-ultraviolet radiation agent aluminum-doped zinc oxide average particle size of 94 nm, and then the functional powder slurry
  • the functional powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 805.1 kg/h.
  • the temperature of the evaporation unit is 275°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 412.5 kg/h
  • the content of the anti-ultraviolet radiation agent aluminum-doped zinc oxide in the functional powder slurry concentrate is 15 wt%
  • the filter press value DFMS is 2.9 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the anti-ultraviolet radiation dispersion of the matrix of the disperse dye at atmospheric pressure and co-polyester can be obtained
  • Dyestuff can be dyed with polyester at normal pressure.
  • the functional polyester has a filter value of DFFP of 0.10 kPa ⁇ cm 2 /g.
  • the anti-ultraviolet radiation disperse dye normal pressure dyeable polyester fiber monofilament fineness is 1.16 dtex, breaking strength is 3.6 cN/dtex, and breaking elongation is 32%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and cotton-like copolymerized modified monomer polyamide slurry, in which terephthalic acid slurry is composed of terephthalic acid It is blended with ethylene glycol at an alkyd molar ratio of 1.12, and the cotton-like copolymerized modified monomer polyamide slurry is prepared by melt blending polyamide at 230°C.
  • the esterification reaction system consists of a vertical first esterification reactor and a vertical second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first esterification reactor at a flow rate of 4141 kg/h.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the vertical second esterification kettle at a flow rate of 54.8 kg/h.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 265°C.
  • the acid value of the polyester oligomer reaches 15 mgKOH/g
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3582 kg/h.
  • the cotton-like copolymerized modified monomer polyamide slurry is directly injected into the polyester oligomer pipe after the second esterification kettle at 375 kg/h through the polyester oligomer pipeline online addition system.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 252.9 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 2.7 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 221.5 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the antibacterial agent copper-doped zinc oxide concentration 30wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered to the functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 267.9kg/h .
  • the antibacterial agent prepared by grinding and the copper-doped zinc oxide functional powder dispersion with an average particle size of 99nm enters into the functional powder dispersion supply tank, and is transported to the metering unit through the functional powder dispersion composed of a delivery pump and a flow meter.
  • the flow rate of 267.9kg/h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an antibacterial agent copper-doped zinc oxide functional powder slurry with an average particle size of 107 nm, and then the functional powder
  • the bulk slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 489.4 kg/h.
  • the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 267.9 kg/h Produced in the material concentration unit.
  • the content of the antibacterial agent copper-doped zinc oxide in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 3.4 kPa ⁇ cm 2 /g.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 260°C and the reactant temperature of the second precondensation reaction kettle is 265°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 270°C.
  • the filter press value DFFP of the functional polyester is 0.12 kPa ⁇ cm 2 /g.
  • the antibacterial cotton-like polyester fiber monofilament has a fineness of 1.16 dtex, a breaking strength of 3.3 cN/dtex, and an elongation at break of 29%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and flame retardant copolymerized modified monomer 2-carboxyethylphenyl hypophosphite diethylene glycol slurry, Among them, the terephthalic acid slurry is prepared from terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.12, and the flame retardant copolymer modified monomer 2-carboxyethyl phenyl hypophosphite diethylene glycol slurry is composed of 2-Carboxyethyl phenyl hypophosphite diethylene glycol and ethylene glycol are formulated at a weight ratio of 4:6.
  • the esterification reaction system is composed of a vertical first esterification reactor and a vertical second esterification reactor.
  • the terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester of the esterification system at a flow rate of 4394kg/h
  • the reaction reactor and the catalyst ethylene glycol antimony solution with a concentration of 3 wt% were continuously and uniformly injected into the vertical second esterification reactor at a flow rate of 54.8 kg/h.
  • the reaction temperature of the first esterification reactor was 260°C
  • the reaction temperature of the second esterification reactor was 270°C.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3804 kg/h.
  • the flame retardant copolymer modified monomer 2-carboxyethylphenyl diphosphite hypoglycol ester slurry was directly injected into the second esterification kettle at a flow rate of 595.5kg/h through the online addition system of the polyester oligomer pipeline. Ester oligomer pipeline.
  • the ethylene glycol-based functional powder pre-dispersion with a far-infrared agent titanium carbide concentration of 20 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 304 kg/h.
  • the functional powder dispersion of the far-infrared agent titanium carbide with an average particle size of 135 nm prepared by grinding enters the functional powder dispersion supply tank, and is transported to the metering unit by a functional powder dispersion composed of a delivery pump and a flow meter at 304 kg/h
  • the flow rate is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 147 nm of the far-infrared agent titanium carbide, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 576.8 kg/h.
  • the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 304 kg/h Produced in the concentration unit.
  • the content of the far-infrared agent titanium carbide in the functional powder slurry concentrate is 20 wt%, and the pressure filtration value DFMS is 5.2 kPa ⁇ cm 2 /g.
  • the functional powder slurry concentrate of the concentrate preparation system enters the functional powder slurry concentrate mixing unit together, and after being uniformly mixed by the mixing unit, it enters the pre-condensation reaction system.
  • the mixing unit is a high-shear pump.
  • the pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the far-infrared resistance of the flame retardant copolyester is obtained.
  • the far infrared flame retardant polyester fiber monofilament fineness is 1.54 dtex, the breaking strength is 3.5 cN/dtex, and the breaking elongation is 32%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and hydrophilic copolymerized modified monomer polyethylene glycol slurry, wherein the terephthalic acid slurry is composed of p-benzene
  • the dicarboxylic acid and ethylene glycol are prepared with an alkyd molar ratio of 1.15, and the hydrophilic copolymer modified monomer polyethylene glycol slurry is prepared by melt-blending polyethylene glycol at 80°C.
  • the esterification reaction system consists of a vertical esterification reactor.
  • the terephthalic acid slurry is continuously and uniformly delivered to the esterification reactor at a flow rate of 4266kg/h.
  • the catalyst ethylene glycol antimony solution with a concentration of 3wt% is 54.8kg/
  • the flow rate of h is continuously and evenly injected into the esterification reactor.
  • the reaction temperature of the esterification reactor was 265°C.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably extracted from the esterification reactor at a flow rate of 3726 kg/h.
  • the hydrophilic copolymer modified monomer polyethylene glycol slurry is directly injected into the polyester oligomer pipeline after the esterification reactor at a flow rate of 300 kg/h through the polyester oligomer pipeline online addition system.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 731.8 kg/h.
  • the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 9.6 kg/h, and the reaction temperature of the carrier preparation reactor was 255°C.
  • the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 646.1 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a concentration of 20wt% of indium tin oxide as a conductive agent is continuously and uniformly delivered to the functional powder dispersion preparation unit formed by connecting four grinding machines in series at a flow rate of 661.8 kg/h.
  • the functional powder dispersion liquid with an average particle diameter of 65 nm of the conductive agent indium tin oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to the metering unit by a functional powder dispersion liquid composed of a delivery pump and a flow meter to 661.8 kg
  • the flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a conductive powder indium tin oxide average particle size of 71nm, and then the functional powder
  • the slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1307.9 kg/h.
  • the temperature of the evaporation unit is 260°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 661.8 kg/h. Produced in the material concentration unit.
  • the content of the conductive agent indium tin oxide in the functional powder slurry concentrate was 20 wt%, and the filter press value DFMS was 2.4 kPa ⁇ cm 2 /g.
  • the concentrate enters the functional powder slurry concentrate mixing unit together, and after being mixed uniformly by the mixing unit, it enters the pre-condensation reaction system.
  • the mixing unit is a high-shear pump.
  • the pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the intrinsic viscosity of the functional polyester reaches 0.60dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening.
  • the temperature is 285°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antistatic hydrophilic polymer with a hydrophilic copolyester matrix is prepared Ester fiber, wherein the functional polyester has a filter value DFFP of 0.09 kPa ⁇ cm 2 /g.
  • the antistatic hydrophilic polyester fiber has a monofilament fineness of 1.16 dtex, a breaking strength of 4.6 cN/dtex, and an elongation at break of 28%.
  • Polyethylene adipate polyol with a molecular weight of 600 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 609.3 kg/h.
  • the reaction temperature of the carrier preparation reactor is 40°C.
  • the carrier metering and delivery unit composed of a delivery pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 609.3 kg/h.
  • the water-based functional powder pre-dispersion with an antibacterial agent graphene concentration of 10 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 188.4 kg/h, which is prepared by grinding
  • the obtained functional powder dispersion with an average particle diameter of 1000 nm of the antibacterial agent enters into the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 188.4 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a grinder and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 1000 nm of the antibacterial agent graphene, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 797.7 kg/h.
  • the temperature of the evaporation unit is 100°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 628.1 kg/h.
  • the content of the antibacterial agent graphene in the functional powder slurry concentrate is 3 wt%
  • the filter press value DFMS is 30 kPa ⁇ cm 2 /g.
  • the polyester waste alcoholysis product from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and are mixed by the mixing unit After being homogenized, it enters the pre-condensation reaction system, and the mixing unit is a SMXL static mixer.
  • the pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to produce antibacterial regenerated polyester fiber, in which the filter press value of the functional polyester is DFFP It is 0.80 kPa ⁇ cm 2 /g.
  • the antibacterial regenerated polyester fiber has a monofilament fineness of 3.47 dtex, a breaking strength of 2.8 cN/dtex, and an elongation at break of 26%.
  • polyester oligomer slurry The raw material slurry of polyester oligomer consists of terephthalic acid slurry and cationic dye-dyeable copolymerizable modified monomer dipropylene isophthalate-5-sulfonate slurry Among them, the terephthalic acid slurry is prepared from terephthalic acid and propylene glycol with an alkyd molar ratio of 1.4, and the cationic dye can be dyed and copolymerized to modify the monomer dipropylene isophthalate-5-sulfonate. Dipropylene isophthalate-5-sulfonate sodium and propylene glycol are formulated at a weight ratio of 4:6.
  • the esterification reaction system consists of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor.
  • the terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4958 kg/h
  • Chemical reactor, cationic dye-dyeable copolymerizable modified monomer dipropylene isophthalate-5-sulfonate sodium slurry was continuously and uniformly injected into the bedroom horizontal second esterification reactor at a flow rate of 349.2kg/h
  • the two-chamber, 10wt% concentration catalyst tetraisopropyl titanate solution was continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 18.8 kg/h.
  • the reaction temperature of the first esterification reactor was 240°C
  • the reaction temperature of the second esterification reactor was 230°C.
  • the acid value of the polyester oligomer reaches 15 mgKOH/g
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4691 kg/h Out.
  • Propylene glycol-based functional powder pre-dispersion with an anti-ultraviolet radiation agent zinc-doped titanium dioxide concentration of 30% by weight was continuously and uniformly delivered to a functional powder dispersion preparation unit made up of 4 grinding machines in series at a flow rate of 239.4 kg/h.
  • the functional powder dispersion liquid with an average particle diameter of 78 nm, which is an anti-ultraviolet radiation agent zinc-doped titanium dioxide prepared by grinding enters the functional powder dispersion liquid supply tank, and is conveyed to the metering unit by the functional powder dispersion liquid composed of a delivery pump and a flow meter.
  • the flow rate of 239.4kg/h was continuously and stably extracted from the functional powder dispersion supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an anti-ultraviolet radiation agent zinc-doped titanium dioxide with an average particle size of 81 nm, and then the function
  • the powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 469.9 kg/h.
  • the temperature of the evaporation unit is 250°C.
  • the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h Produced in the material concentration unit.
  • the content of the anti-ultraviolet radiation agent zinc-doped titanium dioxide in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 3.1 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification system enters into the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system.
  • the mixing unit is a high-shear pump.
  • the pre-polycondensation reaction system is composed of a vertical pre-condensation reactor, in which the temperature of the reactant in the pre-condensation reactor is 230°C. When the intrinsic viscosity of the prepolymer reaches 0.38dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction.
  • the final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 240°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the anti-ultraviolet radiation cationic dye whose matrix is the cationic dyeable copolyester can be prepared.
  • Dyed polyester fiber where the functional polyester has a filter value DFFP of 0.11 kPa ⁇ cm 2 /g.
  • the anti-ultraviolet radiation cationic dyeable polyester fiber monofilament has a fineness of 1.16 dtex, a breaking strength of 3.2 cN/dtex, and an elongation at break of 31%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h.
  • the esterification reaction is carried out in the first esterification reactor of the esterification reaction system composed of the first esterification reactor and the vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 260°C.
  • the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter continuously and steadily from the second at a flow rate of 3980 kg/h Extracted from the esterification reactor.
  • Polyethylene glycol with a molecular weight of 4000 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 10.4 kg/h.
  • the reaction temperature of the carrier preparation reactor is 80°C.
  • the carrier metering and conveying unit composed of a conveying pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 10.4 kg/h.
  • the water-based functional powder pre-dispersion with a titanium dioxide concentration of 60wt% is continuously and uniformly delivered at a flow rate of 329kg/h to a functional powder dispersion preparation unit composed of 5 grinders in series.
  • the functional powder dispersion with a particle size of 71 nm enters the functional powder dispersion supply tank, and is continuously and stably dispersed from the functional powder at a flow rate of 329 kg/h through the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter Extracted from the liquid supply tank.
  • the carrier and the functional powder dispersion together enter the functional powder dispersion composed of a screw extruder and the mixing unit of the carrier to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 88 nm of titanium dioxide.
  • the flow rate of 339.4kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 110°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a conveying pump with a metering function can continuously and stably remove the functional powder from the functional powder at a flow rate of 207.8 kg/h.
  • the content of titanium dioxide in the functional powder slurry concentrate is 95% by weight, and the pressure filtration value DFMS is 9.4 kPa ⁇ cm 2 /g.
  • the first esterification kettle polyester oligomer from the first esterification reactor of the esterification reaction system enters the functional powder slurry together with the functional powder slurry concentrate from the continuous preparation system of the functional powder slurry concentrate
  • the mixing unit of the material concentrate is mixed uniformly by the mixing unit and then enters the second esterification kettle of the esterification system.
  • the mixing unit is a ball and socket type dynamic mixer.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the reaction temperature of the second esterification reactor was 265°C.
  • the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter continuously and stably from the second at a flow rate of 4128 kg/h Extracted from the esterification reactor.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 275°C and the reactant temperature of the second precondensation reaction kettle is 280°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 290°C.
  • the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to produce an optically shielded polyester fiber, in which the filter press value of the functional polyester is DFFP It is 0.32 kPa ⁇ cm 2 /g.
  • the monofilament fineness of this optically shielding polyester fiber was 1.54 dtex, the breaking strength was 3.1 cN/dtex, and the elongation at break was 24%.
  • the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h.
  • the esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor.
  • the reaction temperature of the first esterification reactor is 260°C
  • the reaction temperature of the second esterification reactor is 265°C.
  • the catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h.
  • the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 380 kg/h, concentration
  • the flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.0 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 333.5 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20% by weight is continuously and uniformly transported to a functional powder dispersion preparation unit composed of three grinding machines in series at a flow rate of 343.7 kg/h, which is prepared by grinding
  • the obtained functional powder dispersion with an average particle size of carbon black of 96 nm enters the functional powder dispersion supply tank, and is continuously stabilized at a flow rate of 343.7 kg/h by the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter It is taken from the functional powder dispersion liquid supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 104 nm, and then the functional powder slurry
  • the flow rate of 677.2kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 343.7 kg/h.
  • the content of carbon black in the functional powder slurry concentrate is 20 wt%
  • the pressure filtration value DFMS is 2.1 kPa ⁇ cm 2 /g.
  • the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit
  • the mixing unit is a high-shear pump.
  • the precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
  • the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the obtained matrix is polyethylene terephthalate
  • the monofilament fineness of this dope-colored black polyester fiber was 1.16 dtex, the breaking strength was 8.1 cN/dtex, and the breaking elongation was 17%.
  • the polyester bottle flake waste and alcoholysis glycol are continuously and uniformly transported to the esterification system composed of the esterification alcoholysis reactor at 3562kg/h and 230kg/h respectively, the esterification alcoholysis reactor is parallel A horizontal reaction kettle provided with a stirrer with two stirring paddles meshing with each other. The reaction temperature of the esterification and alcoholysis reactor was 270°C.
  • the oligomer pump and oligomer flow meter composed of an oligomer delivery and metering device continuously and stably from the esterification alcoholysis reactor at a flow rate of 3792 kg/h Mined out.
  • the online addition system of polyester oligomer pipeline is directly injected into the polyester oligomer pipeline after the esterification and alcoholysis reactor at a flow rate of 472kg/h.
  • the raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 380 kg/h, concentration
  • the flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.0 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C.
  • the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 333.5 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
  • the ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20 wt% is continuously and uniformly delivered at a flow rate of 343.7 kg/h to a functional powder dispersion preparation unit formed by two grinding machines connected in series, and prepared by grinding
  • the obtained functional powder dispersion with an average particle size of 146 nm of carbon black enters the functional powder dispersion supply tank, and is continuously stabilized at a flow rate of 343.7 kg/h by the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter It is taken from the functional powder dispersion liquid supply tank.
  • the carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 154 nm.
  • the flow rate of 677.2kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C.
  • the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 343.7 kg/h.
  • the content of carbon black in the functional powder slurry concentrate is 20 wt%
  • the filter press value DFMS is 4.6 kPa ⁇ cm 2 /g.
  • the functional powder slurry concentrate of the continuous preparation system of the material concentrate enters the functional powder slurry concentrate mixing unit together, and after being uniformly mixed by the mixing unit, it enters the pre-polycondensation reaction system.
  • the mixing unit is a ball and socket type dynamic mixer.
  • the pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C.
  • the final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
  • the intrinsic viscosity of the functional polyester reaches 0.60dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening.
  • the temperature is 290°C.
  • the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the base material is the stock solution of flame retardant recycled copolyester coloring Flame-retardant regenerated polyester fiber, in which the functional polyester has a filter value DFFP of 0.15 kPa ⁇ cm 2 /g.
  • the monofilament fineness of this dope colored flame retardant regenerated polyester fiber was 1.16 dtex, the breaking strength was 3.8 cN/dtex, and the breaking elongation was 32%.
  • the polyester melt with an intrinsic viscosity of 0.65 dL/g was continuously and stably extracted from the final polycondensation reactor through a melt discharge pump at a flow rate of 3750 kg/h, and then transferred to a dynamic mixer through a melt pipe.
  • the functional masterbatch melt of Pigment Blue 15:3 with a concentration of 30 wt% and a pressure filtration value of DFMS of 39.2 kPa ⁇ cm 2 /g was injected into the dynamic mixer through a single screw extruder at a flow rate of 326.1 kg/h.
  • the functional polyester melt obtained by uniformly mixing the polyester melt and the functional masterbatch melt through a dynamic mixer is directly transported to the spinning position through a melt pipe for spinning, to prepare a dope-colored blue polyester fiber, in which the functional polymer
  • the pressure filtration value DFFP of the ester was 1.05 kPa ⁇ cm 2 /g. .
  • the monofilament fineness of this dope-colored blue polyester fiber was 0.77 dtex, the breaking strength was 2.3 cN/dtex, and the elongation at break was 15%.
  • the relevant performance of the test is as follows: the average particle size ( ⁇ m) of the functional powder in the functional powder slurry, the test method: first dissolve the functional powder slurry in a good solvent hexafluoroisopropanol, and then use dynamic light scattering particle size The instrument tests the particle size of the functional powder.
  • the filter press value of functional powder slurry concentrate DFMB (kPa ⁇ cm 2 /g), test method: from functional powder slurry concentrate with weight m1 and polyester polyethylene terephthalate with weight m2
  • the total weight of the ester composition is 4000g test mixture, the content of functional powder in the test mixture is 100g; it consists of a single screw extruder with an aspect ratio of ⁇ 25mm ⁇ 25D, a melt metering pump with a volume of 1.2cc, a melt pressure sensor and The 60-100-1400-100-20 mesh four-layer combination screen with a filter area S of 3.8cm2 is connected in sequence to form a filter performance tester; filter performance test process conditions: melt temperature is 295°C, melt metering pump The pre-pump pressure setting is 6.5MPa and the melt metering pump metering flow rate is 38g/min; first squeeze 500g of polyester polyethylene terephthalate from the filter performance tester and record the equilibrium pressure as the initial Pressure Ps, then extrude
  • Intrinsic viscosity of functional polyester (dL/g), test method: refer to GB/T 14190-2008.
  • Functional polyester filter press value DFFP (kPa ⁇ cm 2 /g), test method: single screw extruder with aspect ratio ⁇ 25mm ⁇ 25D, melt metering pump with a volume of 1.2cc, melt pressure sensor and filter
  • the 60-100-1400-100-20 mesh four-layer combined filter screen with a mesh area S of 3.8cm2 is connected in sequence to form a filter performance tester; filter performance test process conditions: melt temperature is 295°C, melt metering pump pump The pre-pressure setting value is 6.5MPa, the metering flow rate of the melt metering pump is 38g/min; first squeeze 500g polyester polyethylene terephthalate from the filter performance tester, and record the equilibrium pressure as the initial pressure Ps, then extrude 3000g of functional polyester from the filter performance tester, and then extrude 500g of polyester polyethylene terephthalate from the filter performance tester, and
  • the filter press value DFFP of the functional polyester prepared by the functional polyester production method of the present invention is not higher than 0.8 kPa ⁇ cm 2 /g, and compared with the masterbatch method
  • the functional polyester has a lower pressure filtration value, and the functional polyester prepared by the production method of the functional polyester of the present invention has a higher uniformity of dispersion of functional powder.
  • the addition amount of the pigment blue 15:3 used in the preparation of the functional polyester in Example 1 and Comparative Example 1 of the present invention is the same, but the pigment blue 15:3 in Example 1 is a continuous preparation of the functional powder slurry concentrate Formed into the polyester oligomer and then through the polycondensation reaction to obtain a functional polyester, and in Comparative Example 1 pigment blue 15:3 in the form of masterbatch is added to the polyester melt prepared by the final polycondensation reaction to obtain a functional polyester .
  • the functional powder is difficult to disperse highly uniformly in the high-viscosity polyester melt, and the prepared functional polyester melt has poor spinning performance.
  • the preparation of the functional powder dispersion liquid adopts a grinding machine. Under the action of the high-speed rotation of the grinding and dispersing shaft, the grinding medium accurately and repeatedly exerts force on the functional powder particles, so that the functional powder particles are crushed to the nanometer level, thereby achieving the functional powder Alcohol or water is efficiently and evenly dispersed on a small scale.
  • the functional powder slurry can be prepared by mixing the functional powder dispersion liquid with a reactive bifunctional compound such as polyester polyol, polyether or polyester oligomer as a carrier.
  • the functional powder slurry is transported to the functional powder slurry concentration unit, and the water or excess alcohol present in the functional powder slurry can be removed through the flash devolatilization treatment, and the low-pressure filtration value of the highly uniformly dispersed functional powder can be prepared.
  • Low hydroxyl value functional powder slurry concentrate Injecting carbon black in the form of functional powder slurry concentrate into the polyester production system can achieve highly uniform dispersion of pigment blue 15:3 particles in the polyester matrix, effectively reducing pigment blue 15:3 particles during the preparation of functional polyester Reunion.
  • the filter press value DFFP of the functional polyester in Example 1 was 0.21 kPa ⁇ cm 2 /g, and the filter press value DFFP of the functional polyester in Comparative Example 1 was 1.05 kPa ⁇ cm 2 /g, in Example 1 Pigment Blue 15 :3 is more uniformly dispersed, and the functional polyester has a lower filter value, so that the functional polyester fiber prepared has a more uniform structure and better mechanical properties.
  • the same pigment blue 15:3 is used to prepare the same amount
  • the linear polyester functional polyester fiber, the functional polyester fiber prepared in Example 1 had a breaking strength of 3.4 cN/dtex, while the functional polyester fiber prepared in Comparative Example 1 had a breaking strength of only 2.3 cN/dtex.

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Abstract

A functional polyester production system, which relates to the technical field of polymer material synthesis. The functional polyester production system comprises a polyester main body production system and a functional powder slurry concentrate preparation system; the polyester main body production system comprises an esterification system, a pre-polycondensation system and a final polycondensation system that are connected in sequence; the functional powder slurry concentrate preparation system comprises an online addition device that is connected to the esterification system or/and to a site between the esterification system and the pre-polycondensation system. By introducing a functional powder slurry concentrate preparation system into a polyester main body production system, a functional powder slurry concentrate having a low hydroxyl value and low pressure filtration value may be continuously prepared, and the prepared functional powder slurry concentrate and a polyester oligomer are uniformly mixed and then undergo a polycondensation reaction to obtain functional polyester in which functional powder is highly uniformly dispersed. The present invention also relates to a functional polyester production method.

Description

一种功能聚酯生产方法、生产系统及功能聚酯纤维Production method, production system and functional polyester fiber of functional polyester 技术领域Technical field
本发明属于高分子材料合成技术领域，具体地说，涉及一种功能聚酯生产方法及、生产系统及功能聚酯纤维。The invention belongs to the technical field of polymer material synthesis, and specifically relates to a production method and production system of functional polyester and functional polyester fiber.
背景技术Background technique
目前，功能聚酯纤维的制备方法主要是采用母粒法，先将功能粉体与载体树脂熔融混合得到高功能粉体含量的功能母粒，然后再将功能母粒熔体与纺丝用聚酯熔体均匀混合经纺丝过程得到功能聚酯纤维。母粒法制备功能聚酯纤维的过程中，由于功能粉体在高粘聚酯熔体中的分散主要是依靠混合设备所提供的机械剪切力，功能粉体难以在聚酯熔体中高均匀分散，制备得到的功能聚酯熔体的纺丝性能较差，不易纺制细旦或超细旦的功能聚酯纤维。At present, the preparation method of the functional polyester fiber mainly adopts the masterbatch method. First, the functional powder and the carrier resin are melted and mixed to obtain the functional masterbatch with high functional powder content, and then the functional masterbatch melt and the spinning polymer are used. The ester melt is uniformly mixed to obtain functional polyester fibers through the spinning process. In the process of preparing functional polyester fibers by the masterbatch method, because the dispersion of the functional powder in the high-viscosity polyester melt mainly depends on the mechanical shear force provided by the mixing equipment, the functional powder is difficult to be uniform in the polyester melt Dispersed, the prepared functional polyester melt has poor spinning performance, and it is not easy to spin functional polyester fibers with fine denier or ultrafine denier.
有鉴于此特提出本发明。In view of this, the present invention is specifically proposed.
发明内容Summary of the invention
本发明要解决的技术问题在于克服现有技术的不足，提供一种功能聚酯生产方法及生产系统，以实现功能粉体高度均匀分散的功能聚酯的连续稳定制备，提高功能聚酯的纺丝性能。The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art, and to provide a production method and production system of functional polyester to realize the continuous and stable preparation of functional polyester with highly uniformly dispersed functional powder and improve the spinning of functional polyester Silk performance.
为解决上述技术问题，本发明采用技术方案的基本构思是：In order to solve the above technical problems, the basic concept of the technical solution adopted by the present invention is:
一种功能聚酯生产系统，包括聚酯主体生产系统和功能粉体浆料浓缩物制备系统，所述的聚酯主体生产系统包括依次连接的酯化系统、预缩聚系统和终缩聚系统，功能粉体浆料浓缩物制备系统包括与酯化系统或/和酯化系统、预缩聚系统之间部位连接的在线添加装置。A functional polyester production system, including a polyester main production system and a functional powder slurry concentrate preparation system. The polyester main production system includes an esterification system, a pre-condensation system and a final polycondensation system connected in sequence. The powder slurry concentrate preparation system includes an online addition device connected to the esterification system or/and between the esterification system and the pre-condensation system.
作为本发明的一种实施方式，功能粉体浆料浓缩物制备系统包括依次连接的浆料制备单元、浆料浓缩单元和在线添加装置，在线添加装置的出料口与酯化系统或/和酯化系统、预缩聚系统之间部位连接。As an embodiment of the present invention, the functional powder slurry concentrate preparation system includes a slurry preparation unit, a slurry concentration unit and an online addition device connected in sequence, and the discharge port of the online addition device and the esterification system or/and The connection between the esterification system and the pre-condensation system.
作为本发明的一种实施方式，功能粉体浆料制备单元包括载体制备单元、功能粉体分散液制备单元和混合单元，载体制备单元经计量输送装置连接功能粉体分散液制备单元，功能粉体分散液制备单元经计量输送装置连接混合单元。As an embodiment of the present invention, the functional powder slurry preparation unit includes a carrier preparation unit, a functional powder dispersion preparation unit, and a mixing unit. The carrier preparation unit is connected to the functional powder dispersion preparation unit via a metering and conveying device. The functional powder The bulk dispersion preparation unit is connected to the mixing unit via a metering and conveying device.
混合单元包括但不限于剪切泵、螺杆挤出机、研磨机、行星齿轮动态混合器、动静齿圈式动态混合器或球窝式动态混合器。Mixing units include but are not limited to shear pumps, screw extruders, grinders, planetary gear dynamic mixers, dynamic and static ring gear type dynamic mixers or ball and socket type dynamic mixers.
优选地，浆料浓缩单元具有闪蒸功能的反应釜，不设置搅拌结构。Preferably, the slurry concentration unit has a reaction kettle with a flashing function, and no stirring structure is provided.
功能粉体浆料进入具有闪蒸功能的反应釜，一方面在负压条件下会闪蒸脱除功能粉体浆料中存在的水或者过量的醇，制备得到功能粉体高度均匀分散的低压滤值的功能粉体浆料浓缩物。另一方面，功能粉体浆料中水或者过量醇的闪蒸气化，会使得物料出现较剧烈的沸腾，代替机械搅拌器达到搅拌的作用，因此，既可以提高反应器的运行可靠性且便于反应器的清洁、降低反应器的运行能耗。The functional powder slurry enters the reaction kettle with flashing function, on the one hand, under negative pressure conditions, the water or excess alcohol present in the functional powder slurry will be flashed off to prepare a low pressure with highly uniformly dispersed functional powder Filter value of functional powder slurry concentrate. On the other hand, the flashing of water or excess alcohol in the functional powder slurry will cause the material to boil violently and replace the mechanical stirrer to achieve the stirring effect. Therefore, it can improve the operation reliability of the reactor and facilitate The cleaning of the reactor reduces the energy consumption of the reactor.
作为本发明的一种实施方式，在线添加装置包括计量输送装置和/或混合装置，计量输送装置包括输送泵和流量计或具有计量功能的输送泵，混合装置包括静态混合器或/和动态混合器。As an embodiment of the present invention, the online addition device includes a metering delivery device and/or a mixing device, the metering delivery device includes a delivery pump and a flow meter or a delivery pump with a metering function, and the mixing device includes a static mixer or/and dynamic mixing Device.
静态混合器包括但不限于SMX型混合器、SMXL型混合器、SMV型混合器；动态混合器包括但不限于剪切泵、螺杆挤出机、行星齿轮动态混合器、动静齿圈式动态混合器、球窝式动态混合器。Static mixers include but are not limited to SMX type mixers, SMXL type mixers, SMV type mixers; dynamic mixers include but not limited to shear pumps, screw extruders, planetary gear dynamic mixers, dynamic and static ring gear type dynamic mixing , Ball and socket dynamic mixer.
作为本发明的一种实施方式，聚酯主体生产系统还包括液相增粘反应釜，终缩聚系统的出料口与液相增粘反应釜的进口连接，液相增粘反应釜的出口与纺丝设备连接。As an embodiment of the present invention, the polyester main production system further includes a liquid-phase tackifying reaction kettle, the outlet of the final polycondensation system is connected to the inlet of the liquid-phase tackifying reaction kettle, and the outlet of the liquid-phase tackifying reaction kettle is Spinning equipment connection.
优选地，聚酯主体生产系统的酯化系统、预缩聚系统和终缩聚系统之间经在线添加装置连接，更优选地，聚酯主体生产系统包括经在线添加装置依次连接的酯化反应釜或酯化醇解反应釜、预缩聚反应釜，终缩聚反应釜和液相增粘反应釜。Preferably, the esterification system, the pre-condensation system and the final polycondensation system of the polyester main production system are connected via an online addition device, and more preferably, the polyester main production system includes an esterification reaction kettle or Esterification alcoholysis reactor, pre-condensation reactor, final polycondensation reactor and liquid-phase thickening reactor.
聚酯主体生产系统的酯化反应釜或酯化醇解反应釜、预缩聚反应釜，终缩聚反应釜和液相增粘反应釜可以设置为一个或多个。One or more esterification reactors, esterification alcoholysis reactors, pre-condensation reactors, final polycondensation reactors and liquid-phase viscosity-increasing reactors in the polyester main production system can be provided.
本发明的另一目的在于提供一种功能聚酯的生产方法，包括如下步骤：Another object of the present invention is to provide a method for producing functional polyester, including the following steps:
S1，制备聚酯低聚物；S1, preparation of polyester oligomers;
S2，将功能粉体分散液、载体混合均匀制备功能粉体浆料，浓缩功能粉体浆料，得到功能粉体浆料浓缩物，所述载体为具有反应活性的双官能团化合物；S2, mixing the functional powder dispersion liquid and the carrier to uniformly prepare the functional powder slurry, concentrating the functional powder slurry, and obtaining a functional powder slurry concentrate, wherein the carrier is a reactive bifunctional compound;
S3，将功能粉体浆料浓缩物在线连续添加至聚酯低聚物中，混合均匀，进行预缩聚反应得到功能聚酯预聚物，功能聚酯预聚物经终缩聚反应，得到功能聚酯。S3: Continuously add the functional powder slurry concentrate to the polyester oligomer online, mix evenly, and perform the pre-condensation reaction to obtain the functional polyester prepolymer. The functional polyester prepolymer undergoes final polycondensation reaction to obtain the functional polymer ester.
功能粉体分散液用如下方法制备：功能粉体和水和/或二元醇为原料进行功能粉体分散液的配置。二元醇包括但不限于乙二醇、丙二醇、丁二醇、己二醇、甲基丙二醇、新戊二醇、二甘醇或三甘醇。The functional powder dispersion is prepared by the following method: the functional powder and water and/or glycol are used as raw materials to configure the functional powder dispersion. Glycols include but are not limited to ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, methyl propylene glycol, neopentyl glycol, diethylene glycol or triethylene glycol.
作为本发明的一种实施方式，所述功能粉体为具有着色、抗菌、防辐射、抗菌、导电、导热、远红外、阻燃、负离子、荧光或磁性功能的粉体；所述载体选自聚酯多元醇、聚醚或聚酯低聚物。As an embodiment of the present invention, the functional powder is a powder having functions of coloring, antibacterial, radiation protection, antibacterial, conductive, thermal conductivity, far infrared, flame retardant, negative ion, fluorescent or magnetic; the carrier is selected from Polyester polyol, polyether or polyester oligomer.
功能粉体可选自下列物质中的一种或几种：炭黑、颜料棕3、颜料蓝5、颜料蓝15、颜料蓝15:1、颜料蓝15:3、颜料蓝15:4、颜料蓝15:6、颜料蓝16、颜料蓝28、颜料蓝29、颜料蓝60、颜料紫19、颜料紫23、颜料紫29、颜料红101、颜料红102、颜料红108、颜料红112、颜料红122、颜料红146、颜料红149、颜料红170、颜料红171、颜料红172、颜料红175、颜料红176、颜料红177、颜料红178、颜料红179、颜料红185、颜料红202、颜料红207、颜料红208、颜料红214、颜料红241、颜料红242、颜料红254、颜料红255、颜料红263、颜料红264、颜料红272、颜料黄6、颜料黄13、颜料黄14、颜料黄17、颜料黄21、颜料黄37、颜料黄77、颜料黄74、颜料黄81、颜料黄97、颜料黄107、颜料黄110、颜料黄120、颜料黄129、颜料黄138、颜料黄139、颜料黄147、颜料黄148、颜料黄150、颜料黄151、颜料黄155、颜料黄168、颜料黄174、颜料黄180、颜料黄187、颜料黄192、颜料黄195、颜料黄196、颜料黄197、颜料橙34、颜料橙36、颜料橙43、颜料橙61、颜料橙64、颜料橙68、颜料橙70、颜料橙73、颜料绿5、颜料绿7、颜料绿36、颜料绿50黄绿夜光粉(ZnS:Cu)、长余辉荧光粉(SrMgAl4O8:Eu2+Dy3+)、天蓝夜光粉(Sr2MgSi2O7)、桔黄夜光粉(Y2O2S:Eu.Mg:Ti)、黄绿光夜光粉(SrAl2O4:Eu.Dy)、蓝绿光夜光粉(Sr4A14O25:Eu.Dy)、橙红夜光粉(Y2O2S:Eu.Mg:Ti)、二氧化硅、银、锗、氧化银、载银沸石、载银二氧化钛、掺锌二氧化钛、掺铜二氧化钛、载银氧化锌、掺锌氧化铜、掺铜氧化锌、氧化亚铜、氧化锌、氧化铝、二氧化钛、二氧化硅、石墨烯、碳纳米管、氮化铝、氮化硼、碳化硅、石墨、竹炭、咖啡碳、碳化锆、氧化锆、碳化钛、碳化铪、电气石、蛋白石、奇才石、层状双氢氧化物、云母、玉石、氢氧化镁、硼酸锌、四氧化三铁或氧化锡锑、氧化铟锡、掺铝氧化锌。The functional powder can be selected from one or more of the following substances: carbon black, pigment brown 3, pigment blue 5, pigment blue 15, pigment blue 15:1, pigment blue 15:3, pigment blue 15:4, pigment Blue 15:6, Pigment Blue 16, Pigment Blue 28, Pigment Blue 29, Pigment Blue 60, Pigment Violet 19, Pigment Violet 23, Pigment Violet 29, Pigment Red 101, Pigment Red 102, Pigment Red 108, Pigment Red 112, Pigment Red 122, Pigment Red 146, Pigment Red 149, Pigment Red 170, Pigment Red 171, Pigment Red 172, Pigment Red 175, Pigment Red 176, Pigment Red 177, Pigment Red 178, Pigment Red 179, Pigment Red 185, Pigment Red 202 , Pigment Red 207, Pigment Red 208, Pigment Red 214, Pigment Red 241, Pigment Red 242, Pigment Red 254, Pigment Red 255, Pigment Red 263, Pigment Red 264, Pigment Red 272, Pigment Yellow 6, Pigment Yellow 13, Pigment Yellow 14, Pigment Yellow 17, Pigment Yellow 21, Pigment Yellow 37, Pigment Yellow 77, Pigment Yellow 74, Pigment Yellow 81, Pigment Yellow 97, Pigment Yellow 107, Pigment Yellow 110, Pigment Yellow 120, Pigment Yellow 129, Pigment Yellow 138 , Pigment yellow 139, pigment yellow 147, pigment yellow 148, pigment yellow 150, pigment yellow 151, pigment yellow 155, pigment yellow 168, pigment yellow 174, pigment yellow 180, pigment yellow 187, pigment yellow 192, pigment yellow 195, pigment Yellow 196, Pigment Yellow 197, Pigment Orange 34, Pigment Orange 36, Pigment Orange 43, Pigment Orange 61, Pigment Orange 64, Pigment Orange 68, Pigment Orange 70, Pigment Orange 73, Pigment Green 5, Pigment Green 7, Pigment Green 36 , Pigment Green 50 yellow-green luminous powder (ZnS:Cu), long afterglow phosphor (SrMgAl4O8:Eu2+Dy3+), sky blue luminous powder (Sr2MgSi2O7), orange yellow luminous powder (Y2O2S:Eu.Mg:Ti), yellow-green luminous powder (SrAl2O4:Eu.Dy), blue-green luminous powder (Sr4A14O25:Eu.Dy), orange-red luminous powder (Y2O2S:Eu.Mg:Ti), silica, silver, germanium, silver oxide, silver-loaded zeolite, supported Silver titanium dioxide, zinc-doped titanium dioxide, copper-doped titanium dioxide, silver-bearing zinc oxide, zinc-doped copper oxide, copper-doped zinc oxide, cuprous oxide, zinc oxide, aluminum oxide, titanium dioxide, silicon dioxide, graphene, carbon nanotubes, nitrogen Aluminum oxide, boron nitride, silicon carbide, graphite, bamboo charcoal, coffee carbon, zirconium carbide, zirconium oxide, titanium carbide, hafnium carbide, tourmaline, opal, wizardry stone, layered double hydroxide, mica, jade, hydroxide Magnesium, zinc borate, ferric oxide or antimony tin oxide, indium tin oxide, aluminum-doped zinc oxide.
作为本发明的一种实施方式，制备功能粉体浆料时，控制功能粉体浆料中功能粉体的平均粒径不高于1000nm，优选不高于500nm，更优选不高于300nm；As an embodiment of the present invention, when preparing the functional powder slurry, the average particle diameter of the functional powder in the functional powder slurry is controlled to be not higher than 1000 nm, preferably not higher than 500 nm, and more preferably not higher than 300 nm;
将功能粉体浆料中功能粉体的平均粒径控制在上述范围，可保证功能粉体在后续制备得到功能粉体浆料浓缩物中呈高度均匀分散，使功能粉体浆料浓缩物具有低压滤值。The average particle diameter of the functional powder in the functional powder slurry is controlled within the above range, which can ensure that the functional powder is highly uniformly dispersed in the subsequent preparation of the functional powder slurry concentrate, so that the functional powder slurry concentrate has Low pressure filter value.
进一步地，功能粉体浆料浓缩物中的功能粉体的含量为3％～95％，优选5％～60％，更优选10％～50％；Further, the content of the functional powder in the functional powder slurry concentrate is 3% to 95%, preferably 5% to 60%, and more preferably 10% to 50%;
将功能粉体浓缩物中功能粉体的含量控制在上述范围，可制备得到功能粉体呈高度均匀分散的功能粉体浓缩物。By controlling the content of the functional powder in the functional powder concentrate to the above range, a functional powder concentrate in which the functional powder is highly uniformly dispersed can be prepared.
进一步地，功能粉体浆料浓缩物的羟值不高于175mgKOH/g，压滤值DFMS不高于30kPa·cm 2/g。 Further, the hydroxyl value of the functional powder slurry concentrate is not higher than 175 mgKOH/g, and the filter press value DFMS is not higher than 30 kPa·cm 2 /g.
将功能粉体浓缩物的羟值控制在上述范围内，在缩聚反应过程中副产物二元醇生成量小，避免注入聚酯生产系统时因为二元醇的蒸发量显著增加而导致生产运行稳定性下降。The hydroxyl value of the functional powder concentrate is controlled within the above range. The amount of by-product diol generated during the polycondensation reaction is small, to avoid stable production operation due to the significant increase in the amount of diol evaporation when injected into the polyester production system. Sexual decline.
将功能粉体浆料浓缩物的压滤值控制在上述范围内，功能粉体浆料浓缩物引入聚酯生产系统时功能粉体具有较好的分散性，使功能粉体在制备的功能聚酯中高度均匀分散。The pressure filtration value of the functional powder slurry concentrate is controlled within the above range. When the functional powder slurry concentrate is introduced into the polyester production system, the functional powder has better dispersibility, so that the functional powder Highly evenly dispersed in the ester.
作为本发明的一种实施方式，制备聚酯低聚物的原料包括对苯二甲酸浆料、共聚改性单体浆料或聚酯废料，所述对苯二甲酸浆料由二元醇与对苯二甲酸按照摩尔比1.05～2.0制备得到，共聚改性单体浆料由共 聚改性单体和/或二元醇为原料配制得到，所述聚酯废料为聚酯瓶废旧料及生产下脚料、聚酯膜废旧料及生产下脚料、聚酯纺织品废旧料及生产下脚料和/或聚酯纤维生产下脚料。As an embodiment of the present invention, raw materials for preparing polyester oligomers include terephthalic acid slurry, copolymer modified monomer slurry or polyester waste. The terephthalic acid slurry is composed of glycol and Terephthalic acid is prepared according to a molar ratio of 1.05 to 2.0. Copolymer modified monomer slurry is prepared from copolymer modified monomer and/or glycol as raw materials. The polyester waste is waste from polyester bottles and production. Materials, polyester film waste and production scrap, polyester textile waste and production scrap and/or polyester fiber production scrap.
将对苯二甲酸浆料中的醇酸摩尔比控制在1.05～2.0，对苯二甲酸具有良好的成浆性，而且该醇酸摩尔比范围内的对苯二甲酸浆料输入酯化系统，酯化系统的气升量在合适的范围内，有利于酯化反应的平稳进行，而且酯化反应过程中乙二醇的冷凝回流量小，有利于节约反应能耗。Control the molar ratio of alkyd acid in the terephthalic acid slurry to 1.05～2.0, terephthalic acid has good slurryability, and the terephthalic acid slurry in the range of the molar ratio of alkyd acid is input into the esterification system, The air lift of the esterification system is in a suitable range, which is conducive to the smooth progress of the esterification reaction, and the small condensate return flow of ethylene glycol during the esterification reaction is conducive to saving the reaction energy consumption.
共聚改性单体包括但不限于下列物质：间苯二甲酸、己二酸、新戊二醇、二甘醇、聚乙二醇、山梨醇、聚酰胺、聚己二酸乙二醇酯、间苯二甲酸二乙二醇酯-5-磺酸钠、间苯二甲酸二乙二醇酯-5-磺酸锂、间苯二甲酸二乙二醇酯-5-磺酸钾、2-羧乙基苯基次磷酸二乙二醇酯、[(6-氧代-6H-二苯并[c,e][1,2]氧磷杂己环-6-基)甲基]丁二酸二乙二醇酯、间苯二甲酸二丙二醇酯-5-磺酸钠、间苯二甲酸二丙二醇酯-5-磺酸锂、间苯二甲酸二丙二醇酯-5-磺酸钾、2-羧乙基苯基次磷酸二丙二醇酯、[(6-氧代-6H-二苯并[c,e][1,2]氧磷杂己环-6-基)甲基]丁二酸二丙二醇酯、间苯二甲酸二丁二醇酯-5-磺酸钠、间苯二甲酸二丁二醇酯-5-磺酸锂、间苯二甲酸二丁二醇酯-5-磺酸钾、2-羧乙基苯基次磷酸二丁二醇酯、[(6-氧代-6H-二苯并[c,e][1,2]氧磷杂己环-6-基)甲基]丁二酸二丁二醇酯。Co-modified monomers include but are not limited to the following substances: isophthalic acid, adipic acid, neopentyl glycol, diethylene glycol, polyethylene glycol, sorbitol, polyamide, polyethylene adipate, Diethylene glycol isophthalate-5-sulfonate sodium, diethylene glycol isophthalate-5-sulfonate lithium, diethylene glycol isophthalate-5-sulfonate potassium, 2- Diethylene glycol carboxyethylphenyl hypophosphite, [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)methyl]butanedi Diethylene glycol acid, dipropylene isophthalate-5-sulfonate sodium, dipropylene isophthalate-5-sulfonate lithium, dipropylene isophthalate-5-sulfonate potassium, 2 -Dipropylene glycol carboxyethylphenyl hypophosphite, [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)methyl]succinic acid Dipropylene glycol ester, dibutyl glycol isophthalate-5-sulfonate sodium, dibutyl glycol isophthalate-5-sulfonate lithium, dibutyl glycol isophthalate-5-sulfonic acid Potassium, 2-carboxyethylphenyl dibutyl glycol hypophosphite, [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorane-6-yl)methan ] Dibutyl glycol succinate.
共聚改性单体浆料的加入可赋予功能粉体改性聚酯阳离子染料染色、分散染料常压染色、抗菌、亲水、低熔点、高收缩、仿棉等复合功能，根据共聚改性单体的性质，共聚改性单体浆料可在酯化系统的不同反应阶段加入。The addition of copolymer modified monomer slurry can endow functional powder modified polyester cationic dye dyeing, disperse dye atmospheric dyeing, antibacterial, hydrophilic, low melting point, high shrinkage, cotton imitation and other composite functions. The nature of the body, the copolymer modified monomer slurry can be added in different reaction stages of the esterification system.
作为本发明的一种实施方式，功能聚酯预聚物的特性粘度为0.1～0.5dL/g，功能聚酯的特性粘度为0.5～1.2dL/g、压滤值DFFP不高于0.8kPa·cm 2/g。 As an embodiment of the present invention, the intrinsic viscosity of the functional polyester prepolymer is 0.1 to 0.5 dL/g, the intrinsic viscosity of the functional polyester is 0.5 to 1.2 dL/g, and the filter press value DFFP is not higher than 0.8 kPa· cm 2 /g.
将特性粘度和压滤值控制在上述范围内，可使功能粉体在聚酯基体中呈高度均匀分散，制备得到的功能聚酯适用于制备高品质薄膜和纤维等产品。酯化系统的反应温度为230～280℃，预缩聚系统的反应温度为230～290℃，终缩聚系统的反应温度为240～300℃。By controlling the intrinsic viscosity and the pressure filtration value within the above range, the functional powder can be highly uniformly dispersed in the polyester matrix. The prepared functional polyester is suitable for preparing high-quality films and fibers. The reaction temperature of the esterification system is 230-280°C, the reaction temperature of the pre-condensation system is 230-290°C, and the reaction temperature of the final polycondensation system is 240-300°C.
本发明的又一目的在于提供一种功能聚酯纤维，所述功能聚酯纤维由上述内容任一所述的功能聚酯生产系统、任一项所述的功能聚酯的生产方法得到的功能聚酯纺制而成。Still another object of the present invention is to provide a functional polyester fiber obtained from the functional polyester production system described in any one of the foregoing, and the function obtained by the functional polyester production method described in any one of the above Made of polyester.
优选地，所述功能聚酯纤维包括原液着色、抗菌、防辐射、抗静电、荧光、远红外、导热或负离子中的一种或几种的功能聚酯纤维。Preferably, the functional polyester fibers include one or more of functional polyester fibers in the colors of undiluted solution, antibacterial, anti-radiation, antistatic, fluorescent, far infrared, thermally conductive, or negative ions.
优选地，所述功能聚酯分子为聚对苯二甲酸乙二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸丁二醇酯；更优选地，功能聚酯分子为具有阳离子染料可染、亲水、仿棉、阻燃、低熔点或高收缩功能的共聚酯。Preferably, the functional polyester molecule is polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate; more preferably, the functional polyester molecule has a cationic dye Dyeable, hydrophilic, cotton-like, flame retardant, low melting point or high shrinkage copolyester.
采用上述技术方案后，本发明与现有技术相比具有以下有益效果：After adopting the above technical solution, the present invention has the following beneficial effects compared with the prior art:
本发明在聚酯主生产系统中引入功能粉体浆料浓缩物制备系统，可连续制备具有低羟值、低压滤值的功能粉体浆料浓缩物，并将制备的功能粉体浆料浓缩物与聚酯低聚物均匀混合后进行缩聚反应，获得功能粉体高度均匀分散的功能聚酯，利于改善功能聚酯的纺丝性能，适合用于生产高品质纤维和薄膜等产品。The invention introduces a functional powder slurry concentrate preparation system into the main polyester production system, which can continuously prepare functional powder slurry concentrates with low hydroxyl value and low pressure filtration value, and concentrate the prepared functional powder slurry concentrate After the material and polyester oligomer are mixed uniformly, the polycondensation reaction is carried out to obtain the functional polyester with highly uniformly dispersed functional powder, which is conducive to improving the spinning performance of the functional polyester and is suitable for the production of high-quality fibers and films.
本发明所述的功能聚酯生产方法，易于工业化实施，可实现功能聚酯的大规模工业化连续生产功能粉体高度均匀分散的功能聚酯，改善功能聚酯的纺丝性能，且提高功能聚酯的生产效率、降低成本。The production method of functional polyester according to the present invention is easy to implement industrially, can realize large-scale industrialization of functional polyester and continuously produce functional polyester with highly uniformly dispersed functional powder, improve the spinning performance of functional polyester, and improve the functional polymerization Ester production efficiency and cost reduction.
附图说明BRIEF DESCRIPTION
附图作为本发明的一部分，用来提供对本发明的进一步的理解，本发明的示意性实施例及其说明用于解释本发明，但不构成对本发明的不当限定。显然，下面描述中的附图仅仅是一些实施例，对于本领域普通技术人员来说，在不付出创造性劳动的前提下，还可以根据这些附图获得其他附图。在附图中：As a part of the present invention, the drawings are used to provide a further understanding of the present invention. The schematic embodiments and descriptions of the present invention are used to explain the present invention, but do not constitute an undue limitation on the present invention. Obviously, the drawings in the following description are only some embodiments, and those of ordinary skill in the art can obtain other drawings based on these drawings without paying any creative labor. In the drawings:
图1是本发明所述的功能聚酯生产方法的一种工艺流程示意图；1 is a schematic process flow diagram of the production method of functional polyester according to the present invention;
图2是本发明所述的功能聚酯生产系统的一种结构示意图；2 is a schematic structural diagram of a functional polyester production system according to the present invention;
图3是本发明所述的功能聚酯生产系统的第二种结构示意图；3 is a schematic diagram of a second structure of the functional polyester production system according to the present invention;
图4是本发明所述的功能聚酯生产系统的第三种结构示意图；4 is a schematic diagram of a third structure of the functional polyester production system according to the present invention;
图5是本发明所述的功能聚酯生产系统的第四种结构示意图。FIG. 5 is a fourth structural schematic diagram of the functional polyester production system according to the present invention.
需要说明的是，这些附图和文字描述并不旨在以任何方式限制本发明的构思范围，而是通过参考特定实施例为本领域技术人员说明本发明的概念。It should be noted that these drawings and text descriptions are not intended to limit the scope of the present invention in any way, but to explain the concept of the present invention to those skilled in the art by referring to specific embodiments.
具体实施方式detailed description
为使本发明的目的、技术方案和优点更加清楚，下面结合部分实施例对本发明的技术方案进行清楚、完整地描述，以下实施例仅用于说明本发明，不用于限制本发明的范围。In order to make the purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be described clearly and completely in conjunction with some embodiments. The following embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention.
实施例1Example 1
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.13的聚酯低聚物浆料聚酯低聚物的原料浆以4613kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3931kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 265°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体的原料浆以293.7kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为2.9kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到15mgKOH/g，通过由输送泵和流量计组成的载体计量输送单元以255kg/h的流量连续稳定地从载体制备反应釜采出。S2, the raw material slurry prepared by mixing terephthalic acid and ethylene glycol into a carrier with an alkyd molar ratio of 1.3 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 293.7 kg/h, with a concentration of 3 wt The flow rate of the% catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 2.9 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 255 kg/h through a carrier metering and conveying unit composed of a conveying pump and a flow meter.
将颜料蓝15:3浓度为40wt％的乙二醇基功能粉体预分散液以244.6kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的颜料蓝15:3平均粒径为143nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以244.6kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The pigment blue 15:3 concentration of 40wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered at a flow rate of 244.6kg/h to a functional powder dispersion preparation unit made up of 3 grinders in series, The pigment powder 15:3 prepared by grinding and the functional powder dispersion with an average particle size of 143nm enters the functional powder dispersion supply tank, and is transported to a measuring unit of 244.6kg through the functional powder dispersion composed of a delivery pump and a flow meter The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到颜料蓝15:3平均粒径为154nm的功能粉体浆料，然后将功能粉体浆料以499.6kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为275℃。当功能粉体浆料浓缩物的羟值达到49mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以326.1kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中颜料蓝15:3的含量为30wt％、压滤值DFMS为6.1kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a pigment blue 15:3 functional powder slurry with an average particle size of 154 nm, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 499.6 kg/h. The temperature of the evaporation unit is 275°C. When the hydroxyl value of the functional powder slurry concentrate reaches 49 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 326.1 kg/h Extracted from the feed concentration unit, the content of the pigment blue 15:3 in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 6.1 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和卧式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.35dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。S3, the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit After entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.35dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
当功能聚酯特性粘度达到0.65dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的原液着色蓝色聚酯纤维，其中，功能聚酯的压滤值DFFP为0.21kPa·cm 2/g。该原液着色蓝色聚酯纤维的单丝纤度为0.77dtex、断裂强度为3.4cN/dtex、断裂伸长率为33％。 When the intrinsic viscosity of the functional polyester reaches 0.65dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the stock solution whose base is polyethylene terephthalate is colored blue. Polyester fiber, wherein the functional polyester has a filter value DFFP of 0.21 kPa·cm 2 /g. The monofilament fineness of this dope-colored blue polyester fiber was 0.77 dtex, the breaking strength was 3.4 cN/dtex, and the elongation at break was 33%.
实施例2Example 2
S1,将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.13的聚酯低聚物浆料聚酯低聚物的原料浆以4613kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3931kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 265°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体浆料载体的原料浆以375kg/h的流量连续 均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为4.2kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到15mgKOH/g，通过由输送泵和流量计组成的载体计量输送单元以326.2kg/h的流量连续稳定地从载体制备反应釜采出。将炭黑浓度为20wt％的乙二醇基功能粉体预分散液以625kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的炭黑平均粒径为96nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以625kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.3. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 375 kg/h, concentration The flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.2 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 326.2 kg/h by the carrier metering and conveying unit composed of a conveying pump and a flow meter. The ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20% by weight is continuously and uniformly delivered at a flow rate of 625 kg/h to a functional powder dispersion preparation unit formed by three grinding machines connected in series, and prepared by grinding The functional powder dispersion with an average particle size of carbon black of 96nm enters the functional powder dispersion supply tank, and is continuously and stably transferred from the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter at a flow rate of 625kg/h Produced in the functional powder dispersion tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到炭黑平均粒径为110nm的功能粉体浆料，然后将功能粉体浆料以951.2kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到77mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以416.7kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中炭黑的含量为30wt％、压滤值DFMS为2.3kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 110 nm, and then the functional powder slurry The flow rate of 951.2kg/h is continuously and uniformly transported to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 77 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 416.7 kg/h Extracted from the feed concentration unit, the content of carbon black in the functional powder slurry concentrate is 30 wt%, and the pressure filtration value DFMS is 2.3 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.16dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。S3, the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit After entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.16dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
当功能聚酯特性粘度达到0.67dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的原液着色黑色聚酯纤维，其中，功能聚酯的压滤值DFFP为0.08kPa·cm 2/g。该原液着色黑色聚酯纤维的单丝纤度为0.77dtex、断裂强度为3.6cN/dtex、断裂伸长率为32％。 When the intrinsic viscosity of the functional polyester reaches 0.67dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw material colored polyethylene terephthalate base black colored polymer is prepared. Ester fiber, wherein the functional polyester has a filter value DFFP of 0.08 kPa·cm 2 /g. The monofilament fineness of this dope-colored black polyester fiber was 0.77 dtex, the breaking strength was 3.6 cN/dtex, and the breaking elongation was 32%.
实施例3Example 3
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.13的聚酯低聚物浆料聚酯低聚物的原料浆以4613kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3931kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 265°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.4的载体浆料载体的原料浆以391kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为4.3kg/h，载体制备釜的反应温度为250℃。当载体的酸值达到25mgKOH/g，通过由输送泵和流量计组成的载体计量输送单元以342.3kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.4. The raw material slurry of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 391 kg/h In the carrier preparation unit, the flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reaction kettle was 4.3 kg/h, and the reaction temperature of the carrier preparation kettle was 250°C. When the acid value of the carrier reaches 25 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 342.3 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
将抗菌剂氧化亚铜浓度为15wt％的乙二醇基功能粉体预分散液以494.5kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的抗菌剂氧化亚铜平均粒径为84nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以494.5kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with an antibacterial agent cuprous oxide concentration of 15% by weight is continuously and uniformly delivered at a flow rate of 494.5 kg/h to a functional powder dispersion preparation unit formed by three grinding machines connected in series, The functional powder dispersion liquid with an average particle size of 84 nm of the antibacterial agent cuprous oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 494.5 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到抗菌剂氧化亚铜平均粒径为92nm的功能粉体浆料，然后将功能粉体浆料以836.8kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到108mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以371kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中抗菌剂氧化亚铜的含量为20wt％、压滤值DFMS为4.8kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an antibacterial agent cuprous oxide functional particle size of 92nm, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 836.8 kg/h. The temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 108 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 371 kg/h. Extracted from the concentration unit, the content of the antibacterial agent cuprous oxide in the functional powder slurry concentrate is 20 wt%, and the filter press value DFMS is 4.8 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和卧式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.40dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.40dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 280°C.
当功能聚酯特性粘度达到0.72dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的抗菌聚酯纤维，其中，功能聚酯的压滤值DFFP为0.12kPa·cm 2/g。该抗菌聚酯纤维的单丝纤度为1.16dtex、断裂强度为4.2cN/dtex、断裂伸长率为33％。 When the intrinsic viscosity of the functional polyester reaches 0.72dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antibacterial polyester fiber with a polyethylene terephthalate matrix is obtained Among them, the press filter value DFFP of the functional polyester is 0.12 kPa·cm 2 /g. The antibacterial polyester fiber has a monofilament fineness of 1.16 dtex, a breaking strength of 4.2 cN/dtex, and an elongation at break of 33%.
实施例4Example 4
S1，将对苯二甲酸和丁二醇调配成的醇酸摩尔比为1.12的聚酯低聚物浆料聚酯低聚物的原料浆以4546kg/h的流量连续均匀的输送到由立式酯化反应釜组成的酯化反应系统中进行酯化反应，酯化反应釜的反应温度为240℃。浓度为20wt％的催化剂钛酸四丁酯溶液以53.6kg/h的流量连续均匀的注入到立式酯化反应釜中。当聚酯低聚物的酸值达到13mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3949kg/h的流量连续稳定地从酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and butylene glycol with an alkyd molar ratio of 1.12 is continuously and uniformly conveyed to the vertical type by the flow rate of 4546kg/h. An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 240°C. The catalyst tetrabutyl titanate solution with a concentration of 20 wt% was continuously and uniformly injected into the vertical esterification reactor at a flow rate of 53.6 kg/h. When the acid value of the polyester oligomer reaches 13 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and a oligomer flow meter continuously and stably withdraws from the esterification reactor at a flow rate of 3949 kg/h.
将对苯二甲酸和丁二醇调配成醇酸摩尔比为1.1的载体浆料载体的原料浆以144.1kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为20wt％的催化剂钛酸四丁酯溶液注入载体制备反应釜的流量为1.6kg/h，载体制备釜的反应温度为250℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以126.9kg/h的流量连续稳定地从载体制备反应釜采出。The terephthalic acid and butylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 1.1. The raw material carrier of the carrier is continuously and uniformly delivered to the carrier preparation unit composed of the carrier preparation reactor at a flow rate of 144.1 kg/h, the concentration is The flow rate of the 20 wt% catalyst tetrabutyl titanate solution injected into the carrier preparation reactor was 1.6 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 126.9 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将导热剂氮化铝浓度为60wt％的丁二醇基功能粉体预分散液以187.5kg/h的流量连续均匀的输送至由5台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的导热剂氮化铝平均粒径为147nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以187.5kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The butadiene glycol-based functional powder pre-dispersion with a thermal conductivity aluminum nitride concentration of 60wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 187.5kg/h. The functional powder dispersion liquid with an average particle size of 147 nm of the thermally conductive aluminum nitride prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 187.5 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
S2，载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到导热剂氮化铝平均粒径为163nm的功能粉体浆料，然后将功能粉体浆料以314.4kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到25mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以239.4kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中导热剂氮化铝的含量为50wt％、压滤值DFMS为8.4kPa·cm 2/g。 S2, the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit and are mixed uniformly to obtain a functional powder slurry with an average particle size of 163 nm as the thermal conductive agent aluminum nitride, and then the function The powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 314.4 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 25 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h Extracted from the material concentration unit, the content of the thermal conductive agent aluminum nitride in the functional powder slurry concentrate is 50 wt%, and the filter press value DFMS is 8.4 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为250℃。当功能聚酯预聚物特性粘度达到0.50dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为260℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 250°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.50 dL/g, it is continuously and stably extracted from the pre-condensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 260°C.
当功能聚酯特性粘度达到1.20dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸丁二醇酯的导热聚酯纤维，其中，功能聚酯的压滤值DFFP为0.28kPa·cm 2/g。该导热纤维的单丝纤度为1.54dtex、断裂强度为3.3cN/dtex、断裂伸长率为30％。 When the intrinsic viscosity of the functional polyester reaches 1.20dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to obtain a thermally conductive polyester fiber with a matrix of polybutylene terephthalate Among them, the press filter value DFFP of the functional polyester is 0.28 kPa·cm 2 /g. The monofilament fineness of this thermally conductive fiber was 1.54 dtex, the breaking strength was 3.3 cN/dtex, and the elongation at break was 30%.
实施例5Example 5
S1，将对苯二甲酸和丙二醇调配成醇酸摩尔比为1.4的聚酯低聚物浆料聚酯低聚物的原料浆以4958kg/h的流量连续均匀的输送到由立式第一酯化反应釜和卧式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为235℃，第二酯化反应釜反应温度240℃。浓度为10wt％的催化剂钛酸四异丙酯溶液以18.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到10mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以4326kg/h的流量连续稳定地从第 二酯化反应釜采出。S1, the terephthalic acid and propylene glycol are formulated into a polyester oligomer slurry with an alkyd molar ratio of 1.4. The raw material slurry of the polyester oligomer is continuously and uniformly delivered to the vertical first ester at a flow rate of 4958 kg/h. The esterification reaction system composed of a chemical reaction kettle and a horizontal second esterification reaction kettle performs an esterification reaction. The reaction temperature of the first esterification reaction kettle is 235°C, and the reaction temperature of the second esterification reaction kettle is 240°C. The catalyst tetraisopropyl titanate solution with a concentration of 10 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 18.8 kg/h. When the acid value of the polyester oligomer reaches 10 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4326 kg/h Out.
将对苯二甲酸和丙二醇调配成醇酸摩尔比为2.0的载体浆料载体的原料浆以667.8kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为10wt％的催化剂钛酸四异丙酯溶液注入载体制备反应釜的流量为2.2kg/h，载体制备釜的反应温度为230℃。当载体的酸值达到7mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以595.2kg/h的流量连续稳定地从载体制备反应釜采出。The terephthalic acid and propylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 2.0. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 667.8 kg/h, with a concentration of 10 wt% The flow rate of the catalyst tetraisopropyl titanate solution into the carrier preparation reactor was 2.2 kg/h, and the reaction temperature of the carrier preparation reactor was 230°C. When the acid value of the carrier reaches 7 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 595.2 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将荧光剂黄绿夜光粉(ZnS:Cu)浓度为10wt％的丙二醇基功能粉体预分散液以478.8kg/h的流量连续均匀的输送至由1台研磨机组成的功能粉体分散液制备单元，经过研磨制备得到的荧光剂黄绿夜光粉(ZnS:Cu)平均粒径为460nm的功能粉体分散液进入功能粉体分散液供应罐，通过由供应泵和流量计组成的功能粉体浆料输送计量单元以478.8kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。Propylene glycol-based functional powder pre-dispersion with a concentration of 10wt% of fluorescent agent yellow-green luminous powder (ZnS:Cu) was continuously and uniformly delivered to a functional powder dispersion composed of 1 grinder at a flow rate of 478.8kg/h Unit, the fluorescent powder yellow-green luminous powder (ZnS:Cu) prepared by grinding and the functional powder dispersion with an average particle size of 460nm enters the functional powder dispersion supply tank, through the functional powder composed of the supply pump and the flow meter The slurry conveying and metering unit continuously and stably withdraws from the functional powder dispersion liquid supply tank at a flow rate of 478.8 kg/h.
S2，载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到荧光剂黄绿夜光粉(ZnS:Cu)平均粒径为500nm的功能粉体浆料，然后将功能粉体浆料以1074kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为245℃。当功能粉体浆料浓缩物的羟值达到37mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以478.8kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中黄绿夜光粉(ZnS:Cu)的含量为10wt％、压滤值DFMS为19.8kPa·cm 2/g。 S2, the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit, and the phosphor yellow-green luminous powder (ZnS:Cu) with an average particle size of 500 nm is obtained after mixing uniformly The slurry, and then the functional powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1074 kg/h. The temperature of the evaporation unit is 245°C. When the hydroxyl value of the functional powder slurry concentrate reaches 37 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 478.8 kg/h Extracted from the material concentration unit, the content of the yellow-green luminous powder (ZnS:Cu) in the functional powder slurry concentrate is 10 wt%, and the filter press value DFMS is 19.8 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为255℃。当预聚物特性粘度达到0.5dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为260℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 255°C. When the intrinsic viscosity of the prepolymer reaches 0.5dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 260°C.
当终聚物特性粘度达到0.95dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸丙二醇酯的荧光聚酯纤维，其中功能聚酯的压滤值DFFP为0.66kPa·cm 2/g。该荧光聚酯纤维的单丝纤度为3.47dtex、断裂强度为2.8cN/dtex、断裂伸长率为27％。 When the intrinsic viscosity of the final polymer reaches 0.95dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the fluorescent polyester fiber with the matrix of polytrimethylene terephthalate is prepared. The filter press value DFFP of the functional polyester is 0.66 kPa·cm 2 /g. This fluorescent polyester fiber has a monofilament fineness of 3.47 dtex, a breaking strength of 2.8 cN/dtex, and an elongation at break of 27%.
实施例6Example 6
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为2.0的聚酯低聚物浆料聚酯低聚物的原料浆以5667kg/h的流量连续均匀的输送到由立式酯化反应釜组成的酯化反应系统中进行酯化反应，酯化反应釜反应温度为255℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到酯化反应釜中。当聚酯低聚物的酸值达到40mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以5021kg/h的流量连续稳定地从酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 2.0 is continuously and uniformly conveyed to the vertical type at a rate of 5667kg/h. An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 255°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 40 mgKOH/g, the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter is continuously and stably extracted from the esterification reactor at a flow rate of 5021 kg/h.
将对苯二甲酸和乙二醇调配成醇酸摩尔比为2.0的载体浆料载体的原料浆以617.7kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为5.9kg/h，载体制备釜的反应温度为250℃。当载体的酸值达到10mgKOH/g，通过输送泵和流量计组成的载体输送计量单元以548.5kg/h的流量连续稳定地从载体制备反应釜采出。The terephthalic acid and ethylene glycol are formulated into a carrier slurry with an alkyd molar ratio of 2.0. The raw material slurry of the carrier is continuously and uniformly delivered to the carrier preparation unit composed of the carrier preparation reactor at a flow rate of 617.7 kg/h, the concentration is The flow rate of the 3 wt% catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 5.9 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C. When the acid value of the carrier reaches 10 mgKOH/g, the carrier delivery metering unit composed of a delivery pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 548.5 kg/h.
将远红外剂碳化锆浓度为20wt％的乙二醇基功能粉体预分散液以511.4kg/h的流量连续均匀的输送至由2台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的远红外剂碳化锆平均粒径为112nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以511.4kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a far-infrared agent zirconium carbide concentration of 20 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by two grinding machines in series at a flow rate of 511.4 kg/h. The far-infrared agent zirconium carbide prepared by grinding the functional powder dispersion with an average particle size of 112nm enters the functional powder dispersion supply tank, and the functional powder dispersion consisting of a delivery pump and a flow meter is transported to a metering unit of 511.4kg The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
S2，载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到远红外剂碳化锆平均粒径为129nm的功能粉体浆料，然后将功能粉体浆料以1059.9kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到160mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以511.4kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中远红外剂碳化锆的含量为20wt％、压滤值DFMS为5.4kPa·cm 2/g。 S2, the carrier and the functional powder dispersion enter the functional powder dispersion composed of a shear pump and the carrier mixing unit and are mixed uniformly to obtain a far-infrared agent zirconium carbide functional powder slurry with an average particle size of 129 nm, and then the function The powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1059.9 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 160 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 511.4 kg/h. Extracted from the feed concentration unit, the content of the far-infrared agent zirconium carbide in the functional powder slurry concentrate is 20 wt%, and the filter press value DFMS is 5.4 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为290℃。当预聚物特性粘度达到0.30dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为285℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the reactant temperature of the pre-condensation reactor is 290°C. When the intrinsic viscosity of the prepolymer reaches 0.30dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 285°C.
当终聚物特性粘度达到0.50dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的远红外聚酯纤维，其中功能聚酯的压滤值DFFP为0.14kPa·cm 2/g。该远红外聚酯纤维的单丝纤度为2.31dtex、断裂强度为3.2cN/dtex、断裂伸长率为31％。 When the intrinsic viscosity of the final polymer reaches 0.50dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the far-infrared polyester whose base is polyethylene terephthalate is prepared. Fiber, in which the functional polyester has a filter value DFFP of 0.14 kPa·cm 2 /g. This far infrared polyester fiber has a monofilament fineness of 2.31 dtex, a breaking strength of 3.2 cN/dtex, and an elongation at break of 31%.
实施例7Example 7
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.05的聚酯低聚物浆料聚酯低聚物的原料浆以4516kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为270℃，第二酯化反应釜反应温度280℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到20mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3841kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.05 is continuously and uniformly conveyed to the vertical type by the flow rate of 4516 kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 270°C, and the reaction temperature of the second esterification reactor is 280°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 20 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3841 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体浆料载体的原料浆以1004.6kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为11.3kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以875.3kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.3. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 1004.6 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 11.3 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 875.3 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将防紫外辐射剂氧化锌浓度为10wt％的乙二醇基功能粉体预分散液以411.5kg/h的流量连续均匀的输送至由2台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的防紫外辐射剂氧化锌平均粒径为340nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以411.5kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with an anti-ultraviolet radiation agent zinc oxide concentration of 10 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by two grinding machines in series at a flow rate of 411.5 kg/h The functional powder dispersion liquid with an average particle size of 340 nm of zinc oxide, an anti-ultraviolet radiation agent prepared by grinding, enters the functional powder dispersion liquid supply tank, and is transported to the metering unit by the functional powder dispersion liquid composed of a delivery pump and a flow meter. The flow rate of 411.5kg/h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到防紫外辐射剂氧化锌平均粒径为362nm的功能粉体浆料，然后将功能粉体浆料以1286.8kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到63mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以823kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中防紫外辐射剂氧化锌的含量为5wt％、压滤值DFMS为10.2kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 362 nm of the anti-UV radiation agent zinc oxide, and then the functional powder The bulk slurry is continuously and uniformly delivered to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1286.8 kg/h. The temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 63 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 823 kg/h The content of the functional powder slurry concentrate, which was extracted from the concentration unit, was 5 wt% of the anti-ultraviolet radiation agent zinc oxide, and the filter press value DFMS was 10.2 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和卧式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为275℃、第二预缩聚反应釜的反应物温度为280℃。当预聚物特性粘度达到0.38dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为285℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 275°C and the reactant temperature of the second precondensation reaction kettle is 280℃. When the intrinsic viscosity of the prepolymer reaches 0.38dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 285°C.
S3，当终聚物特性粘度达到0.62dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的防辐射聚酯纤维，其中功能聚酯的压滤值DFFP为0.25kPa·cm 2/g。该防辐射聚酯纤维的单丝纤度为2.31dtex、断裂强度为3.0cN/dtex、断裂伸长率为31％。 S3, when the intrinsic viscosity of the final polymer reaches 0.62dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the radiation protection matrix of the polyethylene terephthalate is obtained. Polyester fiber, where the functional polyester has a filter value DFFP of 0.25 kPa·cm 2 /g. The monofilament fineness of this radiation-proof polyester fiber was 2.31 dtex, the breaking strength was 3.0 cN/dtex, and the elongation at break was 31%.
实施例8Example 8
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.05的聚酯低聚物浆料聚酯低聚物的原料浆以4516kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为270℃，第二酯化反应釜反应温度280℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到 25mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3848kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.05 is continuously and uniformly conveyed to the vertical type by the flow rate of 4516 kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 270°C, and the reaction temperature of the second esterification reactor is 280°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 25 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3848 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.6的载体浆料载体的原料浆以731.8kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为7.7kg/h，载体制备釜的反应温度为250℃。当载体的酸值达到15mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以643.2kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.6. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 731.8 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 7.7 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C. When the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 643.2 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将导电剂氧化锡锑浓度为20wt％的乙二醇基功能粉体预分散液以661.8kg/h的流量连续均匀的输送至由5台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的导电剂氧化锡锑平均粒径为68nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以661.8kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a concentration of tin oxide and antimony oxide of 20 wt% is continuously and uniformly delivered to the functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 661.8 kg/h. The functional powder dispersion liquid with an average particle diameter of 68 nm of the conductive agent tin antimony oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and the functional powder dispersion liquid composed of a delivery pump and a flow meter is transported to a metering unit of 661.8 kg The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到防紫外辐射剂氧化锌平均粒径为80nm的功能粉体浆料，然后将功能粉体浆料以1305kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到88mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以661.8kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中导电剂氧化锡锑的含量为20wt％、压滤值DFMS为2.2kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 80 nm of the anti-UV radiation agent zinc oxide, and then the functional powder The bulk slurry is continuously and uniformly delivered to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1305 kg/h. The temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 88 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 661.8 kg/h. It was collected in the material concentration unit, and the content of the conductive agent tin antimony oxide in the functional powder slurry concentrate was 20 wt%, and the filter press value DFMS was 2.2 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和卧式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为280℃、第二预缩聚反应釜的反应物温度为285℃。当功能聚酯预聚物特性粘度达到0.50dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为300℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a horizontal second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 280°C and the reactant temperature of the second precondensation reaction kettle is 285℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.50 dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 300°C.
当功能聚酯特性粘度达到0.80dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的抗静电聚酯纤维，其中，功能聚酯的压滤值DFFP为0.07kPa·cm 2/g。该抗静电聚酯纤维的单丝纤度为1.16dtex、断裂强度为6.2cN/dtex、断裂伸长率为28％。 When the intrinsic viscosity of the functional polyester reaches 0.80dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antistatic polyester whose base is polyethylene terephthalate is obtained. For the fiber, the press-filtration value DFFP of the functional polyester is 0.07 kPa·cm 2 /g. The antistatic polyester fiber had a monofilament fineness of 1.16 dtex, a breaking strength of 6.2 cN/dtex, and an elongation at break of 28%.
实施例9Example 9
S1，将对苯二甲酸和丁二醇调配成的醇酸摩尔比为1.12的聚酯低聚物浆料聚酯低聚物的原料浆以4546kg/h的流量连续均匀的输送到由立式酯化反应釜组成的酯化反应系统中进行酯化反应，酯化反应釜的反应温度为240℃。浓度为20wt％的催化剂钛酸四丁酯溶液以53.6kg/h的流量连续均匀的注入到立式酯化反应釜中。当聚酯低聚物的酸值达到13mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3949kg/h的流量连续稳定地从酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and butylene glycol with an alkyd molar ratio of 1.12 is continuously and uniformly conveyed to the vertical type by the flow rate of 4546kg/h. An esterification reaction system composed of an esterification reaction kettle performs an esterification reaction, and the reaction temperature of the esterification reaction kettle is 240°C. The catalyst tetrabutyl titanate solution with a concentration of 20 wt% was continuously and uniformly injected into the vertical esterification reactor at a flow rate of 53.6 kg/h. When the acid value of the polyester oligomer reaches 13 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and a oligomer flow meter continuously and stably withdraws from the esterification reactor at a flow rate of 3949 kg/h.
S2，将对苯二甲酸和丁二醇调配成醇酸摩尔比为1.2的载体浆料载体的原料浆以233.5kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为20wt％的催化剂钛酸四丁酯溶液注入载体制备反应釜的流量为2.7kg/h，载体制备釜的反应温度为250℃。当载体的酸值达到10mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以206.1kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and butylene glycol into a carrier slurry with an alkyd molar ratio of 1.2. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 233.5 kg/h. The flow rate of the catalyst tetrabutyl titanate solution with a concentration of 20 wt% injected into the carrier preparation reactor was 2.7 kg/h, and the reaction temperature of the carrier preparation reactor was 250°C. When the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reaction kettle at a flow rate of 206.1 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将负离子发生剂电气石浓度为30wt％的丁二醇基功能粉体预分散液以267.9kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的负离子发生剂电气石平均粒径为189nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以267.9kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The butanediol-based functional powder pre-dispersion with a concentration of 30% by weight of anion generator tourmaline is continuously and uniformly delivered to the functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 267.9 kg/h. The functional powder dispersion liquid with an average particle size of 189 nm, which is an anion generator tourmaline prepared by grinding, enters the functional powder dispersion liquid supply tank, and is transported to a metering unit of 267.9 kg through the functional powder dispersion liquid composed of a delivery pump and a flow meter The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到负离子发生剂电气石平均粒径为194nm的功能粉体浆料，然后将功能粉体浆料以474kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到56mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以 267.9kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中负离子发生剂电气石的含量为30wt％、压滤值DFMS为15.5kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit and are uniformly mixed to obtain a functional powder slurry with an average particle size of 194 nm, an anion generator tourmaline, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 474 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 56 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 267.9 kg/h The content of the negative ion generator tourmaline in the functional powder slurry concentrate is 30 wt% and the filter press value DFMS is 15.5 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为250℃。当功能聚酯预聚物特性粘度达到0.40dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为250℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The pre-condensation reaction system consists of a vertical pre-condensation reaction kettle, in which the temperature of the reactants in the pre-condensation reaction kettle is 250°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.40dL/g, it is continuously and stably extracted from the pre-condensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 250°C.
当功能聚酯特性粘度达到1.00dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸丁二醇酯的负离子聚酯纤维，其中，功能聚酯的压滤值DFFP为0.51kPa·cm 2/g。该负离子纤维的单丝纤度为2.31dtex、断裂强度为3.1cN/dtex、断裂伸长率为26％。 When the intrinsic viscosity of the functional polyester reaches 1.00dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the negative ion polyester fiber whose base is polybutylene terephthalate is prepared. Among them, the press filter value DFFP of the functional polyester is 0.51 kPa·cm 2 /g. The monofilament fineness of this negative ion fiber was 2.31 dtex, the breaking strength was 3.1 cN/dtex, and the breaking elongation was 26%.
实施例10Example 10
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与低熔点共聚改性单体间苯二甲酸浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.12调配而成、低熔点共聚改性单体间苯二甲酸浆料由间苯二甲酸与乙二醇以醇酸摩尔比1.12调配而成。对苯二甲酸浆料以2760kg/h的流量、低熔点共聚改性单体间苯二甲酸浆料以1841kg/h的流量同时连续均匀的输送至由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统的立式第一酯化反应釜中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3919kg/h的流量连续稳定地从第二酯化反应釜采出。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and low melting point copolymer modified monomer isophthalic acid slurry, wherein the terephthalic acid slurry is composed of p-benzene The dicarboxylic acid and ethylene glycol are formulated with an alkyd molar ratio of 1.12, and the low melting point copolymer modified monomer isophthalic acid slurry is prepared from isophthalic acid and ethylene glycol with an alkyd molar ratio of 1.12. The terephthalic acid slurry with a flow rate of 2760kg/h and the low melting point copolymer modified monomer isophthalic acid slurry with a flow rate of 1841kg/h are continuously and uniformly delivered to the vertical first esterification reactor and the vertical The esterification reaction system of the esterification reaction system composed of the second esterification reaction kettle performs an esterification reaction in the vertical first esterification reaction kettle. The reaction temperature of the first esterification reaction kettle is 260°C, and the reaction temperature of the second esterification reaction kettle is 265°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer delivery and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3919 kg/h Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为2.0的载体浆料载体的原料浆以119.3kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为1.1kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到10mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以106kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 2.0. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 119.3 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 1.1 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 106 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将颜料红254浓度为60wt％的乙二醇基功能粉体预分散液以197.4kg/h的流量连续均匀的输送至由2台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的颜料红254平均粒径为294nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以197.4kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a pigment red 254 concentration of 60% by weight is continuously and uniformly delivered at a flow rate of 197.4 kg/h to a functional powder dispersion preparation unit composed of two grinding machines connected in series, after grinding The prepared functional powder dispersion with an average particle size of 294 nm in Pigment Red 254 enters the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 197.4 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到颜料红254平均粒径为300nm的功能粉体浆料，然后将功能粉体浆料以303.4kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到70mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以197.4kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中颜料红254的含量为60wt％、压滤值DFMS为9.3kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with a pigment red 254 average particle size of 300 nm, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 303.4 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 70 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 197.4 kg/h Extracted from the material concentration unit, the content of pigment red 254 in the functional powder slurry concentrate is 60 wt%, and the filter press value DFMS is 9.3 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为265℃、第二预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.22dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, where the reactant temperature of the first precondensation reaction kettle is 265°C and the reactant temperature of the second precondensation reaction kettle is 270℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.22dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
当功能聚酯特性粘度达到0.74dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为低熔点共聚酯的原液着色红色低熔点聚酯纤维，其中，功能聚酯的压滤值DFFP为0.23kPa·cm 2/g。该原液着色红色低熔点聚酯纤维单丝纤度为1.54dtex、断裂强度为2.8cN/dtex、断裂伸长率为36％。 When the intrinsic viscosity of the functional polyester reaches 0.74dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw liquid colored low-melting polyester fiber whose matrix is a low-melting point copolyester is prepared. Among them, the press filter value DFFP of the functional polyester is 0.23 kPa·cm 2 /g. The stock solution colored red low-melting polyester fiber monofilament fineness was 1.54 dtex, breaking strength was 2.8 cN/dtex, and breaking elongation was 36%.
实施例11Example 11
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与高收缩共聚改性单体新戊二醇浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.05调配而成、高收缩共聚改性单体新戊二醇浆料由新戊二醇与乙二醇以重量比8:2调配而成。对苯二甲酸浆料以4516kg/h的流量、高收缩共聚改性单体新戊二醇浆料以152.5kg/h的流量同时连续均匀的输送至由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统的立式第一酯化反应釜中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3987kg/h的流量连续稳定地从第二酯化反应釜采出。S1, Polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and high shrink copolymerization modified monomer neopentyl glycol slurry, wherein the terephthalic acid slurry is composed of p-benzene The dicarboxylic acid and ethylene glycol are formulated with an alkyd molar ratio of 1.05, and the high shrinkage copolymer modified monomer neopentyl glycol slurry is formulated with neopentyl glycol and ethylene glycol at a weight ratio of 8:2. The terephthalic acid slurry with a flow rate of 4516kg/h and the high shrinkage copolymerization modified monomer neopentyl glycol slurry with a flow rate of 152.5kg/h are continuously and uniformly delivered to the vertical first esterification reactor and the vertical The esterification reaction system of the esterification reaction system composed of the second esterification reaction kettle performs esterification reaction in the vertical first esterification reaction kettle, the reaction temperature of the first esterification reaction kettle is 260°C, and the reaction temperature of the second esterification reaction kettle is 265°C . The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3987kg/h Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.4的载体浆料载体的原料浆以189.2kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为2.1kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以165.5kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.4. The raw material slurry of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 189.2 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 2.1 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 165.5 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将颜料蓝15:3浓度为40wt％的乙二醇基功能粉体预分散液以239.4kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到颜料蓝15:3平均粒径为143nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以239.4kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The pigment blue 15:3 concentration 40wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered at a flow rate of 239.4kg/h to a functional powder dispersion preparation unit made up of 3 grinders in series, After preparation, the functional powder dispersion liquid with pigment blue 15:3 with an average particle size of 143 nm is fed into the functional powder dispersion liquid supply tank, and the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter is 239.4 kg/ The flow rate of h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到颜料蓝15:3平均粒径为154nm的功能粉体浆料，然后将功能粉体浆料以404.9kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到42mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以239.4kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中颜料蓝15:3的含量为40wt％、压滤值DFMS为7.8kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a pigment blue 15:3 functional powder slurry with an average particle size of 154 nm, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 404.9 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 42 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h Extracted from the feed concentration unit, the content of the pigment blue 15:3 in the functional powder slurry concentrate is 40 wt%, and the filter press value DFMS is 7.8 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为265℃、第二预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.20dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, where the reactant temperature of the first precondensation reaction kettle is 265°C and the reactant temperature of the second precondensation reaction kettle is 270℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.20dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
当功能聚酯特性粘度达到0.72dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为高收缩共聚酯的原液着色蓝色高收缩聚酯纤维，其中，功能聚酯的压滤值DFFP为0.26kPa·cm 2/g。该原液着色蓝色高收缩聚酯纤维单丝纤度为1.16dtex、断裂强度为3.6cN/dtex、断裂伸长率为34％。 When the intrinsic viscosity of the functional polyester reaches 0.72dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the raw liquid colored blue high-shrink polyester with the matrix of high-shrink copolyester is obtained The fiber, in which the filter press value DFFP of the functional polyester is 0.26 kPa·cm 2 /g. The stock solution colored blue high shrinkage polyester fiber monofilament fineness was 1.16 dtex, the breaking strength was 3.6 cN/dtex, and the breaking elongation was 34%.
实施例12Example 12
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与阳离子染料可染共聚改性单体间苯二甲酸二乙二醇酯-5-磺酸钠浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.15调配而成、阳离子染料可染共聚改性单体间苯二甲酸二乙二醇酯-5-磺酸钠浆料由间苯二甲酸二乙二醇酯-5-磺酸钠与乙二醇以重量比4:6调配而成。酯化反应系统由立式第一酯化反应釜和卧室卧式三分室结构第二酯化反应釜组成，对苯二甲酸浆料以4637kg/h的流量连续均匀的输送至立式第一酯化反应釜、阳离子染料可染共聚改性单体间苯二甲酸二乙二醇酯-5-磺酸钠浆料以260.7kg/h的流量连续均匀的注入卧室卧式第二酯化反应釜的第二室、浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到卧式第二酯化反应釜的第三室。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and cationic dye-dyeable copolymerizable modified monomer diethylene glycol isophthalate-5-sulfonate sodium slurry The composition is composed of terephthalic acid slurry made from terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.15. The cationic dye can be dyed and copolymerized to modify the monomer diethylene glycol isophthalate-5- The sodium sulfonate slurry is prepared from diethylene glycol isophthalate-5-sodium sulfonate and ethylene glycol at a weight ratio of 4:6. The esterification reaction system is composed of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4637kg/h Chemical reactor, cationic dye-dyeable copolymerized modified monomer diethylene glycol isophthalate-5-sulfonate sodium slurry was continuously and uniformly injected into the bedroom horizontal second esterification reactor at a flow rate of 260.7 kg/h The second chamber and the catalyst ethylene glycol antimony solution with a concentration of 3% by weight are continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 54.8 kg/h.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体浆料载体的原料浆以375.1kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为4.2kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以326.7kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.3. The raw material slurry of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 375.1 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 4.2 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 326.7 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将消光剂二氧化钛浓度为40wt％的乙二醇基功能粉体预分散液以312.5kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的消光剂二氧化钛平均粒径为62nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以312.5kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a matting agent titanium dioxide concentration of 40% by weight is continuously and uniformly delivered at a flow rate of 312.5 kg/h to a functional powder dispersion preparation unit composed of three grinding machines connected in series, after grinding The prepared functional powder dispersion with an average particle size of 62 nm of the matting agent titanium dioxide enters the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 312.5 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到消光剂二氧化钛平均粒径为68nm的功能粉体浆料，然后将功能粉体浆料以639.2kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为280℃。The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 68 nm of the matting agent titanium dioxide, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 639.2 kg/h. The temperature of the evaporation unit is 280°C.
S3，当功能粉体浆料浓缩物的羟值达到40mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以416.7kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出直接输送至卧式第二酯化反应釜的第三室，功能粉体浆料浓缩物中消光剂二氧化钛的含量为30wt％、压滤值DFMS为1.2kPa·cm 2/g。第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度250℃。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以4701kg/h的流量连续稳定地从第二酯化反应釜采出。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.10dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。 S3, when the hydroxyl value of the functional powder slurry concentrate reaches 40 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder at a flow rate of 416.7 kg/h The bulk slurry concentration unit extracts directly to the third chamber of the horizontal second esterification reactor, the content of the matting agent titanium dioxide in the functional powder slurry concentrate is 30wt%, and the filter press value DFMS is 1.2kPa·cm 2 /g. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 250°C. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4701 kg/h. Out. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.10 dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
当功能聚酯特性粘度达到0.60dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为阳离子染料可染共聚酯的全消光阳离子染料可染聚酯纤维，其中，功能聚酯的压滤值DFFP为0.04kPa·cm 2/g。该全消光阳离子染料可染聚酯纤维单丝纤度为1.16dtex、断裂强度为3.3cN/dtex、断裂伸长率为35％。 When the intrinsic viscosity of the functional polyester reaches 0.60dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the fully extinct cationic dyeable dyeable copolyester whose matrix is the cationic dyeable dyeable is prepared. Polyester fiber, wherein the functional polyester has a filter value DFFP of 0.04 kPa·cm 2 /g. The total extinction cationic dyeable polyester fiber monofilament fineness is 1.16 dtex, breaking strength is 3.3 cN/dtex, and breaking elongation is 35%.
实施例13Example 13
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与分散染料常压可染共聚改性单体己二酸二乙二醇酯浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.08调配而成、分散染料常压可染共聚改性单体己二酸二乙二醇酯浆料由己二酸二乙二醇酯与乙二醇以重量比6:4调配而成。酯化反应系统由立式第一酯化反应釜和卧室卧式三分室结构第二酯化反应釜组成，对苯二甲酸浆料以4098kg/h的流量连续均匀的输送至立式第一酯化反应釜、分散染料常压可染共聚改性单体己二酸二乙二醇酯浆料以761.5kg/h的流量连续均匀的注入卧室卧式第二酯化反应釜的第二室、浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到卧式第二酯化反应釜的第三室。第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度250℃。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以4232kg/h的流量连续稳定地从第二酯化反应釜采出。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and disperse dye at atmospheric pressure copolymerizable modified monomer diethylene glycol adipate slurry, of which Phthalic acid slurry is prepared from terephthalic acid and ethylene glycol at an alkyd molar ratio of 1.08. Disperse dyes can be dyed at atmospheric pressure. Copolymerized modified monomer diethylene glycol adipate slurry is made from diethyl adipate Glycol ester and ethylene glycol are formulated at a weight ratio of 6:4. The esterification reaction system consists of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4098kg/h Chemical reactor, disperse dyes, atmospheric pressure dyeable copolymerization modified monomer diethylene glycol adipate slurry was continuously and uniformly injected into the second chamber of the bedroom horizontal second esterification reactor at a flow rate of 761.5 kg/h, The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 54.8 kg/h. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 250°C. When the acid value of the polyester oligomer reaches 15mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4232kg/h Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体浆料载体的原料浆以450.6kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为5.1kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以392.6kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.3. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 450.6 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 5.1 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 392.6 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将防紫外辐射剂掺铝氧化锌浓度为15wt％的乙二醇基功能粉体预分散液以412.5kg/h的流量连续均匀的输送至由4台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的防紫外辐射剂掺铝氧化锌平均粒径为82nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以412.5kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The anti-ultraviolet radiation agent-doped aluminum oxide-based zinc oxide functional powder pre-dispersion with a concentration of 15wt% was continuously and uniformly delivered to the functional powder dispersion formed by 4 grinding machines in series at a flow rate of 412.5kg/h In the preparation unit, the functional powder dispersion liquid with an average particle diameter of 82 nm of the aluminum oxide-doped zinc oxide prepared by grinding and entering the functional powder dispersion liquid supply tank passes through the functional powder dispersion liquid composed of a delivery pump and a flowmeter The conveying and metering unit continuously and stably withdraws from the functional powder dispersion liquid supply tank at a flow rate of 412.5 kg/h.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到防紫外辐射剂掺铝氧化锌平均粒径为94nm的功能粉体浆料，然后将功能粉体浆料以805.1kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为275℃。当功能粉体浆料浓缩物的羟值达到53mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以412.5kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中防紫外辐射剂掺铝氧化锌的含量为15wt％、压滤值DFMS为2.9kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an anti-ultraviolet radiation agent aluminum-doped zinc oxide average particle size of 94 nm, and then the functional powder slurry The functional powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 805.1 kg/h. The temperature of the evaporation unit is 275°C. When the hydroxyl value of the functional powder slurry concentrate reaches 53 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 412.5 kg/h Extracted from the material concentration unit, the content of the anti-ultraviolet radiation agent aluminum-doped zinc oxide in the functional powder slurry concentrate is 15 wt%, and the filter press value DFMS is 2.9 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.19dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。S3. The polyester oligomer from the esterification reaction system enters the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system, and is evenly mixed by the mixing unit Entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.19dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C.
当功能聚酯特性粘度达到0.72dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为分散染料常压可染共聚酯的防紫外辐射分散染料常压可染聚酯纤维，其中，功能聚酯的压滤值DFFP为0.10kPa·cm 2/g。该防紫外辐射分散染料常压可染聚酯纤维单丝纤度为1.16dtex、断裂强度为3.6cN/dtex、断裂伸长率为32％。 When the intrinsic viscosity of the functional polyester reaches 0.72dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the anti-ultraviolet radiation dispersion of the matrix of the disperse dye at atmospheric pressure and co-polyester can be obtained Dyestuff can be dyed with polyester at normal pressure. Among them, the functional polyester has a filter value of DFFP of 0.10 kPa·cm 2 /g. The anti-ultraviolet radiation disperse dye normal pressure dyeable polyester fiber monofilament fineness is 1.16 dtex, breaking strength is 3.6 cN/dtex, and breaking elongation is 32%.
实施例14Example 14
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与仿棉共聚改性单体聚酰胺浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.12调配而成、仿棉共聚改性单体聚酰胺浆料由聚酰胺在230℃熔融调配而成。酯化反应系统由立式第一酯化反应釜、立式第二酯化反应釜组成，对苯二甲酸浆料以4141kg/h的流量连续均匀的输送至立式第一酯化反应釜、浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到立式第二酯化釜。第一酯化反应釜反应温度为260℃、第二酯化反应釜反应温度265℃。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3582kg/h的流量连续稳定地从第二酯化反应釜采出。仿棉共聚改性单体聚酰胺浆料经聚酯低聚物管线在线添加系统以375kg/h直接注入第二酯化釜后的聚酯低聚物管道中。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and cotton-like copolymerized modified monomer polyamide slurry, in which terephthalic acid slurry is composed of terephthalic acid It is blended with ethylene glycol at an alkyd molar ratio of 1.12, and the cotton-like copolymerized modified monomer polyamide slurry is prepared by melt blending polyamide at 230°C. The esterification reaction system consists of a vertical first esterification reactor and a vertical second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first esterification reactor at a flow rate of 4141 kg/h. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the vertical second esterification kettle at a flow rate of 54.8 kg/h. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 265°C. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3582 kg/h. Out. The cotton-like copolymerized modified monomer polyamide slurry is directly injected into the polyester oligomer pipe after the second esterification kettle at 375 kg/h through the polyester oligomer pipeline online addition system.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.5的载体浆料载体的原料浆以252.9kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为2.7kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到15mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以221.5kg/h的流量连续稳定地从载体制备反应釜采出。S2, blending terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.5. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 252.9 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 2.7 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 15 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 221.5 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将抗菌剂掺铜氧化锌浓度为30wt％的乙二醇基功能粉体预分散液以267.9kg/h的流量连续均匀的输送至由5台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的抗菌剂掺铜氧化锌平均粒径为99nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以267.9kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The antibacterial agent copper-doped zinc oxide concentration 30wt% ethylene glycol-based functional powder pre-dispersion was continuously and uniformly delivered to the functional powder dispersion preparation unit made up of 5 grinding machines in series at a flow rate of 267.9kg/h ，The antibacterial agent prepared by grinding and the copper-doped zinc oxide functional powder dispersion with an average particle size of 99nm enters into the functional powder dispersion supply tank, and is transported to the metering unit through the functional powder dispersion composed of a delivery pump and a flow meter. The flow rate of 267.9kg/h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到抗菌剂掺铜氧化锌平均粒径为107nm的功能粉体浆料，然后将功能粉体浆料以489.4kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到73mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以267.9kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出。功能粉体浆料浓缩物中抗菌剂掺铜氧化锌的含量为30wt％、压滤值DFMS为3.4kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an antibacterial agent copper-doped zinc oxide functional powder slurry with an average particle size of 107 nm, and then the functional powder The bulk slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 489.4 kg/h. The temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 73 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 267.9 kg/h Produced in the material concentration unit. The content of the antibacterial agent copper-doped zinc oxide in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 3.4 kPa·cm 2 /g.
S3，来自聚酯低聚物管道的聚酯低聚物和仿棉共聚改性单体聚酰胺浆料的共混物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为260℃、第二预缩聚反应釜的反应物温度为265℃。当功能聚酯预聚物特性粘度达到0.20dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为270℃。S3, blend of polyester oligomer from polyester oligomer pipeline and cotton-like copolymerization modified monomer polyamide slurry and functional powder slurry concentrate from functional powder slurry concentrate preparation system It enters into the functional powder slurry concentrate mixing unit together, enters into the pre-condensation reaction system after being evenly mixed by the mixing unit, and the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 260°C and the reactant temperature of the second precondensation reaction kettle is 265℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.20dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 270°C.
当功能聚酯特性粘度达到0.68dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为仿棉共聚酯的抗菌仿棉聚酯纤维，其中，功能聚酯的压滤值DFFP为0.12kPa·cm 2/g。该抗菌仿棉聚酯纤维单丝纤度为1.16dtex、断裂强度为3.3cN/dtex、断裂伸长率为29％。 When the intrinsic viscosity of the functional polyester reaches 0.68dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antibacterial cotton-like polyester fiber whose base is cotton-like copolyester is prepared. , The filter press value DFFP of the functional polyester is 0.12 kPa·cm 2 /g. The antibacterial cotton-like polyester fiber monofilament has a fineness of 1.16 dtex, a breaking strength of 3.3 cN/dtex, and an elongation at break of 29%.
实施例15Example 15
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.12调配而成、阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料由2-羧乙基苯基次磷酸二乙二醇酯与乙二醇以重量比4:6调配而成。酯化反应系统由立式第一酯化反应釜和立式第二酯化反应釜组成，对苯二甲酸浆料以4394kg/h的流量连续均匀的输送至酯化系统的立式第一酯化反应釜、浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到立式第二酯化反应釜。第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度270℃。当聚酯低聚物的酸值达到10mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3804kg/h的流量连续稳定地从第二酯化反应釜采出。阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料经聚酯低聚物管道在线添加系统以595.5kg/h的流量直接注入第二酯化釜后的聚酯低聚物管道中。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and flame retardant copolymerized modified monomer 2-carboxyethylphenyl hypophosphite diethylene glycol slurry, Among them, the terephthalic acid slurry is prepared from terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.12, and the flame retardant copolymer modified monomer 2-carboxyethyl phenyl hypophosphite diethylene glycol slurry is composed of 2-Carboxyethyl phenyl hypophosphite diethylene glycol and ethylene glycol are formulated at a weight ratio of 4:6. The esterification reaction system is composed of a vertical first esterification reactor and a vertical second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester of the esterification system at a flow rate of 4394kg/h The reaction reactor and the catalyst ethylene glycol antimony solution with a concentration of 3 wt% were continuously and uniformly injected into the vertical second esterification reactor at a flow rate of 54.8 kg/h. The reaction temperature of the first esterification reactor was 260°C, and the reaction temperature of the second esterification reactor was 270°C. When the acid value of the polyester oligomer reaches 10 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3804 kg/h. Out. The flame retardant copolymer modified monomer 2-carboxyethylphenyl diphosphite hypoglycol ester slurry was directly injected into the second esterification kettle at a flow rate of 595.5kg/h through the online addition system of the polyester oligomer pipeline. Ester oligomer pipeline.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.3的载体浆料载体的原料浆以313.2kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为3.5kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以272.8kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.3. The raw material slurry of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 313.2 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor is 3.5 kg/h, and the reaction temperature of the carrier preparation reactor is 260°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 272.8 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将远红外剂碳化钛浓度为20wt％的乙二醇基功能粉体预分散液以304kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的远红外剂碳化钛平均粒径为135nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以304kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a far-infrared agent titanium carbide concentration of 20 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 304 kg/h. The functional powder dispersion of the far-infrared agent titanium carbide with an average particle size of 135 nm prepared by grinding enters the functional powder dispersion supply tank, and is transported to the metering unit by a functional powder dispersion composed of a delivery pump and a flow meter at 304 kg/h The flow rate is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到远红外剂碳化钛平均粒径为147nm的功能粉体浆料，然后将功能粉体浆料以576.8kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到30mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以304kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出。功能粉体浆料浓缩物中远红外剂碳化钛的含量为20wt％、压滤值DFMS为5.2kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of 147 nm of the far-infrared agent titanium carbide, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 576.8 kg/h. The temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 30 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 304 kg/h Produced in the concentration unit. The content of the far-infrared agent titanium carbide in the functional powder slurry concentrate is 20 wt%, and the pressure filtration value DFMS is 5.2 kPa·cm 2 /g.
S3，来自聚酯低聚物管道的聚酯低聚物和阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料的共混物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.18dL/g，通过预聚物泵连续稳定地从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。S3, blend of polyester oligomer from polyester oligomer pipeline and flame retardant copolymer modified monomer 2-carboxyethyl phenyl hypophosphite diethylene glycol slurry with functional powder slurry The functional powder slurry concentrate of the concentrate preparation system enters the functional powder slurry concentrate mixing unit together, and after being uniformly mixed by the mixing unit, it enters the pre-condensation reaction system. The mixing unit is a high-shear pump. The pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.18dL/g, it is continuously and stably extracted from the pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
当功能聚酯终聚物特性粘度达到0.62dL/g，通过终聚物泵连续稳定地从终缩聚反应釜采出并输送至液相增粘反应釜进行液相增粘，液相增粘反应釜的反应温度为285℃。When the intrinsic viscosity of the functional polyester final polymer reaches 0.62dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening, liquid-phase thickening reaction The reaction temperature of the kettle was 285°C.
当功能聚酯增粘物特性粘度达到0.72dL/g，将功能聚酯增粘熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为阻燃共聚酯的远红外阻燃聚酯纤维，其中，功能聚酯的压滤值DFFP为0.17kPa·cm 2/g。该远红外阻燃聚酯纤维单丝纤度为1.54dtex、断裂强度为3.5cN/dtex、断裂伸长率为32％。 When the intrinsic viscosity of the functional polyester tackifier reaches 0.72dL/g, the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the far-infrared resistance of the flame retardant copolyester is obtained. Burning polyester fiber, in which the filter press value DFFP of the functional polyester is 0.17 kPa·cm 2 /g. The far infrared flame retardant polyester fiber monofilament fineness is 1.54 dtex, the breaking strength is 3.5 cN/dtex, and the breaking elongation is 32%.
实施例16Example 16
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与亲水共聚改性单体聚乙二醇浆料组成，其中对苯二甲酸浆料由对苯二甲酸与乙二醇以醇酸摩尔比1.15调配而成、亲水共聚改性单体聚乙二醇浆料由聚乙二醇在80℃熔融调配而成。酯化反应系统由立式酯化反应釜组成，对苯二甲酸浆料以4266kg/h的流量连续均匀的输送至酯化反应釜、浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到酯化反应釜。酯化反应釜的反应温度为265℃。当聚酯低聚物的酸值达到40mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3726kg/h的流量连续稳定地从酯化反应釜采出。亲水共聚改性单体聚乙二醇浆料经聚酯低聚物管道在线添加系统以300kg/h的流量直接注入酯化反应釜后的聚酯低聚物管道中。S1, polyester oligomer slurry The raw material slurry of polyester oligomer includes terephthalic acid slurry and hydrophilic copolymerized modified monomer polyethylene glycol slurry, wherein the terephthalic acid slurry is composed of p-benzene The dicarboxylic acid and ethylene glycol are prepared with an alkyd molar ratio of 1.15, and the hydrophilic copolymer modified monomer polyethylene glycol slurry is prepared by melt-blending polyethylene glycol at 80°C. The esterification reaction system consists of a vertical esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the esterification reactor at a flow rate of 4266kg/h. The catalyst ethylene glycol antimony solution with a concentration of 3wt% is 54.8kg/ The flow rate of h is continuously and evenly injected into the esterification reactor. The reaction temperature of the esterification reactor was 265°C. When the acid value of the polyester oligomer reaches 40 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably extracted from the esterification reactor at a flow rate of 3726 kg/h. The hydrophilic copolymer modified monomer polyethylene glycol slurry is directly injected into the polyester oligomer pipeline after the esterification reactor at a flow rate of 300 kg/h through the polyester oligomer pipeline online addition system.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.6的载体浆料载体的原料浆以731.8kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为9.6kg/h，载体制备釜的反应温度为255℃。当载体的酸值达到20mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以646.1kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.6. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 731.8 kg/h. The flow rate of the catalyst ethylene glycol antimony solution with a concentration of 3 wt% injected into the carrier preparation reactor was 9.6 kg/h, and the reaction temperature of the carrier preparation reactor was 255°C. When the acid value of the carrier reaches 20 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 646.1 kg/h through the carrier delivery metering unit composed of a delivery pump and a flow meter.
将导电剂氧化铟锡浓度为20wt％的乙二醇基功能粉体预分散液以661.8kg/h的流量连续均匀的输送至由4台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的导电剂氧化铟锡平均粒径为65nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以661.8kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a concentration of 20wt% of indium tin oxide as a conductive agent is continuously and uniformly delivered to the functional powder dispersion preparation unit formed by connecting four grinding machines in series at a flow rate of 661.8 kg/h. The functional powder dispersion liquid with an average particle diameter of 65 nm of the conductive agent indium tin oxide prepared by grinding enters the functional powder dispersion liquid supply tank, and is transported to the metering unit by a functional powder dispersion liquid composed of a delivery pump and a flow meter to 661.8 kg The flow rate of /h is continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到导电剂氧化铟锡平均粒径为71nm的功能粉体浆料，然后将功能粉体浆料以1307.9kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为260℃。当功能粉体浆料浓缩物的羟值达到105mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以661.8kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出。功能粉体浆料浓缩物中导电剂氧化铟锡的含量为20wt％、压滤值DFMS为2.4kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a conductive powder indium tin oxide average particle size of 71nm, and then the functional powder The slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 1307.9 kg/h. The temperature of the evaporation unit is 260°C. When the hydroxyl value of the functional powder slurry concentrate reaches 105 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 661.8 kg/h. Produced in the material concentration unit. The content of the conductive agent indium tin oxide in the functional powder slurry concentrate was 20 wt%, and the filter press value DFMS was 2.4 kPa·cm 2 /g.
S3，来自聚酯低聚物管道的聚酯低聚物和亲水共聚改性单体聚乙二醇浆料的共混物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.30dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。S3, blend of polyester oligomer from polyester oligomer pipeline and hydrophilic copolymerization modified monomer polyethylene glycol slurry and functional powder slurry from functional powder slurry concentrate preparation system The concentrate enters the functional powder slurry concentrate mixing unit together, and after being mixed uniformly by the mixing unit, it enters the pre-condensation reaction system. The mixing unit is a high-shear pump. The pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.30 dL/g, it is continuously and stably extracted from the pre-condensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
当功能聚酯特性粘度达到0.60dL/g，通过终聚物泵连续稳定地从终缩聚反应釜采出并输送至液相增粘反应釜进行液相增粘，液相增粘反应釜的反应温度为285℃。When the intrinsic viscosity of the functional polyester reaches 0.60dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening. The temperature is 285°C.
当功能聚酯增粘物特性粘度达到0.86dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为亲水共聚酯的抗静电亲水聚酯纤维，其中，功能聚酯的压滤值DFFP为0.09kPa·cm 2/g。该抗静电亲水聚酯纤维单丝纤度为1.16dtex、断裂强度为4.6cN/dtex、断裂伸长率为28％。 When the intrinsic viscosity of the functional polyester tackifier reaches 0.86dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the antistatic hydrophilic polymer with a hydrophilic copolyester matrix is prepared Ester fiber, wherein the functional polyester has a filter value DFFP of 0.09 kPa·cm 2 /g. The antistatic hydrophilic polyester fiber has a monofilament fineness of 1.16 dtex, a breaking strength of 4.6 cN/dtex, and an elongation at break of 28%.
实施例17Example 17
S1，将聚酯瓶片废料和醇解乙二醇分别以3750kg/h和242kg/h连续均匀的输送至由酯化醇解反应釜组成的酯化系统中，酯化醇解反应釜为平行设置有两个搅拌桨相互啮合的搅拌器的卧式反应釜。酯化醇解反应釜的反应温度为270℃。当聚酯废料醇解物的羟值达到110mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3992kg/h的流量连续稳定地从酯化醇解反应釜中采出。S1: Continuously and uniformly convey the waste of polyester bottle flakes and alcoholysis glycol at 3750kg/h and 242kg/h to the esterification system composed of the esterification alcoholysis reactor, the esterification alcoholysis reactors are parallel A horizontal reaction kettle provided with a stirrer with two stirring paddles meshing with each other. The reaction temperature of the esterification and alcoholysis reactor was 270°C. When the hydroxyl value of the polyester waste alcoholysis product reaches 110mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device continuously and stably from the esterification alcoholysis reactor at a flow rate of 3992kg/h Mined out.
S2，将分子量为600的聚己二酸乙二醇酯多元醇以609.3kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，载体制备釜的反应温度为40℃。通过由输送泵和流量计组成的载体计量输送单元以609.3kg/h的流量连续稳定地从载体制备反应釜采出。S2. Polyethylene adipate polyol with a molecular weight of 600 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 609.3 kg/h. The reaction temperature of the carrier preparation reactor is 40°C. The carrier metering and delivery unit composed of a delivery pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 609.3 kg/h.
将抗菌剂石墨烯浓度为10wt％的水基功能粉体预分散液以188.4kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的抗菌剂石墨烯平均粒径为1000nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以188.4kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The water-based functional powder pre-dispersion with an antibacterial agent graphene concentration of 10 wt% is continuously and uniformly delivered to a functional powder dispersion preparation unit formed by three grinding machines in series at a flow rate of 188.4 kg/h, which is prepared by grinding The obtained functional powder dispersion with an average particle diameter of 1000 nm of the antibacterial agent enters into the functional powder dispersion supply tank, and is transported to the metering unit at a flow rate of 188.4 kg/h through the functional powder dispersion composed of a delivery pump and a flow meter Continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由研磨机组成的功能粉体分散液与载体混合单元混合均匀后得到抗菌剂石墨烯平均粒径为1000nm的功能粉体浆料，然后将功能粉体浆料以797.7kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为100℃。当功能粉体浆料浓缩物的羟值达到175mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以628.1kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中抗菌剂石墨烯的含量为3wt％、压滤值DFMS为30kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a grinder and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 1000 nm of the antibacterial agent graphene, and then the functional powder slurry It is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 797.7 kg/h. The temperature of the evaporation unit is 100°C. When the hydroxyl value of the functional powder slurry concentrate reaches 175 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 628.1 kg/h. Extracted from the material concentration unit, the content of the antibacterial agent graphene in the functional powder slurry concentrate is 3 wt%, and the filter press value DFMS is 30 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯废料醇解物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为SMXL型静态混合器。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.22dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。S3, the polyester waste alcoholysis product from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and are mixed by the mixing unit After being homogenized, it enters the pre-condensation reaction system, and the mixing unit is a SMXL static mixer. The pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.22dL/g, it is continuously and stably extracted from the pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C.
当功能聚酯特性粘度达到0.76dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得抗菌再生聚酯纤维，其中，功能聚酯的压滤值DFFP为0.80kPa·cm 2/g。该抗菌再生聚酯纤维的单丝纤度为3.47dtex、断裂强度为2.8cN/dtex、断裂伸长率为26％。 When the intrinsic viscosity of the functional polyester reaches 0.76dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to produce antibacterial regenerated polyester fiber, in which the filter press value of the functional polyester is DFFP It is 0.80 kPa·cm 2 /g. The antibacterial regenerated polyester fiber has a monofilament fineness of 3.47 dtex, a breaking strength of 2.8 cN/dtex, and an elongation at break of 26%.
实施例18Example 18
S1，聚酯低聚物浆料聚酯低聚物的原料浆包括对苯二甲酸浆料与阳离子染料可染共聚改性单体间苯二甲酸二丙二醇酯-5-磺酸钠浆料组成，其中对苯二甲酸浆料由对苯二甲酸与丙二醇以醇酸摩尔比1.4调配而成、阳离子染料可染共聚改性单体间苯二甲酸二丙二醇酯-5-磺酸钠浆料由间苯二甲酸二丙二醇酯-5-磺酸钠与丙二醇以重量比4:6调配而成。酯化反应系统由立式第一酯化反应釜和卧室卧式三分室结构第二酯化反应釜组成，对苯二甲酸浆料以4958kg/h的流量连续均匀的输送至立式第一酯化反应釜、阳离子染料可染共聚改性单体间苯二甲酸二丙二醇酯-5-磺酸钠浆料以349.2kg/h的流量连续均匀的注入卧室卧式第二酯化反应釜的第二室、浓度为10wt％的催化剂钛酸四异丙酯溶液以18.8kg/h的流量连续均匀的注入到卧式第二酯化反应釜的第三室。第一酯化反应釜反应温度为240℃，第二酯化反应釜反应温度230℃。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以4691kg/h的流量连续稳定地从第二酯化反应釜采出。S1. Polyester oligomer slurry The raw material slurry of polyester oligomer consists of terephthalic acid slurry and cationic dye-dyeable copolymerizable modified monomer dipropylene isophthalate-5-sulfonate slurry Among them, the terephthalic acid slurry is prepared from terephthalic acid and propylene glycol with an alkyd molar ratio of 1.4, and the cationic dye can be dyed and copolymerized to modify the monomer dipropylene isophthalate-5-sulfonate. Dipropylene isophthalate-5-sulfonate sodium and propylene glycol are formulated at a weight ratio of 4:6. The esterification reaction system consists of a vertical first esterification reactor and a bedroom horizontal three-chamber structure second esterification reactor. The terephthalic acid slurry is continuously and uniformly delivered to the vertical first ester at a flow rate of 4958 kg/h Chemical reactor, cationic dye-dyeable copolymerizable modified monomer dipropylene isophthalate-5-sulfonate sodium slurry was continuously and uniformly injected into the bedroom horizontal second esterification reactor at a flow rate of 349.2kg/h The two-chamber, 10wt% concentration catalyst tetraisopropyl titanate solution was continuously and uniformly injected into the third chamber of the horizontal second esterification reactor at a flow rate of 18.8 kg/h. The reaction temperature of the first esterification reactor was 240°C, and the reaction temperature of the second esterification reactor was 230°C. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 4691 kg/h Out.
S2，将对苯二甲酸和丙二醇调配成醇酸摩尔比为2.0的载体浆料载体的原料浆以258.5kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为10wt％的催化剂钛酸四异丙酯溶液注入载体制备反应釜的流量为0.7kg/h，载体制备釜的反应温度为230℃。当载体的酸值达到7mgKOH/g，通过由输送泵和流量计组成的载体输送计量单元以230.5kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and propylene glycol into a carrier slurry with an alkyd molar ratio of 2.0. The raw material slurry of the carrier is continuously and uniformly delivered to the carrier preparation unit composed of the carrier preparation reactor at a flow rate of 258.5 kg/h. The concentration is The flow rate of the 10 wt% catalyst tetraisopropyl titanate solution injected into the carrier preparation reactor was 0.7 kg/h, and the reaction temperature of the carrier preparation reactor was 230°C. When the acid value of the carrier reaches 7 mgKOH/g, it is continuously and stably withdrawn from the carrier preparation reactor at a flow rate of 230.5 kg/h through a carrier delivery metering unit composed of a delivery pump and a flow meter.
将防紫外辐射剂掺锌二氧化钛浓度为30wt％的丙二醇基功能粉体预分散液以239.4kg/h的流量连续均匀的输送至由4台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的防紫外辐射剂掺锌二氧化钛平均粒径为78nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以239.4kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。Propylene glycol-based functional powder pre-dispersion with an anti-ultraviolet radiation agent zinc-doped titanium dioxide concentration of 30% by weight was continuously and uniformly delivered to a functional powder dispersion preparation unit made up of 4 grinding machines in series at a flow rate of 239.4 kg/h. The functional powder dispersion liquid with an average particle diameter of 78 nm, which is an anti-ultraviolet radiation agent zinc-doped titanium dioxide prepared by grinding, enters the functional powder dispersion liquid supply tank, and is conveyed to the metering unit by the functional powder dispersion liquid composed of a delivery pump and a flow meter. The flow rate of 239.4kg/h was continuously and stably extracted from the functional powder dispersion supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到防紫外辐射剂掺锌二氧化钛平均粒径为81nm的功能粉体浆料，然后将功能粉体浆料以469.9kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为250℃。当功能粉体浆料浓缩物的羟值达到28mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以239.4kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出。功能粉体浆料浓缩物中防紫外辐射剂掺锌二氧化钛的含量为30wt％、压滤值DFMS为3.1kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain an anti-ultraviolet radiation agent zinc-doped titanium dioxide with an average particle size of 81 nm, and then the function The powder slurry is continuously and uniformly transported to a functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function at a flow rate of 469.9 kg/h. The temperature of the evaporation unit is 250°C. When the hydroxyl value of the functional powder slurry concentrate reaches 28 mgKOH/g, the functional powder slurry concentrate metering and delivery unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 239.4 kg/h Produced in the material concentration unit. The content of the anti-ultraviolet radiation agent zinc-doped titanium dioxide in the functional powder slurry concentrate is 30 wt%, and the filter press value DFMS is 3.1 kPa·cm 2 /g.
S3，来自酯化系统的聚酯低聚物与来自功能粉体浆料浓缩物制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为230℃。当预聚物特性粘度达到0.38dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚反应系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为240℃。S3. The polyester oligomer from the esterification system enters into the functional powder slurry concentrate mixing unit together with the functional powder slurry concentrate from the functional powder slurry concentrate preparation system. In the pre-condensation reaction system, the mixing unit is a high-shear pump. The pre-polycondensation reaction system is composed of a vertical pre-condensation reactor, in which the temperature of the reactant in the pre-condensation reactor is 230°C. When the intrinsic viscosity of the prepolymer reaches 0.38dL/g, it is continuously and stably extracted from the precondensation reactor by the prepolymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, in which the reaction temperature of the final polycondensation reaction kettle is 240°C.
当终聚物特性粘度达到0.90dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为阳离子染料可染共聚酯的防紫外辐射阳离子染料可染聚酯纤维，其中功能聚酯的压滤值DFFP为0.11kPa·cm 2/g。该防紫外辐射阳离子染料可染聚酯纤维单丝纤度为1.16dtex、断裂强度为3.2cN/dtex、断裂伸长率为31％。 When the intrinsic viscosity of the final polymer reaches 0.90dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning, and the anti-ultraviolet radiation cationic dye whose matrix is the cationic dyeable copolyester can be prepared. Dyed polyester fiber, where the functional polyester has a filter value DFFP of 0.11 kPa·cm 2 /g. The anti-ultraviolet radiation cationic dyeable polyester fiber monofilament has a fineness of 1.16 dtex, a breaking strength of 3.2 cN/dtex, and an elongation at break of 31%.
实施例19Example 19
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.13的聚酯低聚物浆料聚酯低聚物的原料浆以4613kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统的第一酯化釜中进行酯化反应，第一酯化反应釜反应温度为260℃。当第一酯化釜聚酯低聚物的酸值达到50mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3980kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h. The esterification reaction is carried out in the first esterification reactor of the esterification reaction system composed of the first esterification reactor and the vertical second esterification reactor. The reaction temperature of the first esterification reactor is 260°C. When the acid value of the polyester oligomer in the first esterification kettle reaches 50 mgKOH/g, the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter continuously and steadily from the second at a flow rate of 3980 kg/h Extracted from the esterification reactor.
S2，将分子量为4000的聚乙二醇以10.4kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，载体制备釜的反应温度为80℃。通过由输送泵和流量计组成的载体计量输送单元以10.4kg/h的流量连续稳定地从载体制备反应釜采出。将二氧化钛浓度为60wt％的水基功能粉体预分散液以329kg/h的流量连续均匀的输送至由5台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的二氧化钛平均粒径为71nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以329kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。载体与功能粉体分散液一起进入由螺杆挤出机组成的功能粉体分散液与载体混合单元混合均匀后得到二氧化钛平均粒径为88nm的功能粉体浆料，然后将功能粉体浆料以339.4kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为110℃。当功能粉体浆料浓缩物的羟值达到2mgKOH/g，通过由具有计量功能的输送泵组成的功能粉体浆料浓缩物计量输送单元以207.8kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中二氧化钛的含量为95wt％、压滤值DFMS为9.4kPa·cm 2/g。 S2. Polyethylene glycol with a molecular weight of 4000 is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 10.4 kg/h. The reaction temperature of the carrier preparation reactor is 80°C. The carrier metering and conveying unit composed of a conveying pump and a flow meter is continuously and stably extracted from the carrier preparation reactor at a flow rate of 10.4 kg/h. The water-based functional powder pre-dispersion with a titanium dioxide concentration of 60wt% is continuously and uniformly delivered at a flow rate of 329kg/h to a functional powder dispersion preparation unit composed of 5 grinders in series. The functional powder dispersion with a particle size of 71 nm enters the functional powder dispersion supply tank, and is continuously and stably dispersed from the functional powder at a flow rate of 329 kg/h through the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter Extracted from the liquid supply tank. The carrier and the functional powder dispersion together enter the functional powder dispersion composed of a screw extruder and the mixing unit of the carrier to be uniformly mixed to obtain a functional powder slurry with an average particle diameter of 88 nm of titanium dioxide. The flow rate of 339.4kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 110°C. When the hydroxyl value of the functional powder slurry concentrate reaches 2 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a conveying pump with a metering function can continuously and stably remove the functional powder from the functional powder at a flow rate of 207.8 kg/h. Extracted from the slurry concentration unit, the content of titanium dioxide in the functional powder slurry concentrate is 95% by weight, and the pressure filtration value DFMS is 9.4 kPa·cm 2 /g.
S3，来自酯化反应系统第一酯化反应釜的第一酯化釜聚酯低聚物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入酯化系统第二酯化釜，混合单元为球窝式动态混合器。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。第二酯化反应釜反应温度为265℃。当第二酯化釜聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以4128kg/h的流量连续稳定地从第二酯化反应釜采出。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为275℃、第二预缩聚反应釜的反应物温度为280℃。当功能聚酯预聚物特性粘度达到0.20dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为290℃。S3, the first esterification kettle polyester oligomer from the first esterification reactor of the esterification reaction system enters the functional powder slurry together with the functional powder slurry concentrate from the continuous preparation system of the functional powder slurry concentrate The mixing unit of the material concentrate is mixed uniformly by the mixing unit and then enters the second esterification kettle of the esterification system. The mixing unit is a ball and socket type dynamic mixer. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. The reaction temperature of the second esterification reactor was 265°C. When the acid value of the polyester oligomer in the second esterification kettle reaches 15 mgKOH/g, the oligomer delivery and metering device composed of an oligomer pump and an oligomer flow meter continuously and stably from the second at a flow rate of 4128 kg/h Extracted from the esterification reactor. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 275°C and the reactant temperature of the second precondensation reaction kettle is 280℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.20dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 290°C.
当功能聚酯特性粘度达到0.72dL/g，将功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得光学遮蔽聚酯纤维，其中，功能聚酯的压滤值DFFP为0.32kPa·cm 2/g。该光学遮蔽聚酯纤维的单丝纤度为1.54dtex、断裂强度为3.1cN/dtex、断裂伸长率为24％。 When the intrinsic viscosity of the functional polyester reaches 0.72dL/g, the functional polyester melt is directly transported to the spinning position through the melt pipe for spinning to produce an optically shielded polyester fiber, in which the filter press value of the functional polyester is DFFP It is 0.32 kPa·cm 2 /g. The monofilament fineness of this optically shielding polyester fiber was 1.54 dtex, the breaking strength was 3.1 cN/dtex, and the elongation at break was 24%.
实施例20Example 20
S1，将对苯二甲酸和乙二醇调配成的醇酸摩尔比为1.13的聚酯低聚物浆料聚酯低聚物的原料浆以4613kg/h的流量连续均匀的输送到由立式第一酯化反应釜和立式第二酯化反应釜组成的酯化反应系统中进行酯化反应，第一酯化反应釜反应温度为260℃，第二酯化反应釜反应温度265℃。浓度为3wt％的催化剂乙二醇锑溶液以54.8kg/h的流量连续均匀的注入到第二酯化反应釜中。当聚酯低聚物的酸值达到15mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3931kg/h的流量连续稳定地从第二酯化反应釜采出。S1, the polyester oligomer slurry prepared by mixing terephthalic acid and ethylene glycol with an alkyd molar ratio of 1.13 is continuously and uniformly conveyed to the vertical type by the flow rate of 4613kg/h. The esterification reaction system is composed of a first esterification reactor and a vertical second esterification reactor. The reaction temperature of the first esterification reactor is 260°C, and the reaction temperature of the second esterification reactor is 265°C. The catalyst ethylene glycol antimony solution with a concentration of 3 wt% was continuously and uniformly injected into the second esterification reactor at a flow rate of 54.8 kg/h. When the acid value of the polyester oligomer reaches 15 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer pump and metering device are continuously and stably collected from the second esterification reactor at a flow rate of 3931 kg/h. Out.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.6的载体浆料载体的原料浆以380kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为4.0kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到10mgKOH/g，通过由输送泵和流量计组成的载体计量输送单元以333.5kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.6. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 380 kg/h, concentration The flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.0 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 333.5 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
将炭黑浓度为20wt％的乙二醇基功能粉体预分散液以343.7kg/h的流量连续均匀的输送至由3台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的炭黑平均粒径为96nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以343.7kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20% by weight is continuously and uniformly transported to a functional powder dispersion preparation unit composed of three grinding machines in series at a flow rate of 343.7 kg/h, which is prepared by grinding The obtained functional powder dispersion with an average particle size of carbon black of 96 nm enters the functional powder dispersion supply tank, and is continuously stabilized at a flow rate of 343.7 kg/h by the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter It is taken from the functional powder dispersion liquid supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到炭黑平均粒径为104nm的功能粉体浆料，然后将功能粉体浆料以677.2kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到140mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以343.7kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中炭黑的含量为20wt％、压滤值DFMS为2.1kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 104 nm, and then the functional powder slurry The flow rate of 677.2kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 140 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 343.7 kg/h. Extracted from the feed concentration unit, the content of carbon black in the functional powder slurry concentrate is 20 wt%, and the pressure filtration value DFMS is 2.1 kPa·cm 2 /g.
S3，来自酯化反应系统的聚酯低聚物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为高剪切泵。预缩聚反应系统由立式第一预缩聚反应釜和立式第二预缩聚反应釜组成，其中第一预缩聚反应釜的反应物温度为270℃、第二预缩聚反应釜的反应物温度为275℃。当功能聚酯预聚物特性粘度达到0.16dL/g，通过预聚物泵连续稳定的从第二预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为280℃。当功能聚酯终聚物特性粘度达到0.67dL/g，通过终聚物泵连续稳定地从终缩聚反应釜采出并输送至液相增粘反应釜进行液相增粘，液相增粘反应釜的反应温度290℃。S3, the polyester oligomer from the esterification reaction system and the functional powder slurry concentrate from the functional powder slurry concentrate continuous preparation system enter the functional powder slurry concentrate mixing unit, and the mixture is uniformly mixed by the mixing unit After entering the pre-condensation reaction system, the mixing unit is a high-shear pump. The precondensation reaction system is composed of a vertical first precondensation reaction kettle and a vertical second precondensation reaction kettle, in which the reactant temperature of the first precondensation reaction kettle is 270°C and the reactant temperature of the second precondensation reaction kettle is 275℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.16dL/g, it is continuously and stably extracted from the second pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 280°C. When the intrinsic viscosity of the functional polyester final polymer reaches 0.67dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening, liquid-phase thickening reaction The reaction temperature of the kettle was 290°C.
当功能聚酯增粘物特性粘度达到1.00dL/g，将功能聚酯增粘熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为聚对苯二甲酸乙二醇酯的原液着色黑色聚酯纤维，其中，功能聚酯的压滤值DFFP为0.07kPa·cm 2/g。该原液着色黑色聚酯纤维的单丝纤度为1.16dtex、断裂强度为8.1cN/dtex、断裂伸长率为17％。 When the intrinsic viscosity of the functional polyester tackifier reaches 1.00dL/g, the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the obtained matrix is polyethylene terephthalate The dope colored black polyester fiber, of which the functional polyester has a filter press value of DFFP of 0.07 kPa·cm 2 /g. The monofilament fineness of this dope-colored black polyester fiber was 1.16 dtex, the breaking strength was 8.1 cN/dtex, and the breaking elongation was 17%.
实施例21Example 21
S1，将聚酯瓶片废料和醇解乙二醇分别以3562kg/h和230kg/h连续均匀的输送至由酯化醇解反应釜组成的酯化系统中，酯化醇解反应釜为平行设置有两个搅拌桨相互啮合的搅拌器的卧式反应釜。酯化醇解反应釜的反应温度为270℃。当聚酯废料醇解物的羟值达到110mgKOH/g，通过低聚物泵和低聚物流量计组成的低聚物输送计量装置以3792kg/h的流量连续稳定地从酯化醇解反应釜中采出。由2-羧乙基苯基次磷酸二乙二醇酯与乙二醇以5:5调配成的阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料经聚酯低聚物管道在线添加系统以472kg/h的流量直接注入酯化醇解反应釜后的聚酯低聚物管道中。S1, the polyester bottle flake waste and alcoholysis glycol are continuously and uniformly transported to the esterification system composed of the esterification alcoholysis reactor at 3562kg/h and 230kg/h respectively, the esterification alcoholysis reactor is parallel A horizontal reaction kettle provided with a stirrer with two stirring paddles meshing with each other. The reaction temperature of the esterification and alcoholysis reactor was 270°C. When the hydroxyl value of the polyester waste alcoholysis product reaches 110 mgKOH/g, the oligomer pump and oligomer flow meter composed of an oligomer delivery and metering device continuously and stably from the esterification alcoholysis reactor at a flow rate of 3792 kg/h Mined out. The flame retardant copolymer modified monomer 2-carboxyethyl phenyl hypophosphite diethylene glycol formulated with 2-carboxyethyl phenyl hypophosphite diethylene glycol and ethylene glycol at a ratio of 5:5 The online addition system of polyester oligomer pipeline is directly injected into the polyester oligomer pipeline after the esterification and alcoholysis reactor at a flow rate of 472kg/h.
S2，将对苯二甲酸和乙二醇调配成醇酸摩尔比为1.6的载体浆料载体的原料浆以380kg/h的流量连续均匀的输送至由载体制备反应釜组成的载体制备单元，浓度为3wt％的催化剂乙二醇锑溶液注入载体制备反应釜的流量为4.0kg/h，载体制备釜的反应温度为260℃。当载体的酸值达到10mgKOH/g，通过由输送泵和流量计组成的载体计量输送单元以333.5kg/h的流量连续稳定地从载体制备反应釜采出。S2, mixing terephthalic acid and ethylene glycol into a carrier slurry with an alkyd molar ratio of 1.6. The raw material carrier of the carrier is continuously and uniformly delivered to a carrier preparation unit composed of a carrier preparation reactor at a flow rate of 380 kg/h, concentration The flow rate of the 3% by weight catalyst ethylene glycol antimony solution injected into the carrier preparation reactor was 4.0 kg/h, and the reaction temperature of the carrier preparation reactor was 260°C. When the acid value of the carrier reaches 10 mgKOH/g, it is continuously and stably extracted from the carrier preparation reactor at a flow rate of 333.5 kg/h by a carrier metering and conveying unit composed of a conveying pump and a flow meter.
将炭黑浓度为20wt％的乙二醇基功能粉体预分散液以343.7kg/h的流量连续均匀的输送至由2台研磨机串联而成的功能粉体分散液制备单元，经过研磨制备得到的炭黑平均粒径为146nm的功能粉体分散液进入功能粉体分散液供应罐，通过由输送泵和流量计组成的功能粉体分散液输送计量单元以343.7kg/h的流量连续稳定地从功能粉体分散液供应罐中采出。The ethylene glycol-based functional powder pre-dispersion with a carbon black concentration of 20 wt% is continuously and uniformly delivered at a flow rate of 343.7 kg/h to a functional powder dispersion preparation unit formed by two grinding machines connected in series, and prepared by grinding The obtained functional powder dispersion with an average particle size of 146 nm of carbon black enters the functional powder dispersion supply tank, and is continuously stabilized at a flow rate of 343.7 kg/h by the functional powder dispersion liquid metering unit composed of a delivery pump and a flow meter It is taken from the functional powder dispersion liquid supply tank.
载体与功能粉体分散液一起进入由剪切泵组成的功能粉体分散液与载体混合单元混合均匀后得到炭黑平均粒径为154nm的功能粉体浆料，然后将功能粉体浆料以677.2kg/h的流量连续均匀的输送至由具有闪蒸功能的蒸发单元组成的功能粉体浆料浓缩单元，蒸发单元的温度为270℃。当功能粉体浆料浓缩物的羟值达到140mgKOH/g，通过由输送泵和流量计组成的功能粉体浆料浓缩物计量输送单元以343.7kg/h的流量连续稳定地从功能粉体浆料浓缩单元中采出，功能粉体浆料浓缩物中炭黑的含量为20wt％、压滤值DFMS为4.6kPa·cm 2/g。 The carrier and the functional powder dispersion liquid enter the functional powder dispersion liquid composed of a shear pump and the carrier mixing unit to be uniformly mixed to obtain a functional powder slurry with an average particle size of carbon black of 154 nm. The flow rate of 677.2kg/h is continuously and uniformly delivered to the functional powder slurry concentration unit composed of an evaporation unit with a flash evaporation function, and the temperature of the evaporation unit is 270°C. When the hydroxyl value of the functional powder slurry concentrate reaches 140 mgKOH/g, the functional powder slurry concentrate metering and conveying unit composed of a delivery pump and a flow meter continuously and stably removes the functional powder slurry at a flow rate of 343.7 kg/h. Extracted from the feed concentration unit, the content of carbon black in the functional powder slurry concentrate is 20 wt%, and the filter press value DFMS is 4.6 kPa·cm 2 /g.
S3，来自聚酯低聚物管道的聚酯废料醇解物和阻燃共聚改性单体2-羧乙基苯基次磷酸二乙二醇酯浆料的共混物与来自功能粉体浆料浓缩物连续制备系统的功能粉体浆料浓缩物一起进入功能粉体浆料浓缩物混合单元，经混合单元混合均匀后进入预缩聚反应系统，混合单元为球窝式动态混合器。预缩聚反应系统由立式预缩聚反应釜组成，其中预缩聚反应釜的反应物温度为270℃。当功能聚酯预聚物特性粘度达到0.16dL/g，通过预聚物泵连续稳定的从预缩聚反应釜采出并输送至终缩聚系统进行终缩聚反应。终缩聚系 统由卧式终缩聚反应釜组成，其中终缩聚反应釜的反应温度为275℃。当功能聚酯特性粘度达到0.60dL/g，通过终聚物泵连续稳定地从终缩聚反应釜采出并输送至液相增粘反应釜进行液相增粘，液相增粘反应釜的反应温度为290℃。S3, blend of polyester waste alcoholysis from polyester oligomer pipeline and flame retardant copolymerization modified monomer 2-carboxyethylphenyl diethylene glycol diethylene glycol slurry with functional powder slurry The functional powder slurry concentrate of the continuous preparation system of the material concentrate enters the functional powder slurry concentrate mixing unit together, and after being uniformly mixed by the mixing unit, it enters the pre-polycondensation reaction system. The mixing unit is a ball and socket type dynamic mixer. The pre-polycondensation reaction system consists of a vertical pre-condensation reactor, in which the temperature of the reactants in the pre-condensation reactor is 270°C. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.16dL/g, it is continuously and stably extracted from the pre-polycondensation reactor through the pre-polymer pump and sent to the final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reactor, in which the reaction temperature of the final polycondensation reactor is 275°C. When the intrinsic viscosity of the functional polyester reaches 0.60dL/g, it is continuously and stably extracted from the final polycondensation reaction kettle through the final polymer pump and transported to the liquid-phase thickening reaction kettle for liquid-phase thickening. The temperature is 290°C.
当功能聚酯增粘物特性粘度达到0.84dL/g，将功能聚酯增粘熔体通过熔体管道直接输送至纺丝位进行纺丝，制得基体为阻燃再生共聚酯的原液着色阻燃再生聚酯纤维，其中，功能聚酯的压滤值DFFP为0.15kPa·cm 2/g。该原液着色阻燃再生聚酯纤维的单丝纤度为1.16dtex、断裂强度为3.8cN/dtex、断裂伸长率为32％。 When the intrinsic viscosity of the functional polyester tackifier reaches 0.84dL/g, the functional polyester tackified melt is directly transported to the spinning position through the melt pipe for spinning, and the base material is the stock solution of flame retardant recycled copolyester coloring Flame-retardant regenerated polyester fiber, in which the functional polyester has a filter value DFFP of 0.15 kPa·cm 2 /g. The monofilament fineness of this dope colored flame retardant regenerated polyester fiber was 1.16 dtex, the breaking strength was 3.8 cN/dtex, and the breaking elongation was 32%.
对比例1Comparative Example 1
将特性粘度为0.65dL/g的聚酯熔体通过熔体出料泵以3750kg/h的流量连续稳定地从终缩聚反应釜采出经熔体管道输送至动态混合器。颜料蓝15:3浓度为30wt％、压滤值DFMS为39.2kPa·cm 2/g的功能母粒熔体通过单螺杆挤出机以326.1kg/h的流量注入动态混合器。聚酯熔体与功能母粒熔体经动态混合器均匀混合得到的功能聚酯熔体通过熔体管道直接输送至纺丝位进行纺丝，制得原液着色蓝色聚酯纤维，其中功能聚酯的压滤值DFFP为1.05kPa·cm 2/g。。 The polyester melt with an intrinsic viscosity of 0.65 dL/g was continuously and stably extracted from the final polycondensation reactor through a melt discharge pump at a flow rate of 3750 kg/h, and then transferred to a dynamic mixer through a melt pipe. The functional masterbatch melt of Pigment Blue 15:3 with a concentration of 30 wt% and a pressure filtration value of DFMS of 39.2 kPa·cm 2 /g was injected into the dynamic mixer through a single screw extruder at a flow rate of 326.1 kg/h. The functional polyester melt obtained by uniformly mixing the polyester melt and the functional masterbatch melt through a dynamic mixer is directly transported to the spinning position through a melt pipe for spinning, to prepare a dope-colored blue polyester fiber, in which the functional polymer The pressure filtration value DFFP of the ester was 1.05 kPa·cm 2 /g. .
该原液着色蓝色聚酯纤维的单丝纤度为0.77dtex、断裂强度为2.3cN/dtex、断裂伸长率为15％。The monofilament fineness of this dope-colored blue polyester fiber was 0.77 dtex, the breaking strength was 2.3 cN/dtex, and the elongation at break was 15%.
实验例1Experimental Example 1
将如上实施例1～21以及对比例1所制备的功能聚酯及功能纤维产品进行相关性能测试。The functional polyester and functional fiber products prepared in Examples 1 to 21 and Comparative Example 1 above were subjected to relevant performance tests.
测试的相关性能如下：功能粉体浆料中功能粉体平均粒径(μm)，测试方法：先将功能粉体浆料溶解于良溶剂六氟异丙醇中，然后再采用动态光散射粒度仪测试功能粉体粒径。功能粉体浆料浓缩物的羟值(mgKOH/g)，测试方法：参照HG/T 2709-95。功能粉体浆料浓缩物压滤值DFMB(kPa·cm 2/g)，测试方法：由重量为m1的功能粉体浆料浓缩物与重量为m2的聚酯聚对苯二甲酸乙二醇酯组成总重量为4000g测试混合物，测试混合物中功能粉体的含量为100g；由长径比为Φ25mm×25D的单螺杆挤出机、容积为1.2cc的熔体计量泵、熔体压力传感器和滤网面积S为3.8cm2的60-100-1400-100-20目四层组合滤网依次连接组成压滤性能测试仪；压滤性能测试工艺条件：熔体温度为295℃、熔体计量泵泵前压力设定值为6.5MPa、熔体计量泵计量流量为38g/min；先将500g聚酯聚对苯二甲酸乙二醇酯从压滤性能测试仪中挤出，记录平衡压力为初始压力Ps，然后将4000g测试混合物从压滤性能测试仪中挤出，再将500g聚酯聚对苯二甲酸乙二醇酯从压滤性能测试仪中挤出，记录平衡压力为终止压力PT，最后按照公式:计算得出压滤值DFMS。功能聚酯特性粘度(dL/g)，测试方法：参照GB/T 14190-2008。功能聚酯压滤值DFFP(kPa·cm 2/g)，测试方法：由长径比为Φ25mm×25D的单螺杆挤出机、容积为1.2cc的熔体计量泵、熔体压力传感器和滤网面积S为3.8cm2的60-100-1400-100-20目四层组合滤网依次连接组成压滤性能测试仪；压滤性能测试工艺条件：熔体温度为295℃、熔体计量泵泵前压力设定值为6.5MPa、熔体计量泵计量流量为38g/min；先将500g聚酯聚对苯二甲酸乙二醇酯从压滤性能测试仪中挤出，记录平衡压力为初始压力Ps，然后将3000g功能聚酯从压滤性能测试仪中挤出，再将500g聚酯聚对苯二甲酸乙二醇酯从压滤性能测试仪中挤出，记录平衡压力为终止压力PT，最后按照公式:计算得出压滤值DFFP。功能聚酯纤维线密度(dtex)，测试方法：参照GB/T 14343-2008；功能聚酯纤维断裂强度(cN/dtex)，测试方法：参照GB/T14344-2008；功能聚酯纤维断裂伸长(％)，测试方法：参照GB/T 14344-2008。以上各性能的测试结果见表1和表2。 The relevant performance of the test is as follows: the average particle size (μm) of the functional powder in the functional powder slurry, the test method: first dissolve the functional powder slurry in a good solvent hexafluoroisopropanol, and then use dynamic light scattering particle size The instrument tests the particle size of the functional powder. The hydroxyl value (mgKOH/g) of the functional powder slurry concentrate, test method: refer to HG/T 2709-95. The filter press value of functional powder slurry concentrate DFMB (kPa·cm 2 /g), test method: from functional powder slurry concentrate with weight m1 and polyester polyethylene terephthalate with weight m2 The total weight of the ester composition is 4000g test mixture, the content of functional powder in the test mixture is 100g; it consists of a single screw extruder with an aspect ratio of Φ25mm×25D, a melt metering pump with a volume of 1.2cc, a melt pressure sensor and The 60-100-1400-100-20 mesh four-layer combination screen with a filter area S of 3.8cm2 is connected in sequence to form a filter performance tester; filter performance test process conditions: melt temperature is 295℃, melt metering pump The pre-pump pressure setting is 6.5MPa and the melt metering pump metering flow rate is 38g/min; first squeeze 500g of polyester polyethylene terephthalate from the filter performance tester and record the equilibrium pressure as the initial Pressure Ps, then extrude 4000g of the test mixture from the filter performance tester, and then extrude 500g of polyester polyethylene terephthalate from the filter performance tester, and record the equilibrium pressure as the termination pressure PT, Finally, according to the formula: Calculate the pressure filter value DFMS. Intrinsic viscosity of functional polyester (dL/g), test method: refer to GB/T 14190-2008. Functional polyester filter press value DFFP (kPa·cm 2 /g), test method: single screw extruder with aspect ratio Φ25mm×25D, melt metering pump with a volume of 1.2cc, melt pressure sensor and filter The 60-100-1400-100-20 mesh four-layer combined filter screen with a mesh area S of 3.8cm2 is connected in sequence to form a filter performance tester; filter performance test process conditions: melt temperature is 295℃, melt metering pump pump The pre-pressure setting value is 6.5MPa, the metering flow rate of the melt metering pump is 38g/min; first squeeze 500g polyester polyethylene terephthalate from the filter performance tester, and record the equilibrium pressure as the initial pressure Ps, then extrude 3000g of functional polyester from the filter performance tester, and then extrude 500g of polyester polyethylene terephthalate from the filter performance tester, and record the equilibrium pressure as the end pressure PT, Finally, according to the formula: Calculate the pressure filter value DFFP. Functional polyester linear density (dtex), test method: refer to GB/T 14343-2008; functional polyester fiber breaking strength (cN/dtex), test method: refer to GB/T14344-2008; functional polyester fiber break elongation (%), test method: refer to GB/T 14344-2008. The test results of the above performances are shown in Table 1 and Table 2.
表1Table 1
Figure PCTCN2019092058-appb-000001
Figure PCTCN2019092058-appb-000001
Figure PCTCN2019092058-appb-000002
Figure PCTCN2019092058-appb-000002
表2Table 2
Figure PCTCN2019092058-appb-000003
Figure PCTCN2019092058-appb-000003
Figure PCTCN2019092058-appb-000004
Figure PCTCN2019092058-appb-000004
由表1和表2的数据可知，采用本发明的功能聚酯生产方法所制备的功能聚酯的压滤值DFFP均不高于0.8kPa·cm 2/g，而且相比于母粒法制备的功能聚酯具有更低的压滤值，采用本发明的功能聚酯生产方法所制备的功能聚酯具有更高的功能粉体分散均匀度。 From the data in Table 1 and Table 2, it can be seen that the filter press value DFFP of the functional polyester prepared by the functional polyester production method of the present invention is not higher than 0.8 kPa·cm 2 /g, and compared with the masterbatch method The functional polyester has a lower pressure filtration value, and the functional polyester prepared by the production method of the functional polyester of the present invention has a higher uniformity of dispersion of functional powder.
本发明实施例1和对比例1制备功能聚酯所采用的颜料蓝15:3的添加量均相同，但是，实施例1中颜料蓝15:3以连续制备的功能粉体浆料浓缩物的形式加入到聚酯低聚物中再经过缩聚反应得到功能聚酯，而对比例1中颜料蓝15:3以母粒的形式加入到终缩聚反应制备得到的聚酯熔体中得到功能聚酯。对比例1的方法在制备功能聚酯时中，功能粉体在高粘聚酯熔体中难以高度均匀分散，制备得到的功能聚酯熔体的纺丝性能较差。The addition amount of the pigment blue 15:3 used in the preparation of the functional polyester in Example 1 and Comparative Example 1 of the present invention is the same, but the pigment blue 15:3 in Example 1 is a continuous preparation of the functional powder slurry concentrate Formed into the polyester oligomer and then through the polycondensation reaction to obtain a functional polyester, and in Comparative Example 1 pigment blue 15:3 in the form of masterbatch is added to the polyester melt prepared by the final polycondensation reaction to obtain a functional polyester . In the method of Comparative Example 1, in the preparation of functional polyester, the functional powder is difficult to disperse highly uniformly in the high-viscosity polyester melt, and the prepared functional polyester melt has poor spinning performance.
功能粉体分散液的制备采用研磨机，在研磨分散轴的高速旋转作用下研磨介质对功能粉体颗粒准确反复施力，使功能粉体颗粒被粉碎至纳米级，从而实现功能粉体在二元醇或水中以小尺度高效均匀分散。将功能粉体分散液与作为载体的聚酯多元醇、聚醚或聚酯低聚物等具有反应活性的双官能团化合物混合均匀后可制备得到功能粉体浆料。将功能粉体浆料输送至功能粉体浆料浓缩单元通过闪蒸脱挥处理可去除功能粉体浆料中存在的水或者过量的醇，制备得到功能粉体高度均匀分散的低压滤值、低羟值的功能粉体浆料浓缩物。将炭黑以功能粉体浆料浓缩物的形式注入聚酯生产系统可实现颜料蓝15:3粒子在聚酯基体中的高度均匀分散，有效减少功能聚酯制备过程中颜料蓝15:3粒子的团聚。The preparation of the functional powder dispersion liquid adopts a grinding machine. Under the action of the high-speed rotation of the grinding and dispersing shaft, the grinding medium accurately and repeatedly exerts force on the functional powder particles, so that the functional powder particles are crushed to the nanometer level, thereby achieving the functional powder Alcohol or water is efficiently and evenly dispersed on a small scale. The functional powder slurry can be prepared by mixing the functional powder dispersion liquid with a reactive bifunctional compound such as polyester polyol, polyether or polyester oligomer as a carrier. The functional powder slurry is transported to the functional powder slurry concentration unit, and the water or excess alcohol present in the functional powder slurry can be removed through the flash devolatilization treatment, and the low-pressure filtration value of the highly uniformly dispersed functional powder can be prepared. Low hydroxyl value functional powder slurry concentrate. Injecting carbon black in the form of functional powder slurry concentrate into the polyester production system can achieve highly uniform dispersion of pigment blue 15:3 particles in the polyester matrix, effectively reducing pigment blue 15:3 particles during the preparation of functional polyester Reunion.
实施例1中功能聚酯的压滤值DFFP为0.21kPa·cm 2/g、对比例1中功能聚酯的压滤值DFFP为1.05kPa·cm 2/g，于实施例1中颜料蓝15:3的分散得更加均匀、功能聚酯的压滤值更低，从而使得制备的功能聚酯纤维的结构更加均一、力学性能更加优异，比如，采用相同的颜料蓝15:3添加量制备相同线密度的功能聚酯纤维，实施例1制备的功能聚酯纤维的断裂强度为3.4cN/dtex，而对比例1制备的功能聚酯纤维的 断裂强度仅为2.3cN/dtex。 The filter press value DFFP of the functional polyester in Example 1 was 0.21 kPa·cm 2 /g, and the filter press value DFFP of the functional polyester in Comparative Example 1 was 1.05 kPa·cm 2 /g, in Example 1 Pigment Blue 15 :3 is more uniformly dispersed, and the functional polyester has a lower filter value, so that the functional polyester fiber prepared has a more uniform structure and better mechanical properties. For example, the same pigment blue 15:3 is used to prepare the same amount The linear polyester functional polyester fiber, the functional polyester fiber prepared in Example 1 had a breaking strength of 3.4 cN/dtex, while the functional polyester fiber prepared in Comparative Example 1 had a breaking strength of only 2.3 cN/dtex.
以上所述仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制，虽然本发明已以较佳实施例揭露如上，然而并非用以限定本发明，任何熟悉本专利的技术人员在不脱离本发明技术方案范围内，当可利用上述提示的技术内容作出些许更动或修饰为等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明方案的范围内。The above is only the preferred embodiment of the present invention, and does not limit the present invention in any form. Although the present invention has been disclosed as the preferred embodiment above, it is not intended to limit the present invention. Any technology familiar with this patent Personnel can use the technical content of the above tips to make some changes or modifications to equivalent embodiments without departing from the scope of the technical solution of the present invention, but any content that does not deviate from the technical solution of the present invention is based on the technology of the present invention In essence, any simple modifications, equivalent changes and modifications made to the above embodiments still fall within the scope of the present invention.

Claims (10)

  1. 一种功能聚酯生产系统，其特征在于，包括聚酯主体生产系统和功能粉体浆料浓缩物制备系统，所述的聚酯主体生产系统包括依次连接的酯化系统、预缩聚系统和终缩聚系统，功能粉体浆料浓缩物制备系统包括与酯化系统或/和酯化系统、预缩聚系统之间部位连接的在线添加装置。A functional polyester production system, characterized by comprising a polyester main production system and a functional powder slurry concentrate preparation system, the polyester main production system includes an esterification system, a pre-condensation system and a final connection The polycondensation system and the functional powder slurry concentrate preparation system include an online addition device connected to the esterification system or/and between the esterification system and the pre-polycondensation system.
  2. 根据权利要求1所述的功能聚酯生产系统，其特征在于，功能粉体浆料浓缩物制备系统包括依次连接的浆料制备单元、浆料浓缩单元和在线添加装置，在线添加装置的出料口与酯化系统或/和酯化系统、预缩聚系统之间部位连接。The functional polyester production system according to claim 1, wherein the functional powder slurry concentrate preparation system includes a slurry preparation unit, a slurry concentration unit and an online addition device connected in sequence, and the discharge of the online addition device The port is connected to the esterification system or/and between the esterification system and the pre-condensation system.
  3. 根据权利要求2所述的功能聚酯生产系统，其特征在于，功能粉体浆料制备单元包括载体制备单元、功能粉体分散液制备单元和混合单元，载体制备单元经计量输送装置连接功能粉体分散液制备单元，功能粉体分散液制备单元经计量输送装置连接混合单元；The functional polyester production system according to claim 2, wherein the functional powder slurry preparation unit includes a carrier preparation unit, a functional powder dispersion preparation unit and a mixing unit, and the carrier preparation unit is connected to the functional powder via a metering and conveying device A liquid dispersion preparation unit, a functional powder dispersion preparation unit is connected to a mixing unit via a metering and conveying device;
    优选地，浆料浓缩单元为具有闪蒸功能的反应釜；优选地，在线添加装置包括计量输送装置和/或混合装置，计量输送装置包括输送泵和流量计或具有计量功能的输送泵，混合装置包括静态混合器或/和动态混合器。Preferably, the slurry concentration unit is a reaction kettle with a flash evaporation function; preferably, the online addition device includes a metering conveying device and/or a mixing device, and the metering conveying device includes a conveying pump and a flow meter or a conveying pump with a metering function, mixing The device includes a static mixer or/and a dynamic mixer.
  4. 根据权利要求1-3任一项所述的功能聚酯生产系统，其特征在于，聚酯主体生产系统还包括液相增粘反应釜，终缩聚系统的出料口与液相增粘反应釜的进口连接，液相增粘反应釜的出口与纺丝设备连接；The functional polyester production system according to any one of claims 1 to 3, characterized in that the polyester main production system further comprises a liquid-phase thickening reaction kettle, the outlet of the final polycondensation system and the liquid-phase thickening reaction kettle The connection of the inlet of the liquid phase and the outlet of the liquid phase tackifying reactor are connected to the spinning equipment;
    优选地，聚酯主体生产系统的酯化系统、预缩聚系统和终缩聚系统之间经在线添加装置连接，更优选地，聚酯主体生产系统包括经在线添加装置依次连接的酯化反应釜或酯化醇解反应釜、预缩聚反应釜，终缩聚反应釜和液相增粘反应釜。Preferably, the esterification system, the pre-condensation system and the final polycondensation system of the polyester main production system are connected via an online addition device, and more preferably, the polyester main production system includes an esterification reaction kettle or Esterification alcoholysis reactor, pre-condensation reactor, final polycondensation reactor and liquid-phase thickening reactor.
  5. 一种功能聚酯的生产方法，其特征在于，包括如下步骤：A method for producing functional polyester, which is characterized by the following steps:
    S1，制备聚酯低聚物；S1, preparation of polyester oligomers;
    S2，将功能粉体分散液、载体混合均匀制备功能粉体浆料，浓缩功能粉体浆料，得到功能粉体浆料浓缩物，所述载体为具有反应活性的双官能团化合物；S2, mixing the functional powder dispersion liquid and the carrier to uniformly prepare the functional powder slurry, concentrating the functional powder slurry, and obtaining a functional powder slurry concentrate, wherein the carrier is a reactive bifunctional compound;
    S3，将功能粉体浆料浓缩物在线连续添加至聚酯低聚物中，混合均匀，进行预缩聚反应得到功能聚酯预聚物，功能聚酯预聚物经终缩聚反应，得到功能聚酯。S3: Continuously add the functional powder slurry concentrate to the polyester oligomer online, mix evenly, and perform the pre-condensation reaction to obtain the functional polyester prepolymer. The functional polyester prepolymer undergoes final polycondensation reaction to obtain the functional polymer ester.
  6. 根据权利要求5所述的生产方法，其特征在于，所述功能粉体为具有着色、抗菌、防辐射、抗菌、导电、导热、远红外、阻燃、负离子、荧光或磁性功能的粉体；所述载体选自聚酯多元醇、聚醚或聚酯低聚物。The production method according to claim 5, wherein the functional powder is a powder having functions of coloring, antibacterial, anti-radiation, antibacterial, electrically conductive, thermally conductive, far infrared, flame retardant, negative ion, fluorescent or magnetic; The carrier is selected from polyester polyols, polyethers or polyester oligomers.
  7. 根据权利要求5或6所述的生产方法，其特征在于，制备功能粉体浆料时，控制功能粉体浆料中功能粉体的平均粒径不高于1000nm，优选不高于500nm，更优选不高于300nm；The production method according to claim 5 or 6, characterized in that, when preparing the functional powder slurry, the average particle diameter of the functional powder in the functional powder slurry is controlled to be not higher than 1000 nm, preferably not higher than 500 nm, and more Preferably not higher than 300nm;
    进一步地，功能粉体浆料浓缩物中的功能粉体的含量为3％～95％，优选5％～60％，更优选10％～50％；Further, the content of the functional powder in the functional powder slurry concentrate is 3% to 95%, preferably 5% to 60%, and more preferably 10% to 50%;
    进一步地，功能粉体浆料浓缩物的羟值不高于175mgKOH/g，压滤值DFMS不高于30kPa·cm 2/g。 Further, the hydroxyl value of the functional powder slurry concentrate is not higher than 175 mgKOH/g, and the filter press value DFMS is not higher than 30 kPa·cm 2 /g.
  8. 根据权利要求5-7任一项所述的生产方法，其特征在于，制备聚酯低聚物的原料包括对苯二甲酸浆料、共聚改性单体浆料或聚酯废料，所述对苯二甲酸浆料由二元醇与对苯二甲酸按照摩尔比1.05～2.0制备得到，共聚改性单体浆料由共聚改性单体和/或二元醇为原料配制得到，所述聚酯废料为聚酯瓶废旧料及生产下脚料、聚酯膜废旧料及生产下脚料、聚酯纺织品废旧料及生产下脚料和/或聚酯纤维生产下脚料；The production method according to any one of claims 5-7, characterized in that the raw material for preparing the polyester oligomer includes terephthalic acid slurry, copolymer modified monomer slurry or polyester waste, and the The phthalic acid slurry is prepared from glycol and terephthalic acid at a molar ratio of 1.05 to 2.0. The copolymerized modified monomer slurry is prepared from copolymerized modified monomer and/or glycol as raw materials. Ester wastes are polyester bottle wastes and production scraps, polyester film wastes and production scraps, polyester textile wastes and production scraps and/or polyester fiber production scraps;
    优选地，功能聚酯预聚物的特性粘度为0.1～0.5dL/g，功能聚酯的特性粘度为0.5～1.2dL/g、压滤值DFFP不高于0.8kPa·cm 2/g。 Preferably, the intrinsic viscosity of the functional polyester prepolymer is 0.1 to 0.5 dL/g, the intrinsic viscosity of the functional polyester is 0.5 to 1.2 dL/g, and the filter press value DFFP is not higher than 0.8 kPa·cm 2 /g.
  9. 一种功能聚酯纤维，其特征在于，由权利要求1-4任一项所述的功能聚酯生产系统、权利要求5-8任一项所述的功能聚酯的生产方法得到的功能聚酯纺制而成。A functional polyester fiber, characterized in that the functional polyester obtained by the functional polyester production system according to any one of claims 1-4 and the functional polyester production method according to any one of claims 5-8 Ester spinning.
  10. 根据权利要求9所述的功能聚酯纤维，其特征在于，包括原液着色、抗菌、防辐射、抗静电、荧光、远红外、导热或负离子中的一种或几种的功能聚酯分子；优选地，功能聚酯分子为具有阳离子染料可染、亲水、仿棉、阻燃、低熔点或高收缩功能的共聚酯；The functional polyester fiber according to claim 9, characterized in that it includes one or more functional polyester molecules in stock solution coloring, antibacterial, anti-radiation, antistatic, fluorescent, far-infrared, thermal conductivity or negative ions; preferably The functional polyester molecule is a copolyester with cationic dyeable, hydrophilic, cotton-like, flame retardant, low melting point or high shrinkage functions;
    优选地，所述功能聚酯分子为聚对苯二甲酸乙二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸丁二醇酯。Preferably, the functional polyester molecules are polyethylene terephthalate, polypropylene terephthalate, and polybutylene terephthalate.
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