CN115501831A - Polyester device of full-continuous PTT and manufacturing method - Google Patents

Polyester device of full-continuous PTT and manufacturing method Download PDF

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Publication number
CN115501831A
CN115501831A CN202211239531.7A CN202211239531A CN115501831A CN 115501831 A CN115501831 A CN 115501831A CN 202211239531 A CN202211239531 A CN 202211239531A CN 115501831 A CN115501831 A CN 115501831A
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reaction kettle
polycondensation reaction
kettle
esterification reaction
esterification
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Inventor
钱桂海
王读彬
季锋
张宗正
张弛
朱素尧
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Polytex Chemical Engineering Co ltd
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Polytex Chemical Engineering Co ltd
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Priority to CN202211239531.7A priority Critical patent/CN115501831A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
    • B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • 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
    • C08G63/785—Preparation processes characterised by the apparatus used

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

The invention is suitable for the technical field of polyester material production, and provides a fully-continuous PTT polyester device, which comprises a terephthalic acid bin and a terephthalic acid metering system connected with the terephthalic acid bin, wherein the terephthalic acid bin is connected with a slurry preparation kettle through the terephthalic acid metering system, the slurry preparation kettle is also connected with a 1, 3-propylene glycol adding interface, the 1, 3-propylene glycol adding interface is connected with a mass flow meter, the slurry preparation kettle is connected with an esterification reaction system through a slurry conveying pump, the esterification reaction system is connected with a pre-polycondensation reaction system, and the pre-polycondensation reaction system is connected with a final polycondensation reaction and a pelletizing system. The device has the advantages of compact structure, reasonable process, high automation degree, high production efficiency, stable product quality and safe and stable operation. The apparatus and manufacturing method of the present invention ensure that the viscosity of the PTT product can meet higher requirements.

Description

Polyester device of full-continuous PTT and manufacturing method
Technical Field
The invention belongs to the technical field of polyester material production, and particularly relates to a full-continuous PTT polyester device and a manufacturing method thereof.
Background
PTT (polytrimethylene terephthalate) belongs to a novel high polymer polyester material.
The PTT is currently processed into PTT fibers in the largest application, and is widely applied to the fields of clothing, carpets and the like. The PTT fiber has excellent crease resistance and chemical resistance, and the strength meets the textile requirements. The excellent dyeing property is beneficial to improving the economic benefit and the environmental benefit. In addition, it has excellent flexibility, sunlight resistance, stain resistance, low static electricity, low water absorption rate, etc. The new synthetic fiber material made of PTT resin has very wide application prospect. In the application field of chemical fibers, PTT fibers integrate the softness of chinlon (and have better color fastness), the bulkiness of acrylon (so as to avoid abrasion tendency), the shape retention of terylene (but have good hand feeling), and good elasticity, antistatic property and dirt resistance, and integrate the excellent wearability of various fibers into a whole, thereby becoming one of the latest developed hot high polymer materials in the international market at present.
The PTT polyester is produced by taking phthalic acid (PTA) and 1, 3-Propanediol (PDO) as main raw materials, adding a catalyst, a delustering agent, a heat stabilizer, an antioxidant and the like, and carrying out esterification and polycondensation reactions. In the prior art, the production process flow of the PTT polyester is complex, the production process steps are multiple, and the quality of the product is unstable.
Disclosure of Invention
The embodiment of the invention aims to provide a polyester device and a manufacturing method of full-continuous PTT, and aims to solve the problems in the background technology.
The embodiment of the invention is realized in such a way that a full-continuous PTT polyester device comprises a terephthalic acid bin and a terephthalic acid metering system connected with the terephthalic acid bin, wherein the terephthalic acid bin is connected with a slurry preparation kettle through the terephthalic acid metering system, the slurry preparation kettle is also connected with a 1, 3-propanediol adding interface, the 1, 3-propanediol adding interface is connected with a mass flow meter, the slurry preparation kettle is used for stirring and mixing mixed slurry of the terephthalic acid and the 1, 3-propanediol, the slurry preparation kettle is connected with an esterification reaction system through a slurry delivery pump, the esterification reaction system is connected with a pre-polycondensation reaction system, and the pre-polycondensation reaction system is connected with a final polycondensation reaction and a pelletizing system;
the esterification reaction system comprises a first esterification reaction kettle, an esterification product delivery pump, a second esterification reaction kettle and a process tower;
the first esterification reaction kettle is used for carrying out esterification reaction on the slurry conveyed by the slurry conveying pump, and the bottom of the first esterification reaction kettle is provided with an interface for adding a catalyst and refluxing 1, 3-propylene glycol;
the esterification delivery pump is connected with the first esterification reaction kettle and is used for delivering the product esterified by the first esterification reaction kettle to the second esterification reaction kettle;
the process tower is respectively connected with the first esterification reaction kettle and the second esterification reaction kettle through gas phase pipelines and used for rectifying and separating ethylene glycol evaporated by the first esterification reaction kettle and the second esterification reaction kettle and water generated by reaction, the top of the process tower is provided with a tower top condenser, the tower top condenser is connected with a reflux tank used for collecting condensed water, the reflux tank is respectively connected with the top of the process tower and a process water storage tank, the tower bottom of the process tower is connected with a recycling 1, 3-propylene glycol filter, the recycling 1, 3-propylene glycol filter is connected with a recycling 1, 3-propylene glycol delivery pump, and the recycling 1, 3-propylene glycol delivery pump is used for delivering the 1, 3-propylene glycol to the first esterification reaction kettle, the second esterification reaction kettle and a recycling 1, 3-propylene glycol storage tank respectively;
the pre-polycondensation reaction system comprises a first pre-polycondensation reaction kettle, a first pre-polymerization 1, 3-propylene glycol spraying system, a second pre-polycondensation reaction kettle and a second pre-polymerization 1, 3-propylene glycol spraying system;
the first pre-polycondensation reaction kettle is used for further providing esterification rate for the esterified substance flowing from the second esterification reaction kettle and synchronously carrying out polycondensation reaction;
the first prepolymerization 1, 3-propylene glycol spraying system is connected with the first prepolymerization reaction kettle and is used for trapping 1, 3-propylene glycol, water and a small amount of oligomers in gas-phase components generated by the reaction in the first prepolymerization reaction kettle;
the second pre-polycondensation reaction kettle is connected with the first pre-polycondensation reaction kettle and is used for carrying out polycondensation reaction on the prepolymer which automatically flows into the first pre-polycondensation reaction kettle, and the second pre-polycondensation reaction kettle conveys the prepolymer to the final polycondensation reaction kettle through a prepolymer conveying pump;
the second pre-polymerization 1, 3-propylene glycol spraying system is connected with the second pre-polymerization reaction kettle and is used for trapping 1, 3-propylene glycol, water and a small amount of oligomers in gas-phase components generated by the second pre-polymerization reaction;
the vacuum of the first pre-polycondensation reaction system is provided by a vacuum liquid ring pump, and the vacuum of the second pre-polycondensation reaction system is provided by a final polycondensation vacuum pump system;
the final polycondensation reaction kettle is used for carrying out final polycondensation reaction on the prepolymer conveyed from the prepolymer filter;
the final polycondensation reaction system comprises a final polycondensation reaction kettle, a final polymerization 1, 3-propylene glycol spraying system and a final polymerization vacuum system;
the vacuum of the final polycondensation reaction system is provided by a 1, 3-propylene glycol vacuum jet pump and a vacuum liquid ring pump;
the pelletizing system comprises a melt conveying pump, a melt filter and an underwater strand pelletizer;
the underwater bracing and pelletizing machine is connected with a dryer used for separating and drying granular melt, the dryer is connected with a vibrating screen used for screening dried particles, the particles obtained after screening enter a slicing intermediate bin, and an automatic packaging system is adopted to carry out ton packaging on the particles;
according to a further technical scheme, the slurry preparation kettle is a vertical stirring kettle.
According to the further technical scheme, the first esterification reaction kettle is a vertical stirring kettle, a coil type internal heater for heating is arranged in the kettle, and a jacket for heat preservation is arranged outside the kettle.
According to a further technical scheme, the catalyst addition mode of the first esterification reaction kettle is as follows: diluting the catalyst with the refluxed PDO from the bottom of the reaction kettle, and adding the diluted catalyst into the reaction kettle;
in a further technical scheme, the esterification transfer pump is a gear pump.
According to a further technical scheme, the second esterification reaction kettle is a horizontal multi-chamber reaction kettle and is divided into three to four chambers, each chamber is provided with a stirrer and a coil type internal heater, and a jacket for heat preservation is arranged outside the reaction kettle.
According to a further technical scheme, the first pre-polycondensation reaction kettle is a vertical jacket vacuum reactor, a coil type internal heater is arranged inside the first pre-polycondensation reaction kettle, and a jacket is arranged outside the first pre-polycondensation reaction kettle and used for heating and heat preservation.
According to a further technical scheme, the second pre-polycondensation reaction kettle is a horizontal jacket vacuum disc reactor, a single-shaft disc stirrer is arranged in the reaction kettle, and a jacket is arranged outside the reaction kettle for heating and heat preservation.
According to the further technical scheme, the final polycondensation reaction kettle is a horizontal jacket vacuum disc reactor, a double-shaft disc stirrer is arranged in the reaction kettle, double shafts are arranged in a front-back mode, and jacket heating and heat preservation are arranged outside the reaction kettle.
Another object of an embodiment of the present invention is to provide a method for manufacturing a fully continuous PTT, comprising the steps of:
step 1, adopting full-automatic continuous pulping in the slurry preparation kettle, automatically controlling feeding of terephthalic acid (PTA) and 1, 3-Propanediol (PDO) according to a certain proportion (the molar ratio of 1, 3-propanediol to terephthalic acid is 1.15-1.5);
step 2, conveying the slurry into a first esterification reaction kettle, heating the reaction materials to the reaction temperature of 220-240 ℃, controlling the pressure to be 0.3-0.8kPaG for reaction, feeding the evaporated glycol and the water generated by the reaction into a process tower along a gas phase pipeline for rectification and separation, wherein under the action of pressure difference, the esterified substances in the first esterification reaction kettle automatically flow into a second esterification reaction kettle, the reaction temperature of 225-240 ℃ and the pressure to be 0.1-0.3kPaG;
step 3, adding a catalyst prepared from tetrabutyl titanate into the first esterification reaction kettle, feeding the catalyst, diluting the catalyst with the refluxing PDO at the bottom, and adding the diluted catalyst into the reaction kettle to reduce the degradation reaction of the catalyst;
step 4, adding reflux 1, 3-propylene glycol into the first chamber of the second esterification reaction kettle, adding a delustering agent into the second chamber (if needed), and adding additives such as a heat stabilizer, an antioxidant and the like into the latter chambers;
and 5, in the polycondensation reaction stage, the control parameters of the production process are as follows: the working temperature of the first pre-polycondensation reaction kettle is 240-250 ℃, and the working pressure is 8-10kPaA; the working temperature of the second pre-polycondensation reaction kettle is 240-250 ℃, and the working pressure is 0.8-2kPaA; the working temperature of the final polycondensation reaction kettle is 250-260 ℃, and the working pressure is 50-120PaA;
and 6, discharging and pressurizing the polyester melt at the outlet of the final polycondensation reaction kettle by adopting a gear pump, filtering the polyester melt by using a melt filter, and conveying the polyester melt to an underwater bracing granulator for underwater granulation. The slices are conveyed to a centrifugal drier by granulation water for pre-dehydration, and enter a slice intermediate bin after being separated from the abnormal slices by a vibrating screen, and the PTT slices are subjected to ton packaging by adopting an automatic packaging system.
In the step 5, the intrinsic viscosity of the prepolymer at the outlet of the first pre-polycondensation reaction kettle is 0.1-0.15dl/g.
In the step 5, the intrinsic viscosity of the prepolymer at the outlet of the second pre-polycondensation reaction kettle is 0.25 to 0.35dl/g.
In the step 5, the intrinsic viscosity of the melt at the outlet of the final polycondensation reaction kettle is 0.9-1.2dl/g.
The full-continuous PTT polyester device and the manufacturing method thereof provided by the embodiment of the invention have the advantages of compact structure, reasonable process, high automation degree, high production efficiency, stable product quality and safe and stable operation. The apparatus and manufacturing method of the present invention ensure that the viscosity of the PTT product can meet higher requirements.
Drawings
FIG. 1 is a schematic view of a partial structure of a fully continuous PTT polyester apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an esterification system in a fully continuous PTT polyester plant according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a pre-polycondensation reaction system in a full-continuous PTT polyester apparatus according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a final polycondensation reaction and pelletizing system in a fully continuous PTT polyester production apparatus according to an embodiment of the present invention.
In the drawings: a terephthalic acid bin 1; a PTA metering system 2; a slurry preparation kettle 3; a slurry transfer pump 4; a first esterification reaction kettle 5; an esterification product transfer pump 6; a second esterification reaction kettle 7; a process tower 8; an overhead condenser 9; a reflux drum 10; recycling the 1, 3-propylene glycol filter 11; a recycling 1, 3-propylene glycol delivery pump 12; a first pre-polycondensation reaction kettle 13; a first pre-polymerization 1, 3-propanediol spray system 14; a second prepolycondensation reactor 15; a second prepolymerization 1, 3-propanediol spray system 16; a prepolymer feed pump 17; a prepolymer filter 18; a final polycondensation reaction kettle 19; a finishing 1, 3-propanediol spray system 20; a melt pump 21; a melt filter 22; an underwater strand cutter 23; a dryer 24; a vibrating screen 25; a slice intermediate bin 26.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Specific implementations of the present invention are described in detail below with reference to specific embodiments.
As shown in fig. 1, a fully continuous PTT polyester apparatus provided for an embodiment of the present invention includes a terephthalic acid bin 1 and a terephthalic acid metering system 2 connected to the terephthalic acid bin 1, wherein the terephthalic acid bin 1 is connected to a slurry preparation kettle 3 through the terephthalic acid metering system 2, the slurry preparation kettle 3 is further connected to a 1, 3-propanediol adding port, the 1, 3-propanediol adding port is connected to a mass flow meter, the accurately metered PTA and the 1, 3-propanediol metered by the mass flow meter are added to the slurry preparation kettle 3 according to a certain ratio, the slurry preparation kettle 3 is configured to stir and mix a mixed slurry of terephthalic acid and 1, 3-propanediol, the mixed slurry is sent to an esterification reaction system through a slurry delivery pump 4, the esterification reaction system is connected to a pre-polycondensation reaction system, and the pre-polycondensation reaction system is connected to a final polycondensation reaction and a pellet cutting system.
As shown in fig. 2, the esterification reaction system comprises a first esterification reaction kettle 5, an esterification product delivery pump 6, a second esterification reaction kettle 7 and a process tower 8;
the first esterification reaction kettle 5 is used for carrying out esterification reaction on the slurry conveyed by the slurry conveying pump 4, and the bottom of the first esterification reaction kettle 5 is provided with an interface for adding a catalyst and refluxing 1, 3-propylene glycol;
the esterification delivery pump 6 is connected with the first esterification reaction kettle 5, and is used for delivering the product esterified by the first esterification reaction kettle 5 to the second esterification reaction kettle 7. In the second esterification reaction vessel 7, additives such as refluxing 1, 3-propanediol, a matting agent (if necessary), a heat stabilizer, an antioxidant and the like are added to the respective chambers.
The process tower 8 is respectively connected with the first esterification reaction kettle 5 and the second esterification reaction kettle 7 through gas phase pipelines, ethylene glycol evaporated by the first esterification reaction kettle 5 and the second esterification reaction kettle 7 and water generated by reaction enter the process tower 8 along the gas phase pipelines for rectification and separation, the top of the process tower 8 is provided with a tower top condenser 9, water and trace side reaction light components discharged from the top of the process tower 8 are cooled through the tower top condenser 9, the tower top condenser 9 is connected with a reflux tank 10, the water condensed by the tower top condenser 9 is collected in the reflux tank 10, the reflux tank 10 is respectively connected with the top of the process tower 8 and a process water storage tank, part of condensate in the reflux tank 10 flows back to the top of the process tower 8 for cooling, and the other part flows to a process water storage tank and is removed from a stripping tower for initial wastewater treatment. The tower bottom of the process tower 8 is connected with a recycled 1, 3-propylene glycol filter 11, the recycled 1, 3-propylene glycol filter 11 is connected with a recycled 1, 3-propylene glycol delivery pump 12, the 1, 3-propylene glycol in the tower bottom of the process tower 8 is filtered through the recycled 1, 3-propylene glycol filter 11 and then delivered through the recycled 1, 3-propylene glycol delivery pump 12, one part of the 1, 3-propylene glycol is sent to the first esterification reaction kettle 5 and the second esterification reaction kettle 7 for reflux reaction, and the rest is sent to a recycled 1, 3-propylene glycol storage tank for pulping.
As shown in fig. 3, the pre-polycondensation reaction system includes a first pre-polycondensation reaction kettle 13, a first pre-polymerization 1, 3-propylene glycol spray system 14, a second pre-polycondensation reaction kettle 15, and a second pre-polymerization 1, 3-propylene glycol spray system 16;
the first pre-polycondensation reaction kettle 13 is used for completing the esterification rate of the esterified substance flowing from the second esterification reaction kettle 7 and synchronously performing polycondensation reaction;
the first prepolymerization 1, 3-propylene glycol spraying system 14 is connected with the first prepolymerization reaction kettle 13, gas-phase components generated by the reaction in the first prepolymerization reaction kettle 13 enter the first prepolymerization 1, 3-propylene glycol spraying system 14 under the action of vacuum, the first prepolymerization 1, 3-propylene glycol spraying system 14 captures 1, 3-propylene glycol, water and a small amount of oligomers in the gas phase, and the vacuum is provided by a vacuum liquid ring pump;
the second pre-polycondensation reaction vessel 15 is connected to the first pre-polycondensation reaction vessel 13, and is configured to perform a polycondensation reaction on a prepolymer that flows in from the first pre-polycondensation reaction vessel 13. The second pre-polycondensation reaction kettle 15 is connected with a prepolymer filter 18 through a prepolymer delivery pump 17, and the reacted prepolymer passes through the prepolymer delivery pump 17, is filtered by the prepolymer filter 18, and enters a final polycondensation reaction kettle 19;
the second pre-polymerization 1, 3-propylene glycol spraying system 16 is connected with the second pre-polymerization reaction kettle 15, gas-phase components generated by the second pre-polymerization reaction enter the second pre-polymerization 1, 3-propylene glycol spraying system 16 under the action of vacuum, 1, 3-propylene glycol, water and a small amount of oligomers in the gas phase are captured, and the vacuum is provided by the final-polymerization vacuum system.
As shown in FIG. 4, the final polycondensation reaction and pelletizing system comprises a final polycondensation reaction kettle 19, a final polycondensation 1, 3-propanediol spraying system 20, a melt pump 21 and an underwater strand pelletizer 23,
the final polycondensation reaction kettle 19 is used for carrying out final polycondensation reaction on the prepolymer conveyed from the prepolymer filter 18, and the viscosity of the reacted melt is higher;
melt pump 21 is arranged in carrying the fuse-element in the final polycondensation reation kettle 19 to brace pelleter 23 under water and carries out the granulation, just still be provided with between melt pump 21 and the brace pelleter 23 under water and be used for carrying out filterable fuse-element filter 22 to the fuse-element, brace pelleter 23 under water extrudes the fuse-element into strand area through the casting tape head and restraints, is cooled by the cooling water in guider, sends into cutting device and cuts into the granule.
The underwater bracing granulator 23 is connected with a dryer 24 for separating and drying granular melt, the dryer 24 is connected with a vibrating screen 25 for screening dried particles, the particles obtained after screening enter a slicing intermediate bin 26, and an automatic packaging system is adopted to carry out ton packaging on the particles.
The gas phase component generated in the final polycondensation reaction is recovered by a final polycondensation 1, 3-propylene glycol spraying system 20, and the vacuum of the final polycondensation reaction kettle 19 and the final polycondensation 1, 3-propylene glycol spraying system 20 is provided by a polycondensation 1, 3-propylene glycol vacuum jet pump and a liquid ring vacuum pump.
As a preferred embodiment of the present invention, the slurry preparation tank 3 is a vertical stirring tank.
As a preferred embodiment of the invention, the first esterification reaction kettle 5 is a vertical stirring kettle, a coil type internal heater for heating is arranged in the kettle, and a jacket for heat preservation is arranged outside the kettle.
In a preferred embodiment of the present invention, the ester transfer pump 6 is a gear pump.
As a preferred embodiment of the invention, the second esterification reaction kettle 7 is a horizontal multi-chamber reaction kettle which is divided into 3-4 chambers, each chamber is provided with a stirrer and a coil type internal heater, and the outside of the reaction kettle is provided with a jacket for heat preservation.
As a preferred embodiment of the present invention, the first prepolycondensation reactor 13 is a vertical jacketed vacuum reactor having a coil type internal heater inside and a jacket outside for heating and holding. The second pre-polycondensation reaction kettle 15 is a horizontal jacket vacuum disc reactor, a single-shaft disc stirrer is arranged in the reaction kettle, and a jacket is arranged outside the reaction kettle for heating and heat preservation.
As a preferred embodiment of the present invention, the final polycondensation reaction kettle 19 is a horizontal jacketed vacuum disk reactor, the reaction kettle is provided with a double-shaft disk stirrer, the double shafts are arranged in front and back, and the outer part of the reaction kettle is jacketed for heating and heat preservation.
The manufacturing method of the full-continuous PTT provided by one embodiment of the invention comprises the following steps:
step 1, the slurry preparation kettle 3 adopts full-automatic continuous pulping, the feeding of terephthalic acid (PTA) and 1, 3-Propanediol (PDO) is automatically controlled according to a certain proportion (the molar ratio of the raw material 1, 3-propanediol to the terephthalic acid is 1.15-1.5).
And 2, conveying the slurry into a first esterification reaction kettle 5, heating the reaction materials to the reaction temperature of 220-240 ℃, controlling the pressure to be 0.3-0.8kPaG for reaction, feeding the evaporated glycol and water generated in the reaction into a process tower 8 along a gas phase pipeline for rectification and separation, wherein under the action of pressure difference, the esterified substances in the first esterification reaction kettle 5 automatically flow into a second esterification reaction kettle 7, the reaction temperature of the second esterification reaction kettle 7 is 225-240 ℃, and the pressure is controlled to be 0.1-0.3kPaG. The esterification rate of the first esterification reaction kettle is about 89-90%, and the esterification rate of the second esterification reaction kettle is about 95-96%.
And 3, adding a catalyst prepared from tetrabutyl titanate into the first esterification reaction kettle 5, feeding the catalyst, diluting the catalyst with the refluxing PDO at the bottom, and adding the diluted catalyst into the reaction kettle to reduce the degradation reaction of the catalyst.
And 4, adding reflux 1, 3-propylene glycol into the first chamber of the second esterification reaction kettle 7, adding a delustering agent into the second chamber (if needed), and adding additives such as a heat stabilizer, an antioxidant and the like into the latter chambers.
Step 5, in the polycondensation reaction stage, the control parameters of the production process are as follows: the working temperature of the first pre-polycondensation reaction kettle 13 is 240-250 ℃, and the working pressure is 8-10kPaA; the working temperature of the second pre-polycondensation reaction kettle 15 is 240-250 ℃, and the working pressure is 0.8-2kPaA; the working temperature of the final polycondensation reaction kettle 19 is 250-260 ℃, and the working pressure is 50-120PaA.
And 6, discharging and pressurizing the polyester melt at the outlet of the final polycondensation reaction kettle 19 by adopting a gear pump, filtering the polyester melt by using a melt filter 22, and conveying the polyester melt to an underwater strand cutting machine 23 for underwater granulation. The slices are conveyed to a centrifugal drier by granulation water for dehydration, enter a slice intermediate storage bin 26 after being separated into abnormal-shaped slices by a vibrating screen 25, and are subjected to ton packaging by adopting an automatic packaging system.
In the present example, in the step 5, the intrinsic viscosity of the prepolymer at the outlet of the first prepolycondensation reactor 13 is from 0.1 to 0.15dl/g;
in the step 5, the intrinsic viscosity of the prepolymer at the outlet of the second pre-polycondensation reaction kettle 15 is 0.25 to 0.35dl/g;
in the step 5, the intrinsic viscosity of the outlet melt of the final polycondensation reaction vessel 19 is 0.9 to 1.2dl/g.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (10)

1. A full-continuous PTT polyester device is characterized by comprising a terephthalic acid bin and a terephthalic acid metering system connected with the terephthalic acid bin, wherein the terephthalic acid bin is connected with a slurry preparation kettle through the terephthalic acid metering system, the slurry preparation kettle is also connected with a 1, 3-propanediol adding interface, the 1, 3-propanediol adding interface is connected with a mass flowmeter, the slurry preparation kettle is connected with an esterification reaction system through a slurry conveying pump, the esterification reaction system is connected with a pre-polycondensation reaction system, and the pre-polycondensation reaction system is connected with a final polycondensation reaction and a pelletizing system;
the esterification reaction system comprises a first esterification reaction kettle, an esterification product delivery pump, a second esterification reaction kettle and a process tower;
the first esterification reaction kettle is used for carrying out esterification reaction on the slurry conveyed by the slurry conveying pump, and the bottom of the first esterification reaction kettle is provided with an interface for adding a catalyst and refluxing 1, 3-propylene glycol;
the esterification delivery pump is connected with the first esterification reaction kettle and is used for delivering the product esterified by the first esterification reaction kettle to the second esterification reaction kettle;
the process tower is respectively connected with the first esterification reaction kettle and the second esterification reaction kettle through gas phase pipelines, the tower kettle of the process tower is connected with a recycled 1, 3-propylene glycol filter, and the recycled 1, 3-propylene glycol filter is connected with a recycled 1, 3-propylene glycol delivery pump;
the pre-polycondensation reaction system comprises a first pre-polycondensation reaction kettle, a first pre-polymerization 1, 3-propylene glycol spraying system, a second pre-polycondensation reaction kettle and a second pre-polymerization 1, 3-propylene glycol spraying system;
the first pre-polymerization reaction kettle is connected with the second esterification reaction kettle, and the first pre-polymerization 1, 3-propylene glycol spraying system is connected with the first pre-polymerization reaction kettle;
the second pre-polycondensation reaction kettle is connected with the first pre-polycondensation reaction kettle and conveys the prepolymer to a final polycondensation reaction through a prepolymer conveying pump;
the second pre-polymerization 1, 3-propylene glycol spraying system is connected with the second pre-polymerization reaction kettle and is used for trapping 1, 3-propylene glycol, water and a small amount of oligomers in gas-phase components generated by the second pre-polymerization reaction;
the vacuum of the first pre-polycondensation reaction system is provided by a vacuum liquid ring pump, and the vacuum of the second pre-polycondensation reaction system is provided by a final polycondensation vacuum pump system;
the final polycondensation reaction kettle is used for carrying out final polycondensation reaction on the prepolymer conveyed from the prepolymer filter;
the final polycondensation reaction system comprises a final polycondensation reaction kettle, a final polymerization 1, 3-propylene glycol spraying system and a final polymerization vacuum system;
the vacuum of the final polycondensation reaction system is provided by a 1, 3-propylene glycol vacuum jet pump and a vacuum liquid ring pump;
the pelletizing system comprises a melt conveying pump, a melt filter, an underwater strand pelletizer, a dryer and a vibrating screen;
and filtering the PTT melt produced by the final polycondensation reaction, extruding the PTT melt into a strand belt bundle through a belt casting head, cooling the strand belt bundle in a guide device by cooling water, feeding the strand belt bundle into a cutting device, cutting the strand belt bundle into particles, separating, drying and screening by a vibrating screen to obtain a PTT product.
2. The polyester device for the full-continuous PTT according to claim 1, wherein the first esterification reaction kettle is a vertical stirring kettle, a coil type internal heater for heating is arranged in the kettle, a jacket for heat preservation is arranged outside the kettle, and a catalyst feed of the first esterification reaction kettle is added into the reaction kettle after being diluted with the refluxing PDO at the bottom of the reaction kettle.
3. The full-continuous PTT polyester device according to claim 1, wherein the second esterification reaction kettle is a horizontal multi-chamber reaction kettle which is divided into three to four chambers, each chamber is provided with a stirrer and a coil type internal heater, and a jacket for heat preservation is arranged outside the reaction kettle.
4. The full-continuous PTT polyester device according to claim 1, wherein the polycondensation reaction device is carried out in three stages, and comprises a first pre-polycondensation reaction kettle, a second pre-polycondensation reaction kettle and a final polycondensation reaction kettle.
5. The full-continuous PTT polyester device according to claim 1, wherein the final polycondensation reaction kettle is a double-shaft disc vacuum reactor, the double shafts are arranged in a front-back manner, and a plurality of film-forming discs are mounted on two stirring shafts to form a two-disc stirring system, so that the viscosity of the PTT product can meet higher requirements.
6. The polyester device for the full continuous PTT according to claim 1, wherein the underwater strand cutting machine is connected with a drying machine for separating and drying granular melt, the drying machine is connected with a vibrating screen for screening dried particles, the screened particles enter a slicing intermediate bin, and an automatic packaging system is adopted for ton packaging of the particles.
7. A method for producing a fully continuous PTT, comprising the steps of:
step 1, adopting full-automatic continuous pulping in a pulp preparation kettle, wherein the raw material comprises 1.15-1.5 of 1, 3-propanediol and terephthalic acid in a molar ratio of: automatically controlling the feeding of terephthalic acid and 1, 3-propanediol, preparing slurry in a slurry preparation kettle and conveying the slurry to a first esterification reaction kettle;
step 2, conveying the slurry into a first esterification reaction kettle, heating the reaction material to the reaction temperature of 220-240 ℃, controlling the pressure to be 0.3-0.8kPaG for reaction, feeding the evaporated ethylene glycol and water generated by the reaction into a process tower along a gas phase pipeline for rectification and separation, conveying the ethylene glycol and the water through an ester conveying pump, feeding the ester in the first esterification reaction kettle into a second esterification reaction kettle, controlling the reaction temperature of 225-240 ℃ and the pressure to be 0.1-0.3kPaG;
step 3, adding a catalyst prepared from tetrabutyl titanate into the first esterification reaction kettle, feeding the catalyst, diluting the catalyst with the refluxing PDO at the bottom, and adding the diluted catalyst into the reaction kettle to reduce the degradation reaction of the catalyst;
step 4, adding reflux 1, 3-propylene glycol into the first chamber of the second esterification reaction kettle, adding a delustering agent into the second chamber, and adding various additives into the subsequent chambers;
step 5, in the polycondensation reaction stage, the control parameters of the production process are as follows: the working temperature of the first pre-polycondensation reaction kettle is 240-250 ℃, and the working pressure is 8-10kPaA; the working temperature of the second pre-polycondensation reaction kettle is 240-250 ℃, and the working pressure is 0.8-2kPaA; the working temperature of the final polycondensation reaction kettle is 250-260 ℃, and the working pressure is 50-120PaA;
and 6, discharging and pressurizing the polyester melt at the outlet of the final polycondensation reaction kettle by adopting a gear pump, filtering the polyester melt by using a melt filter, conveying the polyester melt to an underwater bracing granulator for underwater granulation, conveying the slices to a centrifugal drier for pre-dehydration by using granulation water, separating abnormal slices by using a vibrating screen, feeding the slices into a slice intermediate bin, and carrying out ton packaging on the PTT slices by adopting an automatic packaging system.
8. The process for producing a fully continuous PTT according to claim 7, wherein in the step 5, the intrinsic viscosity of the prepolymer at the outlet of the first prepolycondensation reactor is in the range of 0.1 to 0.15dl/g.
9. The process for producing a full-continuous PTT according to claim 7, wherein in said step 5, the intrinsic viscosity of the prepolymer at the outlet of the second prepolycondensation reactor is from 0.25 to 0.35dl/g.
10. The process for producing a fully continuous PTT according to claim 7, wherein in step 5, the intrinsic viscosity of the outlet melt of the final polycondensation reaction vessel is from 0.9 to 1.2dl/g.
CN202211239531.7A 2022-10-11 2022-10-11 Polyester device of full-continuous PTT and manufacturing method Pending CN115501831A (en)

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CN202211239531.7A CN115501831A (en) 2022-10-11 2022-10-11 Polyester device of full-continuous PTT and manufacturing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211239531.7A CN115501831A (en) 2022-10-11 2022-10-11 Polyester device of full-continuous PTT and manufacturing method

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CN115501831A true CN115501831A (en) 2022-12-23

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