CN103147163A - Skin-core type recycled polyester staple fiber and preparation method thereof - Google Patents
Skin-core type recycled polyester staple fiber and preparation method thereof Download PDFInfo
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- CN103147163A CN103147163A CN2013100916973A CN201310091697A CN103147163A CN 103147163 A CN103147163 A CN 103147163A CN 2013100916973 A CN2013100916973 A CN 2013100916973A CN 201310091697 A CN201310091697 A CN 201310091697A CN 103147163 A CN103147163 A CN 103147163A
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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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- 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
- D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
- D01F13/04—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of synthetic polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to a skin-core type recycled polyester staple fiber and a preparation method thereof. The recycled polyester staple fiber is formed by a skin layer and a core layer, wherein the skin layer is low-melting-point recycled polyester; the melting point of the low-melting-point recycled polyester is 70-160 DEG C; the content of a carboxylic end group is smaller than or equal to 35mmol/kg; the intrinsic viscosity is 0.5-1.0dL/g; the core layer is a high-melting point recycled polyester; the melting point of the high-melting-point recycled polyester is 250-270 DEG C; the content of the carboxylic end group is smaller than or equal to 20mmol/kg; the intrinsic viscosity is 0.7-1.0dL/g; two polyester melts enter a composite spinning component after being metered by each metering pump; the melt jetted from a spinneret plate of the composite component is cooled, wound, bundled, drawn, sized, cut off and packaged to obtain the skin-core type recycled polyester staple fiber. The skin-core type recycled polyester staple fiber prepared by the method disclosed by the invention is stable in quality and excellent in quality.
Description
Technical field
The present invention relates to belong to the chemical fibre production technical field, relate in particular to a kind of core-skin type regenerative polyester staple fiber and preparation method thereof.
Background technology
Low melting point core-skin type complex polyester staple fibre refers to be distributed in low-melting point polyester and these two kinds of different polymer of normal polyester the fiber of making among same fiber with skin-core structure.Cortex is low-melting point polyester, and it has kept the part of properties of normal polyester, has the characteristics of good compatibility with normal polyester.The low melting point core-skin composite fiber is mainly used in heat-bondable fiber, and Main Function is low-melting fiber cortex polymer fusing at a certain temperature in non-weaving cloth production, coheres effect thereby play in fiber web.Intensity is high, bulkiness good, elastic restoration ratio is high because low-melting point polyester staple fiber has, and the non-weaving cloth of producing has soft, elasticity high is widely used in the fields such as the hygienic materials such as surgical mask, bandage and house decorative material at present.
Production method for low-melting point polyester staple fiber has more research report at present.As patent of invention " a kind of copolyester with low melting point and preparation method thereof " (application number: the method for designing that 200810063395.4) discloses copolyester with low melting point, melting point polyester can be down to 110 ℃, and this copolyester with low melting point crystal property is good, inherent viscosity is high, particle is difficult for adhesion, have good spinnability etc.Patent of invention " a kind of production method of low-melting point polyester staple fiber " (application number: 200410072878.2) adopt 120 ℃～130 ℃ low melting point polyester chips through after low-temperature vacuum drying, can get the low melting point staple fibre through melt spinning.(application number: 200810123792.6) disclosed is water-soluble polyester component and the polytrimethylene terephthalate component low melting point short fiber that is composited side by side to patent of invention " the low melting point short fiber that a kind of parallel type is compound ", and this fiber has good percent thermal shrinkage stability.Research about low melting point core-sheath polyester fiber also has some reports.As patent of invention " a kind of production method of sheath-core type low-melting point polyester staple fiber " (application number: 200810163542.5) it is characterized in that cortex is the low-melting point polyester melt that obtains by fused mass directly spinning, the conventional PET polyester fondant of sandwich layer for obtaining by conventional PET section spinning process.But utilizing reworked material to prepare polyester staple fiber does not report so far as the sandwich layer of core-sheath compound fibre.
Along with polyester material developing rapidly and using in each field, the discharge capacity of polyester waste material grows with each passing day, its refractory organics has now caused great pollution to environment, and due to the present shortage of the raw material of industry, and the recycling of polyester waste material has been become the required of sustainable development society.Most of for low additional fields such as fillers with the staple fibre of polyester waste material preparation at present.Study modified accent adhering process, solve that the polyester waste material source is wide, complicated component, technical barrier that quality fluctuation is large, utilize the polyester waste material preparation to have the key subjects that high value-added product becomes upgrading transition of regeneration industry.In addition, this technology substitutes the spinning of eutectic polyester slice with fused mass directly spinning, the series of problems such as preferably resolve that the low-melting point polyester drying cost is large, poor stability, fiber spinnability are poor, and production cost declines to a great extent.
Summary of the invention
Utilize reworked material to prepare the technical problem that polyester sheath core type composite fibre exists in order to solve, one object of the present invention is to provide a kind of preparation method of core-skin type regenerative polyester staple fiber, the method has improved the added value that polyester waste material prepares regenerative polyester staple fiber, the core-skin type regenerative polyester staple fiber of preparation has steady quality, colory characteristics.Another object of the present invention is to provide the regenerative polyester staple fiber that adopts above-mentioned method preparation.
In order to realize first above-mentioned purpose, the present invention has adopted following technical scheme:
A kind of preparation method of core-skin type regenerative polyester staple fiber, this regenerative polyester staple fiber is made of cortex and sandwich layer, and cortex weight accounts for 10%～90% of composite fibre gross weight, and sandwich layer is completely wrapped in cortex; Cortex is the low melting point recycled polyester that reworked material prepares by the modified poly of degrading again, and the fusing point of low melting point recycled polyester is 70～160 ℃, content of carboxyl end group≤35 mmol/kg, and inherent viscosity is 0.5dL/g～1.OdL/g; Sandwich layer is the high-melting-point recycled polyester that reworked material passes through modified accent adhering process preparation, and the fusing point of described high-melting-point recycled polyester is 250～270 ℃, content of carboxyl end group≤20mmol/kg, and inherent viscosity is 0.7dl/g～1.0 dl/g; Two kinds of polyester fondants are by entering composite spinneret pack after the measuring pump metering separately, and the melt that sprays from the spinnerets of composite component through cooling, coiling, boundling, drawing-off, typing, cut-out and packing, can get the core-skin type regenerative polyester staple fiber.
As preferably, the inherent viscosity of described low melting point recycled polyester is 0.55dL/g ~ 0.75dL/g, and the inherent viscosity of high-melting-point recycled polyester is 0.75dl/g～0.85dl/g.
As preferably, described regeneration low-melting point polyester makes by degraded and polycondensation reaction for following raw material:
A. regenerative raw materials;
B. methyl alcohol, water or ethylene glycol;
C. one or more in zinc acetate, potassium acetate, manganese acetate, magnesium acetate, lead acetate, cobalt chloride, butyl titanate, tetraisopropyl titanate and the basic tin laurate of fourth two;
D. M-phthalic acid, one or more in adipic acid and decanedioic acid;
E. neopentyl glycol, hexylene glycol, one or more in butanediol and polyethylene glycol;
F. the catalytic antimony trioxide and cobalt acetate;
G. stabilizing agent trimethyl phosphate;
Select following a kind of method preparation regeneration low-melting point polyester according to the b raw material:
One, methyl alcohol alcoholysis method
1) with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:4～14, the mass ratio of a and c is 100:0.5～1; Degradation temperature is 170～250 ℃, pressure is 1.5～4.0Mpa, reaction time is 2.5～5h, when equal pressure is got back to atmospheric pressure, reaction finishes, reactant is filtered, and the liquid in rotation evaporation that obtains boils off respectively methyl alcohol and ethylene glycol, the solids that obtains is dissolved in hot ethanol and filters, and gained liquid boils off ethanol and obtains dimethyl terephthalate (DMT);
2) esterification of dimethyl terephthalate (DMT) and ethylene glycol adds to depress at nitrogen and carries out, and the molar ratio of dimethyl terephthalate (DMT) and d is 2～5:1; The molar ratio of dimethyl terephthalate (DMT) and e is 3～19:1; The mol ratio of dimethyl terephthalate (DMT) and ethylene glycol is: 20:80～80:20; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of sour total amount, and described alcohol is the summation of ethylene glycol and e; The temperature of esterification is 180～250 ℃, and pressure is 0.05MPa～0.4MPa, reaction time 1.5～3h; The polycondensation reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h;
Two, Hydrolyze method
1) hydrolysis: with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:1～5, the mass ratio of a and c is 100:0.5～1; Reaction temperature is 190～280 ℃, pressure is 3.0～6.0Mpa, reaction time is 2～5h, when reaction end equal pressure is got back to atmospheric pressure, reactant is filtered, gained liquid in rotation evaporation obtains ethylene glycol, then will filter solids and be dissolved in DMF and filtering, and gained liquid is recrystallized and obtains terephthalic acid (TPA);
2) esterification of terephthalic acid (TPA) and ethylene glycol adds to depress at nitrogen and carries out, and the molar ratio of terephthalic acid (TPA) and d is 2～5:1; The molar ratio of terephthalic acid (TPA) and e is 3～19:1; The mol ratio of terephthalic acid (TPA) and ethylene glycol is: 20:80～80:20; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of acid; Described alcohol is the summation of ethylene glycol and e, and described acid is the summation of terephthalic acid (TPA) and d; The temperature of esterification is 180-250 ℃, and pressure is 0.05MPa～0.4MPa, reaction time 1.5～3h; The polycondensation reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h;
Three, glycolysis method
1) with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:1～4; The mass ratio of a and c is 100:0.5～1; Carry out under nitrogen pressurization or condition of normal pressure, reaction temperature is 170～220 ℃, and pressure is 0 ℃ of 0.4MPa, and the reaction time is 1.5～3h, until the inherent viscosity of reactant liquor reaches 0.2～0.35dl/g; After reaction finishes, the reactant liquor Rapid Thermal is filtered, filtrate is carried out decompression distillation reclaim ethylene glycol, the liquid after decompression distillation is dissolved in heat alcohol, ester, chlorinated hydrocabon or ketone solvent, heat filtering is gone out insoluble matter, naturally cooling ethylene glycol terephthalate and the oligomer thereof of obtaining of filtrate;
2) polycondensation reaction of ethylene glycol terephthalate and oligomer thereof, the molar weight that feeds intake of d is the quality of quality/960-a of a/384; The molar weight that feeds intake of e is the quality/576 of quality/1728-a of a; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of sour total amount, and reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h.
As further improvement, described recycled polyester prepares by modified accent adhering process take polyester bottle slice as main recovery polyester raw material, concrete technology is as follows: regenerative raw materials-cleaning-proportioning-drum dried-multistage filtering-liquid-phase tackifying, wherein, the drum dried temperature is 100 ~ 150 ℃, and be 7 ~ 10h drying time.
As further improvement, the step of described liquid-phase tackifying is as follows:
1) temperature after the screw rod melting is 0.5dl/g ~ 0.70dl/g 260 ℃ ~ 290 ℃ inherent viscosities melt is pumped to the vacuum separation tower through melt Conveying, melt is 10pa ~ 400pa in vacuum, temperature is 270 ℃ ~ 300 ℃, stops under condition that inherent viscosity can reach 0.55dl/g ~ 0.78dl/g after 15min ~ 40min;
2) melt enters the sticking device of the modified accent of secondary afterwards, melt temperature in the sticking device of the modified accent of secondary is identical with the vacuum separation tower with vacuum, melt constantly advances under the effect of rotatable propeller, melt viscosity constantly increases, angle of rake rotary speed is 1.5r/min ~ 10r/min, time of staying 15min ~ 30min, final melt characteristic viscosity is at 0.60dl/g ~ 0.88dl/g.
Liquid-phase tackifying process using Chinese invention patent of the present invention (application number: 201010574044.7, the applying date: 2010-12-01) the modified accent of described a kind of waste plastics glues system.
As further improvement, described recovery polyester raw material also comprises the useless polyester-containing textiles that mixes.
The control of spinning temperature is the key of production low melting point core-skin type composite short fiber, should consider the material characteristic that cortex is different with sandwich layer, to two kinds of component pipelines and spin manifold temperature, adopts different temperature to control.After two kinds of melts meet at main box, should control by adaptable temperature both.As further improvement, described low-melting point polyester spinning pipeline holding temperature is 220～240 ℃; 270～300 ℃ of the extruder temperatures of recycled polyester, recycled polyester spinning pipeline holding temperature is 270-290 ℃, spinning body temperature is 270～290 ℃.
The compounding flux thread is in spinning shaft, and through quenching, melt viscosity increases gradually until solidified forming.If cooling insufficient, go out after spinneret orifice because the cortex fusing point is lower, as-spun fibre is molten state, can stick to connect together.As further improvement, described cooling employing ring blowing is carried out, and wind-warm syndrome is 15～32 ℃, and wind speed is 0.5～5.0m/s, and spinning speed is 800～1200m/min.
As further improvement, the draw ratio of described drawing-off is 1.2～3.5, and 50～72 ℃ of drawing temperatures, draft speed are 100～150m/min.
In order to realize second above-mentioned purpose, the regenerative polyester staple fiber that the present invention also provides above-mentioned preparation method to prepare.
The core-skin type regenerative polyester staple fiber steady quality of the inventive method preparation, best in quality, can be used for producing in the industries such as non-weaving cloth, flocking, composite.
The specific embodiment
Embodiment 1
1, the preparation of regeneration low-melting point polyester: the mass ratio that feeds intake of regenerative raw materials and methyl alcohol is 1:6; The mass ratio of regenerative raw materials and zinc acetate is 100:0.5; Above raw material by the methyl alcohol alcoholysis after polymerization preparation regeneration low-melting point polyester: degradation temperature is 190 ℃, pressure is 2.5Mpa, reaction time is 3h, when equal pressure is got back to atmospheric pressure, reaction finishes, reactant is filtered, and the liquid in rotation evaporation that obtains boils off respectively methyl alcohol and ethylene glycol, the solids that obtains is dissolved in hot ethanol and filters, and gained liquid boils off ethanol and obtains dimethyl terephthalate (DMT) (DMT).Dimethyl terephthalate (DMT) (DMT) is 3:1 with the molar ratio of M-phthalic acid (IPA); Dimethyl terephthalate (DMT) (DMT) is 7:1 with the molar ratio of neopentyl glycol (NPG); Dimethyl terephthalate (DMT) (DMT) is 1:2 with the mol ratio of ethylene glycol; The molar ratio of alcohol (summation of ethylene glycol and neopentyl glycol (NPG)) acid is 1.5:1; The catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) are the 300ppm of sour total amount in reaction system, then to add weight be the stabilizing agent trimethyl phosphate (TMP) of 0.01% (relatively sour composition).Esterification adds to depress at nitrogen carries out, and temperature is 220 ℃, and pressure is 0.15MPa, reaction time 2.2h; The polycondensation reaction temperature is 275 ℃, and vacuum is 90Pa, reaction time 3.5h.The fusing point of the low-melting point polyester that obtains is 110 ℃, and content of carboxyl end group is 25mmol/kg, and inherent viscosity is 0.69dL/g.
2, the preparation of recycled polyester: adopt bottle chips through the technological process of cleaning, drum dried, multistage filtering, liquid-phase tackifying.Wherein, the drum dried temperature is 130 ℃, and be 8h drying time.The step of liquid-phase tackifying is as follows: 1) temperature after the screw rod melting is 0.55dl/g 270 ℃ of inherent viscosities melt is pumped to the vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 ℃, stop 30min under condition after inherent viscosity can reach 0.68dl/g; 2) melt enters the sticking device of the modified accent of secondary afterwards, melt temperature in the sticking device of the modified accent of secondary is identical with the vacuum separation tower with vacuum, melt constantly advances under the effect of rotatable propeller, melt viscosity constantly increases, angle of rake rotary speed is 5r/min, time of staying 20min, final melt characteristic viscosity is at 0.79dl/g.The fusing point of recycled polyester is 264 ℃, and content of carboxyl end group is 16 mmol/kg, and inherent viscosity is 0.79dl/g.
3, core-skin type regenerative polyester staple fiber: above-mentioned low-melting point polyester and recycled polyester are entered composite spinneret pack with the accurate measurement of 4:6 core-skin weight respectively, the melt that sprays from the spinnerets of composite component, through cooling, coiling, boundling, drawing-off, typing, cut-out and packing, can get the core-skin type regenerative polyester staple fiber.The baking temperature of recycled polyester is 150 ℃, and be 7h drying time, 280 ℃ of extruder temperatures; Low-melting point polyester spinning pipeline holding temperature is 230 ℃, and recycled polyester spinning pipeline holding temperature is 275 ℃, and spinning body temperature is 280 ℃; Ring quenching wind-warm syndrome is 15 ℃, and wind speed is 2.0m/s; Spinning speed is 1100m/min; Draw ratio is 2.0, and 60 ℃ of drawing temperatures, draft speed are 110m/min.The core-skin type regenerative polyester staple fiber quality index that obtains through above-mentioned production technology is:
Line density: 4.21dtex
Fracture strength: 3.14cN/dtex
Elongation at break: 40%
Shearing length: 51.2mm.
Embodiment 2
1, the preparation of regeneration low-melting point polyester: the mass ratio that feeds intake of regenerative raw materials and water is 1:4; The mass ratio of regenerative raw materials and potassium acetate is 100:0.5; Above raw material prepares the regeneration low-melting point polyester by the rear polymerization of hydrolysis: hydrolysis temperature is 220 ℃, pressure is 4.5Mpa, reaction time is 2.8h, when reaction end equal pressure is got back to atmospheric pressure, reactant is filtered, gained liquid in rotation evaporation obtains ethylene glycol, then will filter solids and be dissolved in DMF and filtering, and gained liquid is recrystallized and obtains terephthalic acid (TPA) (TPA).Terephthalic acid (TPA) (TPA) is 3.5:1 with the molar ratio of adipic acid (AA); Terephthalic acid (TPA) (TPA) is 6:1 with the molar ratio of hexylene glycol (HG); Terephthalic acid (TPA) (TPA) is 1.5:1 with the mol ratio of ethylene glycol; The molar ratio of alkyd is 1.5:1; The catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) are the 300ppm of sour total amount in reaction system, then to add weight be the stabilizing agent trimethyl phosphate (TMP) of 0.01% (relatively sour composition).Esterification adds to depress at nitrogen carries out, and temperature is 220 ℃, and pressure is 0.3MPa, reaction time 2.5h; The polycondensation reaction temperature is 275 ℃, and vacuum is 80Pa, and reaction time 3h, the fusing point of the low-melting point polyester that obtains are 105 ℃, and content of carboxyl end group is 28mmol/kg, and inherent viscosity is 0.67dL/g.
2, the preparation of recycled polyester: adopt bottle chips through the technological process of cleaning, drum dried, multistage filtering, liquid-phase tackifying.Wherein, the drum dried temperature is 110 ℃, and be 7h drying time.The step of liquid-phase tackifying is as follows: 1) temperature after the screw rod melting is 0.55dl/g 270 ℃ of inherent viscosities melt is pumped to the vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 ℃, stop 30min under condition after inherent viscosity can reach 0.68dl/g; 2) melt enters the sticking device of the modified accent of secondary afterwards, melt temperature in the sticking device of the modified accent of secondary is identical with the vacuum separation tower with vacuum, melt constantly advances under the effect of rotatable propeller, melt viscosity constantly increases, angle of rake rotary speed is 5r/min, time of staying 15min, final melt characteristic viscosity is at 0.78dl/g.The fusing point of recycled polyester is 269 ℃, and content of carboxyl end group is 14 mmol/kg, and inherent viscosity is 0.78dl/g.
3, core-skin type regenerative polyester staple fiber: above-mentioned low-melting point polyester and recycled polyester are entered composite spinneret pack with the accurate measurement of 5:5 core-skin weight respectively, the melt that sprays from the spinnerets of composite component, through cooling, coiling, boundling, drawing-off, typing, cut-out and packing, can get the core-skin type regenerative polyester staple fiber.The baking temperature of recycled polyester raw material is 140 ℃, and be 7.5h drying time, 270 ℃ of extruder temperatures; Low-melting point polyester spinning pipeline holding temperature is 220 ℃, and recycled polyester spinning pipeline holding temperature is 275 ℃, and spinning body temperature is 280 ℃; Ring quenching wind-warm syndrome is 20 ℃, and wind speed is 3.0m/s; Spinning speed is 1000m/min; Draw ratio is 3.0, and 56 ℃ of drawing temperatures, draft speed are 120m/min.The core-skin type regenerative polyester staple fiber quality index that obtains through above-mentioned production technology is:
Line density: 4.05dtex
Fracture strength: 3.22cN/dtex
Elongation at break: 42%
Shearing length: 51.6mm.
Embodiment 3
1, the preparation of regeneration low-melting point polyester: the mass ratio that feeds intake of regenerative raw materials and ethylene glycol is 1:3.5; The mass ratio of regenerative raw materials and fourth two basic tin laurates is 100:0.5; The alcoholysis reaction temperature is 196 ℃, and pressure is 0.15MPa, and the reaction time is 2h, and the inherent viscosity of reactant liquor reaches 0.29dl/g.After reaction finishes, the reactant liquor Rapid Thermal is filtered, filtrate is carried out decompression distillation reclaim ethylene glycol, liquid after decompression distillation (being solid under normal temperature) is dissolved in heat alcohol, ester, chlorinated hydrocabon, ketone equal solvent, heat filtering is gone out insoluble matter, naturally cooling ethylene glycol terephthalate (BHET) and the oligomer thereof of obtaining of filtrate.Add M-phthalic acid (IPA), neopentyl glycol (NPG), the catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) and stabilizing agent trimethyl phosphate (TMP) in ethylene glycol terephthalate (BHET) and oligomer thereof, carry out polycondensation reaction, the polycondensation reaction temperature of ethylene glycol terephthalate (BHET) and oligomer thereof is 275 ℃, vacuum is 95Pa, reaction time 3.5h.The fusing point of the low-melting point polyester that obtains is 115 ℃, and content of carboxyl end group is 30mmol/kg, and inherent viscosity is 0.68dL/g.The molar weight that feeds intake of M-phthalic acid (IPA) is the quality/450 of regenerative raw materials; The molar weight that feeds intake of neopentyl glycol (NPG) is regenerative raw materials quality/960; The molar ratio of alkyd is 1.4; The catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) are the 400ppm of sour total amount in reaction system, then to add weight be the stabilizing agent trimethyl phosphate (TMP) of 0.01% (relatively sour composition).
2, the preparation of recycled polyester: adopt bottle chips through the technological process of cleaning, drum dried, multistage filtering, liquid-phase tackifying.Wherein, the drum dried temperature is 100 ℃, and be 7h drying time.The step of liquid-phase tackifying is as follows: 1) temperature after the screw rod melting is 0.55dl/g 270 ℃ of inherent viscosities melt is pumped to the vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 ℃, stop 30min under condition after inherent viscosity can reach 0.68dl/g; 2) melt enters the sticking device of the modified accent of secondary afterwards, melt temperature in the sticking device of the modified accent of secondary is identical with the vacuum separation tower with vacuum, melt constantly advances under the effect of rotatable propeller, melt viscosity constantly increases, angle of rake rotary speed is 5r/min, time of staying 15min, final melt characteristic viscosity is at 0.78dl/g.The fusing point of recycled polyester is 267 ℃, and content of carboxyl end group is 16 mmol/kg, and inherent viscosity is 0.78dl/g.
3, core-skin type regenerative polyester staple fiber: above-mentioned low-melting point polyester and recycled polyester are entered composite spinneret pack with the accurate measurement of 6:4 core-skin weight respectively, the melt that sprays from the spinnerets of composite component, through cooling, coiling, boundling, drawing-off, typing, cut-out and packing, can get the core-skin type regenerative polyester staple fiber.The baking temperature of recycled polyester raw material is 140 ℃, and be 7h drying time, 280 ℃ of extruder temperatures; Low-melting point polyester spinning pipeline holding temperature is 230 ℃, and recycled polyester spinning pipeline holding temperature is 270 ℃, and spinning body temperature is 285 ℃; Ring quenching wind-warm syndrome is 22 ℃, and wind speed is 2.5m/s; Spinning speed is 900m/min; Draw ratio is 2.5, and 58 ℃ of drawing temperatures, draft speed are 110m/min.The core-skin type regenerative polyester staple fiber quality index that obtains through above-mentioned production technology is:
Line density: 4.24 dtex
Fracture strength: 2.67 cN/dtex
Elongation at break: 47%
Shearing length: 50.8mm.
Claims (9)
1. the preparation method of a core-skin type regenerative polyester staple fiber, this regenerative polyester staple fiber is made of cortex and sandwich layer, and cortex weight accounts for 10%～90% of composite fibre gross weight, and sandwich layer is completely wrapped in cortex; It is characterized in that: cortex is the low melting point recycled polyester that reworked material prepares by the modified poly of degrading again, and the fusing point of low melting point recycled polyester is 70～160 ℃, content of carboxyl end group≤35mmol/kg, and inherent viscosity is 0.5dL/g ~ 1.OdL/g; Sandwich layer is the high-melting-point recycled polyester that reworked material passes through modified accent adhering process preparation, and the fusing point of described high-melting-point recycled polyester is 250～270 ℃, content of carboxyl end group≤20mmol/kg, and inherent viscosity is 0.7dl/g～1.0dl/g; Two kinds of polyester fondants are by entering composite spinneret pack after the measuring pump metering separately, and the melt that sprays from the spinnerets of composite component through cooling, coiling, boundling, drawing-off, typing, cut-out and packing, can get the sheath-core type low-melting point regenerative polyester staple fiber.
2. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, the inherent viscosity that it is characterized in that the low melting point recycled polyester is 0.55dL/g ~ 0.75dL/g, the inherent viscosity of high-melting-point recycled polyester is 0.75dl/g～0.85dl/g.
3. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1 is characterized in that described low melting point recycled polyester makes by degraded and polycondensation reaction for following raw material:
A. regenerative raw materials;
B. methyl alcohol, water or ethylene glycol;
C. one or more in zinc acetate, potassium acetate, manganese acetate, magnesium acetate, lead acetate, cobalt chloride, butyl titanate, tetraisopropyl titanate and the basic tin laurate of fourth two;
D. M-phthalic acid, one or more in adipic acid and decanedioic acid;
E. neopentyl glycol, hexylene glycol, one or more in butanediol and polyethylene glycol;
F. the catalytic antimony trioxide and cobalt acetate;
G. stabilizing agent trimethyl phosphate;
Select following a kind of method preparation regeneration low-melting point polyester according to the b raw material:
One, methyl alcohol alcoholysis method
1) with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:4～14, the mass ratio of a and c is 100:0.5～1; Degradation temperature is 170～250 ℃, pressure is 1.5～4.0Mpa, reaction time is 2.5～5h, when equal pressure is got back to atmospheric pressure, reaction finishes, reactant is filtered, and the liquid in rotation evaporation that obtains boils off respectively methyl alcohol and ethylene glycol, the solids that obtains is dissolved in hot ethanol and filters, and gained liquid boils off ethanol and obtains dimethyl terephthalate (DMT);
2) esterification of dimethyl terephthalate (DMT) and ethylene glycol adds to depress at nitrogen and carries out, and the molar ratio of dimethyl terephthalate (DMT) and d is 2～5:1; The molar ratio of dimethyl terephthalate (DMT) and e is 3～19:1; The mol ratio of dimethyl terephthalate (DMT) and ethylene glycol is: 20:80～80:20; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of sour total amount, and described alcohol is the summation of ethylene glycol and e; The temperature of esterification is 180～250 ℃, and pressure is 0.05MPa～0.4MPa, reaction time 1.5～3h; The polycondensation reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h;
Two, Hydrolyze method
1) hydrolysis: with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:1～5, the mass ratio of a and c is 100:0.5～1; Reaction temperature is 190～280 ℃, pressure is 3.0～6.0Mpa, reaction time is 2～5h, when reaction end equal pressure is got back to atmospheric pressure, reactant is filtered, gained liquid in rotation evaporation obtains ethylene glycol, then will filter solids and be dissolved in DMF and filtering, and gained liquid is recrystallized and obtains terephthalic acid (TPA);
2) esterification of terephthalic acid (TPA) and ethylene glycol adds to depress at nitrogen and carries out, and the molar ratio of terephthalic acid (TPA) and d is 2～5:1; The molar ratio of terephthalic acid (TPA) and e is 3～19:1; The mol ratio of terephthalic acid (TPA) and ethylene glycol is: 20:80～80:20; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of acid; Described alcohol is the summation of ethylene glycol and e, and described acid is the summation of terephthalic acid (TPA) and d; The temperature of esterification is 180 ~ 250 ℃, and pressure is 0.05MPa～0.4MPa, reaction time 1.5～3h; The polycondensation reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h;
Three, glycolysis method
1) with a, b with mix after c feeds intake, the mass ratio that feeds intake of a and b is 1:1～4; The mass ratio of a and c is 100:0.5～1; Carry out under nitrogen pressurization or condition of normal pressure, reaction temperature is 170～220 ℃, and pressure is 0 ℃ of 0.4MPa, and the reaction time is 1.5～3h, until the inherent viscosity of reactant liquor reaches 0.2～0.35dl/g; After reaction finishes, the reactant liquor Rapid Thermal is filtered, filtrate is carried out decompression distillation reclaim ethylene glycol, the liquid after decompression distillation is dissolved in heat alcohol, ester, chlorinated hydrocabon or ketone solvent, heat filtering is gone out insoluble matter, naturally cooling ethylene glycol terephthalate and the oligomer thereof of obtaining of filtrate;
2) polycondensation reaction of ethylene glycol terephthalate and oligomer thereof, the molar weight that feeds intake of d is the quality of the quality of a/960 ~ a/384; The molar weight that feeds intake of e is the quality/576 of the quality/1728 ~ a of a; The molar ratio of alkyd is 1.4～1.6:1; Feeding intake of f and g is 200～600ppm of sour total amount, and reaction temperature is 250～285 ℃, and vacuum is 30～200Pa, reaction time 2.5～5h.
4. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, it is characterized in that: recycled polyester prepares by modified accent adhering process take polyester bottle slice as main recovery polyester raw material, concrete technology is as follows: regenerative raw materials-cleaning-proportioning-drum dried-multistage filtering-liquid-phase tackifying, wherein, the drum dried temperature is 100 ~ 150 ℃, and be 7 ~ 10h drying time.
5. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 4 is characterized in that the step of liquid-phase tackifying is as follows:
1) temperature after the screw rod melting is 0.5dl/g ~ 0.70dl/g 260 ℃ ~ 290 ℃ inherent viscosities melt is pumped to the vacuum separation tower through melt Conveying, melt is 10pa ~ 400pa in vacuum, temperature is 270 ℃ ~ 300 ℃, stops under condition that inherent viscosity can reach 0.55dl/g ~ 0.78dl/g after 15min ~ 40min;
2) melt enters the sticking device of the modified accent of secondary afterwards, melt temperature in the sticking device of the modified accent of secondary is identical with the vacuum separation tower with vacuum, melt constantly advances under the effect of rotatable propeller, melt viscosity constantly increases, angle of rake rotary speed is 1.5r/min ~ 10r/min, time of staying 15min ~ 30min, final melt characteristic viscosity is at 0.60dl/g ~ 0.88dl/g.
6. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, it is characterized in that: low-melting point polyester spinning pipeline holding temperature is 220～240 ℃; 270～300 ℃ of the extruder temperatures of recycled polyester, recycled polyester spinning pipeline holding temperature is 270 ~ 290 ℃, spinning body temperature is 270 ~ 290 ℃.
7. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1 is characterized in that: cooling employing ring blowing is carried out, and wind-warm syndrome is 15～32 ℃, and wind speed is 0.5～5.0m/s, and spinning speed is 800～1200m/min.
8. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, it is characterized in that: the draw ratio of drawing-off is 1.2～3.5,50～72 ℃ of drawing temperatures, draft speed are 100～150m/min.
9. the regenerative polyester staple fiber for preparing of according to claim 1 ~ 8 described preparation methods of any one claim.
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