CN103147163B - 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
- Publication number
- CN103147163B CN103147163B CN201310091697.3A CN201310091697A CN103147163B CN 103147163 B CN103147163 B CN 103147163B CN 201310091697 A CN201310091697 A CN 201310091697A CN 103147163 B CN103147163 B CN 103147163B
- Authority
- CN
- China
- Prior art keywords
- polyester
- temperature
- staple fiber
- ethylene glycol
- recycled polyester
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
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 and belong to experimental branch line technical field, particularly relate 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 that the polymer with low-melting point polyester is different with normal polyester these two kinds is distributed in the fiber made among same fiber with skin-core structure.Cortex is low-melting point polyester, it preserves the part of properties of normal polyester, has the feature of good compatibility with normal polyester.Low melting point core-skin composite fiber is mainly used in heat-bondable fiber, and in non-weaving cloth is produced, Main Function is low-melting fiber cortex polymer fusing at a certain temperature, thus plays in fiber web and cohere effect.Because low-melting point polyester staple fiber has, intensity is high, bulkiness good, elastic restoration ratio is high, and the non-weaving cloth produced has soft, elasticity high, is widely used in the fields such as the hygienic material such as surgical mask, bandage and house decorative material at present.
Production method at present for low-melting point polyester staple fiber has more research report.As patent of invention " a kind of copolyester with low melting point and preparation method thereof " (application number: the method for designing 200810063395.4) disclosing copolyester with low melting point, melting point polyester can be down to 110 DEG C, and this copolyester with low melting point crystal property is good, inherent viscosity is high, particle not easily 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 DEG C ~ 130 DEG C low melting point polyester chips after low-temperature vacuum drying, low melting point staple fibre can be obtained through melt spinning.Patent of invention " a kind of low melting point short fiber of parallel type compound " (application number: be that water-soluble polyester component and polytrimethylene terephthalate component are composited low melting point short fiber side by side 200810123792.6), this fiber has good percent thermal shrinkage stability.Research about low melting point core-sheath polyester fiber also has some to report.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 obtained by fused mass directly spinning, sandwich layer is the conventional PET polyester fondant obtained by conventional PET section spinning process.But utilize reworked material to prepare polyester staple fiber 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 now causes great pollution to environment, and due to the shortage of the current raw material of industry, has become needed for sustainable development society the recycling of polyester waste material.Staple fibre major part prepared by current polyester waste material is for low additional fields such as fillers.Study modified tune adhering process, solve the technical barrier that polyester waste material source is wide, complicated component, quality fluctuation are large, utilize polyester waste material to prepare and there are the key subjects that high value-added product becomes regeneration industry transition and upgrade.In addition, this technology substitutes the spinning of eutectic polyester slice with fused mass directly spinning, and preferably resolve the series of problems such as low-melting point polyester drying cost is large, poor stability, fiber spinnability difference, production cost declines to a great extent.
Summary of the invention
In order to solve the technical problem utilizing reworked material to prepare the existence of polyester sheath core type composite fibre, one object of the present invention is the preparation method providing a kind of core-skin type regenerative polyester staple fiber, the method increase 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 feature.Another object of the present invention is to provide the regenerative polyester staple fiber adopting above-mentioned method to prepare.
In order to realize first above-mentioned object, present invention employs following technical scheme:
A preparation method for core-skin type regenerative polyester staple fiber, this regenerative polyester staple fiber is made up 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 that reworked material passes through to degrade again low melting point recycled polyester prepared by modified poly, and the fusing point of low melting point recycled polyester is 70 ~ 160 DEG C, 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 is prepared by modified tune adhering process, and the fusing point of described high-melting-point recycled polyester is 250 ~ 270 DEG C, content of carboxyl end group≤20mmol/kg, and inherent viscosity is 0.7dl/g ~ 1.0 dl/g; Two kinds of polyester fondants, by entering composite spinneret pack, the melt sprayed from the spinnerets of composite component after respective measuring pump metering, through cooling, winding, boundling, drawing-off, sizing, cut-out and packing, can obtain 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 is obtained 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 base tin laurate of zinc acetate, potassium acetate, manganese acetate, magnesium acetate, lead acetate, cobalt chloride, butyl titanate, tetraisopropyl titanate and 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;
Following a kind of method preparation regeneration low-melting point polyester is selected according to b raw material:
One, Methanolysis method
1) mix after a, b and c being fed intake, the mass ratio that feeds intake of a and b is 1:4 ~ 14, and the mass ratio of a and c is 100:0.5 ~ 1; Degradation temperature is 170 ~ 250 DEG C, pressure is 1.5 ~ 4.0Mpa, reaction time is 2.5 ~ 5h, equal pressure reacts when getting back to atmospheric pressure and terminates, filtered by reactant, the liquid in rotation evaporation obtained, boils off methyl alcohol and ethylene glycol respectively, the solids obtained 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 is carried out under nitrogen pressurization, 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; F and g feeds intake as 200 ~ 600ppm of sour total amount, and described alcohol is the summation of ethylene glycol and e; The temperature of esterification is 180 ~ 250 DEG C, and pressure is 0.05MPa ~ 0.4MPa, reaction time 1.5 ~ 3h; Polycondensation reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h;
Two, Hydrolyze method
1) be hydrolyzed: mix after a, b and c being fed intake, the mass ratio that feeds intake of a and b is 1:1 ~ 5, and the mass ratio of a and c is 100:0.5 ~ 1; Reaction temperature is 190 ~ 280 DEG C, pressure is 3.0 ~ 6.0Mpa, reaction time is 2 ~ 5h, when reaction end equal pressure gets back to atmospheric pressure, reactant is filtered, the evaporation of gained liquid in rotation obtains ethylene glycol, then is dissolved in DMF by filtering solids thing and filters, and gained liquid recrystallization obtains terephthalic acid (TPA);
2) esterification of terephthalic acid (TPA) and ethylene glycol is carried out under nitrogen pressurization, 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; F and g feeds intake as 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 DEG C, and pressure is 0.05MPa ~ 0.4MPa, reaction time 1.5 ~ 3h; Polycondensation reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h;
Three, glycolysis method
1) mix after a, b and c being fed 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 DEG C, and pressure is 0 DEG C 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 terminates, reactant liquor Rapid Thermal is filtered, decompression distillation is carried out to filtrate and reclaims ethylene glycol, the liquid after decompression distillation is dissolved in hot alcohol, ester, chlorinated hydrocabon or ketone solvent, heat filtering goes out insoluble matter, and filtrate naturally cools and obtains ethylene glycol terephthalate and oligomer thereof;
2) polycondensation reaction of ethylene glycol terephthalate and oligomer thereof, the molar weight that feeds intake of d is quality/384 of the quality/960-a of a; The molar weight that feeds intake of e is quality/576 of the quality/1728-a of a; The molar ratio of alkyd is 1.4 ~ 1.6:1; F and g feeds intake as 200 ~ 600ppm of sour total amount, and reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h.
As further improvement, the Pillar recovery raw material of described recycled polyester based on polyester bottle slice is by modified tune adhering process preparation, concrete technology is as follows: regenerative raw materials-cleaning-proportioning-drum dried-multistage filtering-liquid-phase tackifying, wherein, drum dried temperature is 100 ~ 150 DEG C, and drying time is 7 ~ 10h.
As further improvement, the step of described liquid-phase tackifying is as follows:
1) melt that the temperature after screw rod melting is 0.5dl/g ~ 0.70dl/g 260 DEG C ~ 290 DEG C inherent viscosities is pumped to vacuum separation tower through melt Conveying, melt is 10pa ~ 400pa in vacuum, temperature is 270 DEG C ~ 300 DEG C, and after stopping 15min ~ 40min under condition, inherent viscosity can reach 0.55dl/g ~ 0.78dl/g;
2) after, melt enters the modified tune of secondary and glues device, the melt temperature that the modified tune of secondary glues in device is identical with vacuum separation tower with vacuum, under the effect of rotatable propeller, melt constantly advances, 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 technique of the present invention adopts the modified tune of a kind of waste plastics described in Chinese invention patent (application number: 201010574044.7, the applying date: 2010-12-01) to glue system.
As further improvement, described Pillar recovery raw material also comprises the Waste Polyester textiles mixed.
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 both adaptable temperature.As further improvement, described low-melting point polyester spinning pipeline holding temperature is 220 ~ 240 DEG C; The extruder temperature of recycled polyester 270 ~ 300 DEG C, recycled polyester spinning pipeline holding temperature is 270-290 DEG C, and spinning body temperature is 270 ~ 290 DEG C.
Compounding flux thread is in spinning shaft, and through quenching, melt viscosity increases gradually until solidified forming.If cool insufficient, go out because cortex fusing point is lower after spinneret orifice, as-spun fibre is molten state, can be adhered together.As further improvement, described cooling adopts ring blowing to carry out, and wind-warm syndrome is 15 ~ 32 DEG C, 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, drawing temperature 50 ~ 72 DEG C, and draft speed is 100 ~ 150m/min.
In order to realize second above-mentioned object, present invention also offers the regenerative polyester staple fiber that above-mentioned preparation method prepares.
Core-skin type regenerative polyester staple fiber steady quality prepared by the inventive method, best in quality, can be used for producing in the industries such as non-weaving cloth, flocking, composite.
Detailed description of the invention
embodiment 1
1, the preparation of low-melting point polyester is regenerated: 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 is by polymerization preparation regeneration low-melting point polyester after Methanolysis: degradation temperature is 190 DEG C, pressure is 2.5Mpa, reaction time is 3h, equal pressure reacts when getting back to atmospheric pressure and terminates, filtered by reactant, the liquid in rotation evaporation obtained, boils off methyl alcohol and ethylene glycol respectively, the solids obtained 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 300ppm that the catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) they are total amount sour in reaction system, then add the stabilizing agent trimethyl phosphate (TMP) that weight is 0.01% (relatively sour composition).Esterification is carried out under nitrogen pressurization, and temperature is 220 DEG C, and pressure is 0.15MPa, reaction time 2.2h; Polycondensation reaction temperature is 275 DEG C, and vacuum is 90Pa, reaction time 3.5h.The fusing point of the low-melting point polyester obtained is 110 DEG C, 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, drum dried temperature is 130 DEG C, and drying time is 8h.The step of liquid-phase tackifying is as follows: the melt that the temperature 1) after screw rod melting is 0.55dl/g 270 DEG C of inherent viscosities is pumped to vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 DEG C, and after stopping 30min under condition, inherent viscosity can reach 0.68dl/g; 2) after, melt enters the modified tune of secondary and glues device, the melt temperature that the modified tune of secondary glues in device is identical with vacuum separation tower with vacuum, under the effect of rotatable propeller, melt constantly advances, 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 DEG C, 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 sprayed from the spinnerets of composite component, through cooling, winding, boundling, drawing-off, sizing, cut-out and packing, core-skin type regenerative polyester staple fiber can be obtained.The baking temperature of recycled polyester is 150 DEG C, and drying time is 7h, extruder temperature 280 DEG C; Low-melting point polyester spinning pipeline holding temperature is 230 DEG C, and recycled polyester spinning pipeline holding temperature is 275 DEG C, and spinning body temperature is 280 DEG C; Ring quenching wind-warm syndrome is 15 DEG C, and wind speed is 2.0m/s; Spinning speed is 1100m/min; Draw ratio is 2.0, drawing temperature 60 DEG C, and draft speed is 110m/min.The core-skin type regenerative polyester staple fiber quality index obtained 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 low-melting point polyester is regenerated: 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 is by polymerization preparation regeneration low-melting point polyester after hydrolysis: hydrolysis temperature is 220 DEG C, pressure is 4.5Mpa, reaction time is 2.8h, when reaction end equal pressure gets back to atmospheric pressure, reactant is filtered, the evaporation of gained liquid in rotation obtains ethylene glycol, then is dissolved in DMF by filtering solids thing and filters, and gained liquid recrystallization 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 300ppm that the catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) they are total amount sour in reaction system, then add the stabilizing agent trimethyl phosphate (TMP) that weight is 0.01% (relatively sour composition).Esterification is carried out under nitrogen pressurization, and temperature is 220 DEG C, and pressure is 0.3MPa, reaction time 2.5h; Polycondensation reaction temperature is 275 DEG C, and vacuum is 80Pa, reaction time 3h, and the fusing point of the low-melting point polyester obtained is 105 DEG C, 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, drum dried temperature is 110 DEG C, and drying time is 7h.The step of liquid-phase tackifying is as follows: the melt that the temperature 1) after screw rod melting is 0.55dl/g 270 DEG C of inherent viscosities is pumped to vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 DEG C, and after stopping 30min under condition, inherent viscosity can reach 0.68dl/g; 2) after, melt enters the modified tune of secondary and glues device, the melt temperature that the modified tune of secondary glues in device is identical with vacuum separation tower with vacuum, under the effect of rotatable propeller, melt constantly advances, 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 DEG C, 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 sprayed from the spinnerets of composite component, through cooling, winding, boundling, drawing-off, sizing, cut-out and packing, core-skin type regenerative polyester staple fiber can be obtained.The baking temperature of recycled polyester raw material is 140 DEG C, and drying time is 7.5h, extruder temperature 270 DEG C; Low-melting point polyester spinning pipeline holding temperature is 220 DEG C, and recycled polyester spinning pipeline holding temperature is 275 DEG C, and spinning body temperature is 280 DEG C; Ring quenching wind-warm syndrome is 20 DEG C, and wind speed is 3.0m/s; Spinning speed is 1000m/min; Draw ratio is 3.0, drawing temperature 56 DEG C, and draft speed is 120m/min.The core-skin type regenerative polyester staple fiber quality index obtained 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 low-melting point polyester is regenerated: 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 base tin laurate is 100:0.5; Alcoholysis reaction temperature is 196 DEG C, and pressure is 0.15MPa, and the reaction time is 2h, and the inherent viscosity of reactant liquor reaches 0.29dl/g.After reaction terminates, reactant liquor Rapid Thermal is filtered, decompression distillation is carried out to filtrate and reclaims ethylene glycol, liquid (being solid under normal temperature) after decompression distillation is dissolved in hot alcohol, ester, chlorinated hydrocabon, ketone equal solvent, heat filtering goes out insoluble matter, and filtrate naturally cools and obtains ethylene glycol terephthalate (BHET) and oligomer thereof.M-phthalic acid (IPA), neopentyl glycol (NPG), the catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) and stabilizing agent trimethyl phosphate (TMP) is added 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 DEG C, vacuum is 95Pa, reaction time 3.5h.The fusing point of the low-melting point polyester obtained is 115 DEG C, 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 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 400ppm that the catalytic antimony trioxide (Sb203) and cobalt acetate (Co (Ac) 2) they are total amount sour in reaction system, then add the stabilizing agent trimethyl phosphate (TMP) that weight is 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, drum dried temperature is 100 DEG C, and drying time is 7h.The step of liquid-phase tackifying is as follows: the melt that the temperature 1) after screw rod melting is 0.55dl/g 270 DEG C of inherent viscosities is pumped to vacuum separation tower through melt Conveying, melt is 100pa in vacuum, temperature is 280 DEG C, and after stopping 30min under condition, inherent viscosity can reach 0.68dl/g; 2) after, melt enters the modified tune of secondary and glues device, the melt temperature that the modified tune of secondary glues in device is identical with vacuum separation tower with vacuum, under the effect of rotatable propeller, melt constantly advances, 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 DEG C, 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 sprayed from the spinnerets of composite component, through cooling, winding, boundling, drawing-off, sizing, cut-out and packing, core-skin type regenerative polyester staple fiber can be obtained.The baking temperature of recycled polyester raw material is 140 DEG C, and drying time is 7h, extruder temperature 280 DEG C; Low-melting point polyester spinning pipeline holding temperature is 230 DEG C, and recycled polyester spinning pipeline holding temperature is 270 DEG C, and spinning body temperature is 285 DEG C; Ring quenching wind-warm syndrome is 22 DEG C, and wind speed is 2.5m/s; Spinning speed is 900m/min; Draw ratio is 2.5, drawing temperature 58 DEG C, and draft speed is 110m/min.The core-skin type regenerative polyester staple fiber quality index obtained 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 (8)
1. a preparation method for core-skin type regenerative polyester staple fiber, this regenerative polyester staple fiber is made up 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 that reworked material passes through to degrade again low melting point recycled polyester prepared by modified poly, and the fusing point of low melting point recycled polyester is 70 ~ 160 DEG C, content of carboxyl end group≤35mmol/kg, and inherent viscosity is 0.5dL/g ~ 1.0dL/g; Sandwich layer is the high-melting-point recycled polyester that reworked material is prepared by modified tune adhering process, and the fusing point of described high-melting-point recycled polyester is 250 ~ 270 DEG C, content of carboxyl end group≤20mmol/kg, and inherent viscosity is 0.7dl/g ~ 1.0dl/g; Two kinds of polyester fondants, by entering composite spinneret pack, the melt sprayed from the spinnerets of composite component after respective measuring pump metering, through cooling, winding, boundling, drawing-off, sizing, cut-out and packing, can obtain sheath-core type low-melting point regenerative polyester staple fiber;
Described low melting point recycled polyester is for following raw material is by degraded and polycondensation reaction and obtaining:
A. regenerative raw materials;
B. methyl alcohol, water or ethylene glycol;
C. one or more in base tin laurate of zinc acetate, potassium acetate, manganese acetate, magnesium acetate, lead acetate, cobalt chloride, butyl titanate, tetraisopropyl titanate and 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;
Following a kind of method preparation regeneration low-melting point polyester is selected according to b raw material:
One, Methanolysis method
1) mix after a, b and c being fed intake, the mass ratio that feeds intake of a and b is 1:4 ~ 14, and the mass ratio of a and c is 100:0.5 ~ 1; Degradation temperature is 170 ~ 250 DEG C, pressure is 1.5 ~ 4.0Mpa, reaction time is 2.5 ~ 5h, equal pressure reacts when getting back to atmospheric pressure and terminates, filtered by reactant, the liquid in rotation evaporation obtained, boils off methyl alcohol and ethylene glycol respectively, the solids obtained 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 is carried out under nitrogen pressurization, 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; F and g feeds intake as 200 ~ 600ppm of sour total amount, and described alcohol is the summation of ethylene glycol and e; The temperature of esterification is 180 ~ 250 DEG C, and pressure is 0.05MPa ~ 0.4MPa, reaction time 1.5 ~ 3h; Polycondensation reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h;
Two, Hydrolyze method
1) be hydrolyzed: mix after a, b and c being fed intake, the mass ratio that feeds intake of a and b is 1:1 ~ 5, and the mass ratio of a and c is 100:0.5 ~ 1; Reaction temperature is 190 ~ 280 DEG C, pressure is 3.0 ~ 6.0Mpa, reaction time is 2 ~ 5h, when reaction end equal pressure gets back to atmospheric pressure, reactant is filtered, the evaporation of gained liquid in rotation obtains ethylene glycol, then is dissolved in DMF by filtering solids thing and filters, and gained liquid recrystallization obtains terephthalic acid (TPA);
2) esterification of terephthalic acid (TPA) and ethylene glycol is carried out under nitrogen pressurization, 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; F and g feeds intake as 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 DEG C, and pressure is 0.05MPa ~ 0.4MPa, reaction time 1.5 ~ 3h; Polycondensation reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h;
Three, glycolysis method
1) mix after a, b and c being fed 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 DEG C, and pressure is 0 DEG C 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 terminates, reactant liquor Rapid Thermal is filtered, decompression distillation is carried out to filtrate and reclaims ethylene glycol, the liquid after decompression distillation is dissolved in hot alcohol, ester, chlorinated hydrocabon or ketone solvent, heat filtering goes out insoluble matter, and filtrate naturally cools and obtains ethylene glycol terephthalate and oligomer thereof;
2) polycondensation reaction of ethylene glycol terephthalate and oligomer thereof, the molar weight that feeds intake of d is quality/384 of the quality/960 ~ a of a; The molar weight that feeds intake of e is quality/576 of the quality/1728 ~ a of a; The molar ratio of alkyd is 1.4 ~ 1.6:1; F and g feeds intake as 200 ~ 600ppm of sour total amount, and reaction temperature is 250 ~ 285 DEG C, and vacuum is 30 ~ 200Pa, reaction time 2.5 ~ 5h.
2. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, is characterized in that the inherent viscosity of 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.
3. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, it is characterized in that: the Pillar recovery raw material of recycled polyester based on polyester bottle slice is by modified tune adhering process preparation, concrete technology is as follows: regenerative raw materials-cleaning-proportioning-drum dried-multistage filtering-liquid-phase tackifying, wherein, drum dried temperature is 100 ~ 150 DEG C, and drying time is 7 ~ 10h.
4. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 3, is characterized in that the step of liquid-phase tackifying is as follows:
1) melt that the temperature after screw rod melting is 0.5dl/g ~ 0.70dl/g 260 DEG C ~ 290 DEG C inherent viscosities is pumped to vacuum separation tower through melt Conveying, melt is 10pa ~ 400pa in vacuum, temperature is 270 DEG C ~ 300 DEG C, and after stopping 15min ~ 40min under condition, inherent viscosity can reach 0.55dl/g ~ 0.78dl/g;
2) after, melt enters the modified tune of secondary and glues device, the melt temperature that the modified tune of secondary glues in device is identical with vacuum separation tower with vacuum, under the effect of rotatable propeller, melt constantly advances, 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.
5. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, is characterized in that: low-melting point polyester spinning pipeline holding temperature is 220 ~ 240 DEG C; The extruder temperature of recycled polyester 270 ~ 300 DEG C, recycled polyester spinning pipeline holding temperature is 270 ~ 290 DEG C, and spinning body temperature is 270 ~ 290 DEG C.
6. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, is characterized in that: cooling adopts ring blowing to carry out, and wind-warm syndrome is 15 ~ 32 DEG C, and wind speed is 0.5 ~ 5.0m/s, and spinning speed is 800 ~ 1200m/min.
7. the preparation method of a kind of core-skin type regenerative polyester staple fiber according to claim 1, is characterized in that: the draw ratio of drawing-off is 1.2 ~ 3.5, drawing temperature 50 ~ 72 DEG C, and draft speed is 100 ~ 150m/min.
8. the regenerative polyester staple fiber that the preparation method according to claim 1 ~ 7 any one claim prepares.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310091697.3A CN103147163B (en) | 2013-03-21 | 2013-03-21 | Skin-core type recycled polyester staple fiber and preparation method thereof |
| PCT/CN2014/073754 WO2014146591A1 (en) | 2013-03-21 | 2014-03-20 | Skin-core type recycled polyester staple fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310091697.3A CN103147163B (en) | 2013-03-21 | 2013-03-21 | Skin-core type recycled polyester staple fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103147163A CN103147163A (en) | 2013-06-12 |
| CN103147163B true CN103147163B (en) | 2015-03-18 |
Family
ID=48545465
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310091697.3A Active CN103147163B (en) | 2013-03-21 | 2013-03-21 | Skin-core type recycled polyester staple fiber and preparation method thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN103147163B (en) |
| WO (1) | WO2014146591A1 (en) |
Families Citing this family (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147163B (en) * | 2013-03-21 | 2015-03-18 | 宁波大发化纤有限公司 | Skin-core type recycled polyester staple fiber and preparation method thereof |
| CN103145957B (en) * | 2013-03-21 | 2015-08-26 | 宁波大发化纤有限公司 | Degradation of ethylene glycol produces the method for core-skin type polyester low melting point recycled polyester |
| CN105803573A (en) * | 2014-12-30 | 2016-07-27 | 上海水星家用纺织品股份有限公司 | Preparation method of natural mint fibers |
| CN104862825B (en) * | 2015-06-10 | 2017-10-27 | 马海燕 | Major diameter core-skin type composite monofilament and its production method |
| EP3429451B1 (en) | 2016-03-17 | 2020-02-26 | Eurofilters N.V. | Vacuum-cleaner filter bag made from recycled plastic |
| EP3219375B1 (en) | 2016-03-17 | 2018-09-26 | Eurofilters N.V. | Vacuum cleaner filter bag containing dust and/or fibrous recycled material |
| CN106149075A (en) * | 2016-08-25 | 2016-11-23 | 宁波大发化纤有限公司 | A kind of dual-component parallel composite fiber prepared with Pillar recovery raw material |
| CN106319656A (en) * | 2016-08-25 | 2017-01-11 | 宁波大发化纤有限公司 | Preparation method for two-component side-by-side composite fibres |
| CN106435824A (en) * | 2016-10-11 | 2017-02-22 | 漳州市鼎鑫电子科技有限公司 | Self-fragrant natural anti-bacterial deodorizing fiber |
| CN106637498A (en) * | 2016-10-11 | 2017-05-10 | 漳州市鼎鑫电子科技有限公司 | Preparation method of self-fragrance natural antibacterial and deodorizing fiber and application thereof |
| CN110616474B (en) * | 2019-10-22 | 2021-02-12 | 宁波大发化纤有限公司 | Method for preparing skin-core composite low-melting-point regenerated polyester fiber from waste polyester textile |
| CN110685037A (en) * | 2019-11-11 | 2020-01-14 | 南通新帝克单丝科技股份有限公司 | High-strength wear-resistant zipper monofilament and production method thereof |
| CN111676528B (en) * | 2020-05-29 | 2022-05-17 | 绍兴柯桥恒鸣化纤有限公司 | Preparation method of melt direct-spun polyester-nylon composite superfine fiber |
| CN111705370B (en) * | 2020-05-29 | 2021-07-20 | 绍兴柯桥恒鸣化纤有限公司 | Method for preparing potential two-component elastic fiber based on melt direct spinning technology |
| CN112251828A (en) * | 2020-10-13 | 2021-01-22 | 江苏华亚化纤有限公司 | Preparation process of LMPET/PET sheath-core composite elastic fiber |
| CN112760748A (en) * | 2020-12-14 | 2021-05-07 | 浙江理工大学 | Method for preparing self-adhesive antibacterial skin-core fiber by regenerating waste polyester |
| CN112813528A (en) * | 2020-12-30 | 2021-05-18 | 浪莎针织有限公司 | Degradable flame-retardant polylactic acid elastic fiber and preparation method thereof |
| CN113445171A (en) * | 2021-07-30 | 2021-09-28 | 苏州贤辉新纺织科技有限公司 | Finishing method for 5tex fiber drafting process by utilizing recycled polyester fibers |
| CN114108125A (en) * | 2021-09-22 | 2022-03-01 | 安徽农业大学 | Preparation process of micro-cavity hollow uvioresistant regenerated PET (polyethylene terephthalate) fiber filament |
| CN114506054A (en) * | 2022-02-21 | 2022-05-17 | 富海(山东)包装材料有限公司 | Process technology for producing colored and permanent anti-sticking sheet by continuous polyester polymerization |
| CN115382297B (en) * | 2022-04-12 | 2023-10-31 | 江阴市华思诚无纺布有限公司 | Melt direct spinning bi-component PET (polyethylene terephthalate) spinning liquid filtering material and preparation method thereof |
| CN114805777A (en) * | 2022-04-14 | 2022-07-29 | 福建赛隆科技有限公司 | Regenerated PTT polymer and preparation method and application thereof |
| CN115142162A (en) * | 2022-07-05 | 2022-10-04 | 诸暨鼎丰化纤有限公司 | Regenerated polyester composite antibacterial polyester filament yarn and production process thereof |
| CN115074858A (en) * | 2022-08-04 | 2022-09-20 | 扬州天富龙集团股份有限公司 | Antibacterial low-melting-point polyester staple fiber and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445972A (en) * | 2008-12-29 | 2009-06-03 | 浙江理工大学 | Method for producing sheath-core type low-melting point polyester staple fiber |
| CN102093590A (en) * | 2010-12-01 | 2011-06-15 | 宁波大发化纤有限公司 | Waste plastic conditioning and viscosity modifying system |
| CN102899729A (en) * | 2012-10-19 | 2013-01-30 | 宁波大发化纤有限公司 | Method for processing regenerated polyester staple fiber by using waste polyester textile |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004211223A (en) * | 2002-12-27 | 2004-07-29 | Ashimori Ind Co Ltd | Rope |
| KR101183146B1 (en) * | 2010-05-14 | 2012-09-14 | 코오롱글로텍주식회사 | non-woven fabric with high elasticity and recoverability, and material for cushion utilizing the same |
| CN203212688U (en) * | 2013-03-07 | 2013-09-25 | 宁波大发化纤有限公司 | Fully recycled sheath-core low-melting point polyester staple fiber |
| CN103145958B (en) * | 2013-03-21 | 2015-08-26 | 宁波大发化纤有限公司 | Methanol degradation produces the method for core-skin type polyester low melting point recycled polyester |
| CN103147163B (en) * | 2013-03-21 | 2015-03-18 | 宁波大发化纤有限公司 | Skin-core type recycled polyester staple fiber and preparation method thereof |
| CN103145957B (en) * | 2013-03-21 | 2015-08-26 | 宁波大发化纤有限公司 | Degradation of ethylene glycol produces the method for core-skin type polyester low melting point recycled polyester |
| CN103145959B (en) * | 2013-03-21 | 2015-08-26 | 宁波大发化纤有限公司 | Hydrolytic deterioration produces the method for core-skin type polyester low melting point recycled polyester |
-
2013
- 2013-03-21 CN CN201310091697.3A patent/CN103147163B/en active Active
-
2014
- 2014-03-20 WO PCT/CN2014/073754 patent/WO2014146591A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445972A (en) * | 2008-12-29 | 2009-06-03 | 浙江理工大学 | Method for producing sheath-core type low-melting point polyester staple fiber |
| CN102093590A (en) * | 2010-12-01 | 2011-06-15 | 宁波大发化纤有限公司 | Waste plastic conditioning and viscosity modifying system |
| CN102899729A (en) * | 2012-10-19 | 2013-01-30 | 宁波大发化纤有限公司 | Method for processing regenerated polyester staple fiber by using waste polyester textile |
Non-Patent Citations (1)
| Title |
|---|
| 从废聚酯合成多组分共聚酯的研究;祝根平;《浙江大学硕士学位论文》;20040101;第17，18，22-26，52-54页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103147163A (en) | 2013-06-12 |
| WO2014146591A1 (en) | 2014-09-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103147163B (en) | Skin-core type recycled polyester staple fiber and preparation method thereof | |
| CN103145957B (en) | Degradation of ethylene glycol produces the method for core-skin type polyester low melting point recycled polyester | |
| CN103147162B (en) | Sandwich layer adopts core-skin type polyester staple fiber of recycled polyester and preparation method thereof | |
| CN103145958B (en) | Methanol degradation produces the method for core-skin type polyester low melting point recycled polyester | |
| CN101445972B (en) | Method for producing sheath-core type low-melting point polyester staple fiber | |
| CN103145959B (en) | Hydrolytic deterioration produces the method for core-skin type polyester low melting point recycled polyester | |
| CN103146020A (en) | High-melting-point renewable polyester for core layers of sheath-core polyester staple fibers and preparation method and application thereof | |
| CN106400140A (en) | Processing technology of low-melting-point sheath-core composite filament | |
| CN107502976B (en) | Crystalline PET, delustering PTT and composite elastic fiber prepared from crystalline PET and delustering PTT | |
| WO2023115980A1 (en) | Composite material, preparation method therefor and use thereof | |
| CN108479426A (en) | A kind of preparation method and product of High-strength hollow fiber film | |
| CN113005563A (en) | Preparation method of low-melting-point PTT sheath-core composite copolyester fiber | |
| CN107118521A (en) | A kind of poly- furandicarboxylic acid glycol ester resin combination and its preparation method and application | |
| CN104695047A (en) | Novel high-softness polylactic acid fiber composite material and preparation method thereof | |
| CN115896976A (en) | Regenerated low-melting-point polyester composite fiber with flame retardant function and preparation method thereof | |
| CN1896346A (en) | Preparation of multi-stage shrinkage polyester fibre by one-step method | |
| JP2010065348A (en) | Method for producing polyester conjugated fiber | |
| CN103541040B (en) | The preparation method of PLA superfine fibre and PLA superfine fibre | |
| KR102115821B1 (en) | Low melting polyester resin and polyester composite fiber with excellent thermal fusing property using the same | |
| CN109722741B (en) | Sheath-core flame-retardant filament and preparation method thereof | |
| JPH0347325B2 (en) | ||
| CN115726057A (en) | Regenerated low-melting-point polyester composite fiber with ultraviolet shielding function and preparation method thereof | |
| TWI803790B (en) | Sheath-core type heat-bonding fiber and non-woven fabric | |
| JP2011012154A (en) | Polyester resin and binder fiber | |
| KR100323611B1 (en) | Manufacturing method of high shrinkage polyester bland |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201118 Address after: No.8 Xingyao Road, Binhai New Town, Yuyao Economic Development Zone, Ningbo City, Zhejiang Province Patentee after: Yuyao Dafa Chemical Fiber Co.,Ltd. Address before: 315336 No. two, No. 266 Binhai Road, Hangzhou Bay Development Zone, Zhejiang, Ningbo Patentee before: NINGBO DAFA CHEMICAL FIBER Co.,Ltd. |