CN114592248A - Preparation method of PET and PBT composite elastic fiber - Google Patents

Preparation method of PET and PBT composite elastic fiber Download PDF

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Publication number
CN114592248A
CN114592248A CN202210222939.7A CN202210222939A CN114592248A CN 114592248 A CN114592248 A CN 114592248A CN 202210222939 A CN202210222939 A CN 202210222939A CN 114592248 A CN114592248 A CN 114592248A
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pbt
pet
melting
slices
elastic fiber
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李达
张正松
吕继红
沈安昌
李宏
陈和松
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ZHOUSHAN XINXIN CHEMICAL FIBER CO Ltd
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ZHOUSHAN XINXIN CHEMICAL FIBER CO Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/32Side-by-side structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00Complete machines for producing artificial threads
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, 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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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Multicomponent Fibers (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Abstract

A preparation method of PET and PBT composite elastic fiber comprises the following steps of preparing PET slices and PBT slices; the slices are respectively put into a parallel composite spinning device and respectively melted and flowed to a spinning mechanism through respective melt pipelines; co-extruding from a spinneret orifice; drafting, cross-blowing, heat setting and winding the mixed yarn; adding 1-10% by mass of PBT functional master batch into a melt pipeline of the PBT slice through an injector; PET adheres to PBT and is co-extruded during extrusion. The invention has the advantages that: the invention can realize the tight connection of the internal structure of the composite fiber, thereby enhancing the elasticity and the toughness of the elastic fiber, and effectively reducing the phenomenon that the elastic and unwinding phenomena are influenced by a large amount of stumbled wires and cobweb wires in the preparation process, and the elastic fiber has stable elastic performance and small tension fluctuation.

Description

Preparation method of PET and PBT composite elastic fiber
Technical Field
The invention relates to the technical field of elastic fiber manufacturing, in particular to a preparation method of PET and PBT composite elastic fiber.
Background
Polybutylene terephthalate (PBT) has a softer molecular chain than its homologues, polyethylene terephthalate (PET) and trimethylene terephthalate (PTT), and has PTT-like elasticity. Because PET and PBT have different heat resistance, when the PET and the PBT meet high temperature, the thermal shrinkage rates of the PET and the PBT are different, and according to the difference, people usually obtain the parallel bi-component self-crimping elastic filament after the PBT melt and the PET melt reach a spinneret plate through respective melt pipelines and are extruded from spinneret holes of the spinneret plate by a parallel composite spinning technology. The PBT/PET composite elastic filament has the PET component outside the coiled spiral and the PBT component inside the coiled spiral, and has permanent elasticity due to the fact that the coiled spiral stretches when being stretched by external force.
The prior Chinese patent application with the application number of CN201711485504.7, namely 'a production process of PBT/PET double-component elastic composite fiber' discloses that a differential PBT component and PET component raw materials are extruded and compounded into a single filament bundle at a spinneret micropore by two groups of metering pumps and two groups of spinning components, a PBT melt and a PET melt are stretched, cooled, solidified and wound to form double-component POY (polyester pre-oriented yarn), and then the double-component elastic composite fiber product is prepared by stretching, false twisting and deforming.
In addition, the Chinese patent application with the application number of CN201910444144.9, namely 'a production method of high-elasticity fibers', defines the preparation and production technology of the PBT/PET parallel composite elastic filament, and comprises the technological processes of the viscosity of PET being 0.45-0.55 dl/g, the viscosity of PBT being 1.25-1.4 dl/g, the ratio of PET to PBT being 1: 1-1: 1.1, and the processes of cross air blowing, oiling, pre-networking, drafting and shaping, main networking, winding and shaping, inspection, grading packaging and the like which are needed after spinning.
Therefore, in the prior art, functional modification of the polyester fiber is mainly realized through physical modification and chemical modification, wherein the physical modification is various special-shaped sections, surface etching and compounding with other fibers, and the chemical modification is mainly to add various functional substances, such as flame retardants, antistatic agents, antibacterial agents and the like, or add functional active monomers for copolymerization in the spinning process so as to improve the performance of the polyester fiber. Functional modification of PBT and PET composite fibers mainly focuses on adding functional monomers in a blending manner or adding functional monomers in a parallel composite spinning PET component, but a technical scheme for improving the functionality of PBT/PET parallel composite elastic fibers by adding functional monomers in a PBT part of an elastic component does not exist, so that the preparation method of elastic fibers in the prior art needs further improvement.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of PET and PBT composite elastic fiber which can effectively reduce the phenomenon that the phenomenon of elasticity increasing and unwinding is influenced by a large amount of stumbling threads and cobweb threads in the preparation process, has stable elastic performance and small tension fluctuation.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the PET and PBT composite elastic fiber comprises the following steps,
firstly, respectively manufacturing a PET slice and a PBT slice;
secondly, respectively placing the prepared PET slices and PBT slices into a parallel composite spinning device, and respectively melting the PET slices and the PBT slices through respective melt pipelines and flowing to a spinning mechanism of the parallel composite spinning device along the respective melt pipelines;
thirdly, extruding the molten PET slices and the molten PBT slices out of a spinneret hole of a spinneret mechanism together;
fourthly, drawing, cross-blowing, heat setting and winding the extruded mixed yarn;
the method is characterized in that: in the first step, the PBT slice is a PBT slice with the viscosity of 0.9-1.25dl/g formed by liquid-phase tackifying of a polycondensation kettle in the polymerization process or solid-phase tackifying after polymerization;
in the second step, 1-10% by mass of PBT functional master batch is added into a melt pipeline of the PBT slice through an injector;
in the third step, the molten PET slices and the molten PBT slices are extruded together from two spinneret orifices with the aperture ratio of 3.5: 6.5-6.5: 3.5, the PET is adhered to the PBT to be extruded together in the extrusion process, and the PET and PBT composite elastic fiber which can be dyed at the temperature of 90 ℃ under normal pressure, has the dye uptake of 86.2-92.8%, the K/S value of 20.42-23.74 and the curling elastic elongation of more than 30% is obtained through the fourth step after extrusion.
As an improvement, the PBT functional master batch is formed by melting, mixing, stretching and slicing the PBT resin and a functional material, wherein the functional material is one or a mixture of zinc oxide, a silver-series antibacterial agent, a titanium dioxide anti-penetrating agent, an antistatic agent, a flame retardant, far infrared powder, an oxygen anion material, magnetic therapy powder and the like.
The PBT master batch is further improved, and the weight percentage of the functional material in the PBT functional master batch is 80-95%.
The PBT slice is further improved, the glass transition temperature of the PBT slice is 22-43 ℃, the melting point of the PBT slice is 220-230 ℃, and the viscosity of the PBT slice is 1.02-1.25 dl/g.
As an improvement, the step two of melting respectively means that the PET slices are melted in a melt pipeline with one side having a melting temperature of 260-280 ℃ and sheared by a screw; and melting the PBT slices and the PBT master batches in a melt pipeline with the melting temperature of 250-270 ℃ at the other side and cut by a screw.
As an improvement, in the third step, the extrusion temperature is 260-270 ℃.
As an improvement, the drawing refers to drawing the filament bundle to be thin by the extruded mixed filament so as to gradually straighten the fiber macromolecules therein, wherein the drawing multiple is 2-6 times; the lateral blowing is cooling and solidifying mixed yarn in a drafting channel, the wind pressure is 50-300 Pa, the wind temperature is 10-50 ℃, the wind speed is 50-80%, and the wind speed is 0.4-0.7 m/s; the heat setting means that the drawn mixed filament is kept at the temperature in a heat setting device for a period of time, so that the fiber structure of the drawn mixed filament is stable, the temperature is 80-150 ℃, and the heat treatment time is 5-30 min.
As an improvement, the parallel composite spinning device comprises a bracket, a first blanking part, a second blanking part, a pre-crystallization part, a first drying part, a second drying part, a first melting part, a second melting part, a spinning mechanism, a spinning beam-collecting part, a side blowing part, a first winding part, a heat setting part and a second winding part;
the spinning mechanism comprises a support, a first blanking portion, a second blanking portion, a discharging pipe, a pre-crystallizing portion, a discharging pipe, a first melting portion, a second melting portion, a spinning mechanism and a second winding portion, wherein the first blanking portion and the second blanking portion are connected to the support respectively, the discharging pipe of the first blanking portion is connected with the pre-crystallizing portion, the discharging pipe of the pre-crystallizing portion is connected with the first drying portion, the discharging pipe of the second blanking portion is connected with the second drying portion, the discharging pipe of the first drying portion is connected with the first melting portion, the discharging pipe of the second drying portion is connected with the second melting portion, the discharging ports of the first melting portion and the second melting portion are communicated with a feeding port of the spinning mechanism respectively, the discharging port of the spinning mechanism is located above the spinning winding portion, a bottom opening of the spinning winding portion is located above the side blowing portion, the first winding portion is located below the side blowing portion, the heat setting portion is located on one side of the first winding portion, and the second winding portion is connected to the heat setting portion.
The spinning mechanism comprises a positioning shell for mounting a spinning sheet, and a feeding body, a connecting body, a first stirring sheet, a second stirring sheet, a third stirring sheet, a fourth stirring sheet and a fifth stirring sheet which are arranged in the positioning shell in sequence, wherein the top of the feeding body extends out of an opening in the top of the positioning shell.
The heat setting part comprises a positioning frame, a first stretching roller, a heat setting box, a false twisting part, a second setting part, a second stretching roller, an upper oil groove and a third stretching roller;
first drawing roller can connect on the locating rack with rotating, is provided with the guide bar on the locating rack of first stay cord roller top, the guide bar is corresponding with the incoming line mouth of thermal setting case, the export of thermal setting case is provided with the wire conduit, the export of wire conduit is corresponding with the false twist rod of false twist portion be provided with the guide pulley on the locating rack in the export outside of false twist portion, second winding portion sets up on the locating rack of false twist portion below, second winding portion sets up on the locating rack at second winding portion rear, and the second drawing roller is located second winding portion below, it is located the below of second drawing roller to go up the oil groove, third stay cord roller is corresponding with the second drawing roller, the place ahead at second winding portion is connected to the third drawing roller.
Compared with the prior art, the invention has the advantages that: the invention can realize the tight connection of the internal structure of the composite fiber yarn, thereby enhancing the elasticity and the toughness of the elastic fiber, and compared with the fiber produced by the prior art, the tensile allowance of the elastic fiber is more than 150 percent. In addition, the functional composite elastic fiber is realized by adding a proper amount of functional substances on different components through a parallel composite spinning technology. Wherein the PET component adopts a third monomer and a fourth monomer which are added with long chain fatty acid or alcohol, polyether polyol and the like to obtain a modified low-viscosity PET slice with the viscosity of 0.46-0.56dl/g, and can be dyed at low temperature and normal pressure; the PBT component is a functional master batch prepared by increasing the viscosity to 0.9-1.25dl/g by a liquid phase or solid phase tackifying technology and adding functional substances. The modified PET component and the PBT functional component are respectively placed into respective melt pipelines of parallel composite spinning equipment, functional master batches are injected into the PBT pipelines through injectors, respectively melted and flow into spinneret orifices of a spinneret mechanism along the respective melt pipelines, the functional master batches are jointly extruded at certain extrusion temperature and with the spinneret orifices in aperture proportion, and further the functional master batches are subjected to drawing, cross-blowing, heat setting and winding to form the environment-friendly PBT/PET composite elastic fiber with the functions of low-temperature dyeability, high elasticity, antibiosis, permeation prevention, static resistance and the like. Functional substances are added into the PBT elastic component with smaller apparent viscosity, and the PET component is modified, so that the problems that elastic and unwinding are influenced and tension fluctuation and broken ends occur due to the fact that functional substances are added into the PET component or the two components respectively, and the bilateral phenomenon exists in common PET/PBT fiber dyeing are solved.
Drawings
FIG. 1 is a front perspective view of an embodiment of the present invention with the second winding portion and the heat-set portion removed;
FIG. 2 is a perspective view of FIG. 1 at another angle;
FIG. 3 is a perspective view of FIG. 2 at another angle;
FIG. 4 is a bottom view of the bottom opening of the oven of FIG. 3;
FIG. 5 is a perspective view of the spinning mechanism of FIG. 4;
FIG. 6 is a cross-sectional view of the vertical plane of FIG. 5 with the alignment shell removed and taken along the central axis;
FIG. 7 is an exploded view of the structure of FIG. 6;
FIG. 8 is a perspective view of FIG. 7 at another angle;
FIG. 9 is an exploded view of the configuration of FIG. 7 with five stirring blades remaining;
FIG. 10 is a perspective view of a second winding portion and a heat-set portion in an embodiment of the present invention;
FIG. 11 is a perspective view of FIG. 10 at another angle;
FIG. 12 is a perspective view of FIG. 11 at another angle;
FIG. 13 is a schematic diagram of the operation of the composite fiber heat setting of FIG. 10;
fig. 14 is a cross-sectional view of the composite filament of fig. 4 exiting the oven.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
(1) Terephthalic acid, isophthalic acid, adipic acid, ethylene glycol and 1, 4-butanediol are used as raw materials to carry out a first-step esterification reaction, the feeding time is 3.0h, the temperature is 255-258 ℃, and the esterification rate is 95-96%; and then adding polyethylene glycol and a composite stabilizer of triphenyl phosphate, organosilicon quaternary ammonium salt and sodium acetate, and carrying out a second-step polycondensation reaction, wherein the low-vacuum reaction time is 50min, the high-vacuum reaction time is 4.0h, the polycondensation temperature is 288-290 ℃, and the pressure is not higher than 70Pa, so as to obtain a modified low-viscosity polyester slice dyed at low temperature and normal pressure, wherein the viscosity is 0.48dl/g and is used as a component A.
(2) Adopting 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent to carry out esterification (the temperature is 240-242 ℃, the pressure is 40-45 KPa, the residence time is 2.5-3.0 h), pre-polycondensation (the temperature is 242-244 ℃, the pressure is 1.5-2.0 KPa, the residence time is 50-70 min), final polycondensation (the temperature is 245-250 ℃, the pressure is 0.1-0.15 KPa, the residence time is 2.5-3.0 h), granulating and other links, and obtaining 1.10dl/g PBT slices by a liquid phase tackifying technology; and (3) melting, blending, stretching and slicing the PBT slices and 90 wt% of the silver-series antibacterial agent to form the PBT antibacterial master batch. And mixing the PBT slices and the PBT antibacterial master batch to form a component B, wherein the antibacterial agent accounts for 5% of the component B by mass.
(3) Respectively putting the component A and the component B into respective melt pipelines of parallel composite spinning equipment, respectively melting (A. screw temperature 262, 266, 267, 268 ℃, B. screw temperature 258, 260 ℃) and flowing to parallel spinneret orifices along the respective melt pipelines, wherein the ratio of two hole diameters is 4 at the extrusion temperature of 265 ℃:6 extruding spinneret orifices together; and (3) cross air blowing: wind pressure is 200Pa, wind temperature is 40 ℃, rheumatism is 60%, and wind speed is 0.5 m/s; heat setting at 120 deg.c for 20 min; the draft was 5 times and the winding speed was 2500 m/min.
The PBT/PET composite elastic fiber with low-temperature dyeability, high elasticity, antistatic property and antibacterial function can be obtained, and can be dyed at normal pressure at 90 ℃, the dye-uptake rate is 90%, the K/S value is 24.32, the crimp elastic elongation is 35%, and the antibacterial rate (escherichia coli, staphylococcus aureus and candida albicans) is more than or equal to 99%.
Example 2
(1) Terephthalic acid, isophthalic acid, sebacic acid, ethylene glycol and 1, 3-propylene glycol are adopted as raw materials to carry out the first-step esterification reaction, the feeding time is 3.5h, the temperature is 256-258 ℃, and the esterification rate is 94-95%; and then adding polyoxypropylene glycol and a composite stabilizer of triphenyl phosphate, organosilicon quaternary ammonium salt and sodium acetate, carrying out a second-step polycondensation reaction, wherein the low-vacuum reaction time is 50min, the high-vacuum reaction time is 4.5h, the polycondensation temperature is 288-290 ℃, and the pressure is not higher than 70Pa, so as to obtain the modified low-viscosity polyester slice dyed at low temperature and normal pressure, wherein the viscosity is 0.50dl/g and is used as a component A.
(2) Adopting 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent to carry out esterification (the temperature is 240-242 ℃, the pressure is 40-45 KPa, the residence time is 2.5-3.0 h), pre-polycondensation (the temperature is 242-244 ℃, the pressure is 1.5-2.0 KPa, the residence time is 50-70 min), final polycondensation (the temperature is 245-250 ℃, the pressure is 0.1-0.15 KPa, the residence time is 2.5-3.0 h), granulating and other links, and obtaining PBT slices of 1.05dl/g by a liquid phase tackifying technology; and melting, blending, stretching and slicing the PBT slices and 90 wt% of 2000-mesh far-infrared ceramic powder to form the PBT far-infrared master batch. And mixing the PBT slices with the PBT far infrared master batch to form a component B, wherein the far infrared ceramic powder accounts for 10 mass percent of the component B.
(3) The component A and the component B are respectively put into respective melt pipelines of parallel composite spinning equipment, respectively melted (A. screw temperature 263, 265, 267, 268 ℃ and B. screw temperature 258, 262 ℃) and flowed to parallel spinneret orifices along the respective melt pipelines, and the ratio of two pore diameters is 5 at the extrusion temperature of 260 ℃: 5 extruding spinneret orifices together; cross air blowing: wind pressure is 200Pa, wind temperature is 40 ℃, rheumatism is 60%, and wind speed is 0.5 m/s; heat setting at 130 deg.C for 30 min; the draft was 4 times and the winding speed was 2600 m/min.
The obtained PBT/PET composite elastic fiber has low-temperature dyeability, high elasticity, antistatic property and far infrared health care function, can be dyed at normal pressure at 90 ℃, has the dye-uptake of 91 percent, the K/S value of 23.82 and the crimp elastic elongation of 33 percent, has the normal emissivity of 0.92 within the range of 8-14 microns, and has the temperature rise effect improved by 3 ℃ compared with the conventional PBT/PET composite elastic fiber.
Example 3
(1) Terephthalic acid, isophthalic acid, glutaric acid, ethylene glycol and 1, 6-hexanediol are used as raw materials to carry out the first-step esterification reaction, the feeding time is 4.0h, the temperature is 255-257 ℃, and the esterification rate is 93-94%; and then adding polytetrahydrofuran diol, flame-retardant polyether polyol and a composite stabilizer of triphenyl phosphate, organosilicon quaternary ammonium salt and sodium acetate, and carrying out a second-step polycondensation reaction, wherein the low-vacuum reaction time is 50min, the high-vacuum reaction time is 5.0h, the polycondensation temperature is 288-290 ℃, and the pressure is not higher than 70Pa, so that a modified low-viscosity polyester slice which is dyed at low temperature and normal pressure and has certain flame-retardant performance is obtained, and the viscosity is 0.52dl/g and is used as a component A.
(2) Adopting 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent to carry out esterification (the temperature is 240-242 ℃, the pressure is 40-45 KPa, the residence time is 2.5-3.0 h), pre-polycondensation (the temperature is 242-244 ℃, the pressure is 1.5-2.0 KPa, the residence time is 50-70 min), final polycondensation (the temperature is 245-250 ℃, the pressure is 0.1-0.15 KPa, the residence time is 3.0-3.5 h), granulating and other links, and obtaining 1.15dl/g PBT slices by a liquid phase tackifying technology; and (3) melting, blending, stretching and slicing the PBT slices and 90 wt% of tris (2-chloroethyl) phosphate (TCEP) flame retardant to form the PBT flame-retardant master batch. And mixing the PBT slices and the PBT flame-retardant master batch to form a component B, wherein the mass fraction of the tris (2-chloroethyl) phosphate in the component B is 10%.
(3) Respectively placing the component A and the component B into respective melt pipelines of parallel composite spinning equipment, respectively melting (A. screw temperature 263, 264, 266, 268 and 268 ℃, B. screw temperature 260, 262 and 262 ℃) and flowing to parallel spinneret orifices along the respective melt pipelines, wherein the ratio of the two pore diameters is 4 at an extrusion temperature of 270 ℃:6 extruding spinneret orifices together; and (3) cross air blowing: wind pressure is 200Pa, wind temperature is 40 ℃, rheumatism is 60%, and wind speed is 0.5 m/s; heat setting at 125 deg.c for 30 min; the draft was 4.5 times and the winding speed was 2700 m/min.
The obtained PBT/PET composite elastic fiber has the functions of low-temperature dyeability, high elasticity, antistatic property and flame retardance, can be dyed at normal pressure at 90 ℃, has the dye uptake of 89 percent, the K/S value of 23.20 and the crimp elastic elongation of 31 percent, and improves the limit oxygen index to 31.6.
As shown in fig. 1 to 14, the method for preparing the PET and PBT composite elastic fiber of the embodiment includes the following steps,
firstly, respectively manufacturing a PET slice and a PBT slice;
secondly, respectively placing the prepared PET slices and PBT slices into a parallel composite spinning device, and respectively melting the PET slices and the PBT slices through respective melt pipelines and flowing to a spinning mechanism of the parallel composite spinning device along the respective melt pipelines;
thirdly, extruding the molten PET slices and the molten PBT slices out of a spinneret hole of a spinneret mechanism together;
fourthly, drawing, cross-blowing, heat setting and winding the extruded mixed filament;
in the first step, the PBT slice is a PBT slice which is subjected to liquid phase tackifying in a polycondensation kettle in the polymerization process or solid phase tackifying after polymerization and has the viscosity of 0.9-1.25 dl/g;
in the second step, 1-10% by mass of PBT functional master batch is added into a melt pipeline of the PBT slice through an injector; the injector may comprise a storage bin and a screw feeder 33, and the specific structure of the injector is known in the art and will not be described in detail.
In the third step, the molten PET slices and the molten PBT slices are extruded together from two spinneret orifices with the aperture ratio of 3.5: 6.5-6.5: 3.5, the PET is adhered to the PBT to be extruded together in the extrusion process, and the PET and PBT composite elastic fiber which can be dyed at the temperature of 90 ℃ under normal pressure, has the dye uptake of 86.2-92.8%, the K/S value of 20.42-23.74 and the curling elastic elongation of more than 30% is obtained through the fourth step after extrusion.
The functional PBT master batch is prepared by melting, mixing, stretching and slicing the PBT resin and a functional material, wherein the functional material is one or a mixture of zinc oxide, a silver antibacterial agent, a titanium dioxide anti-penetration agent, an antistatic agent, a flame retardant, far infrared powder, a negative oxygen ion material, magnetic therapy powder and the like. The functional material in the PBT functional master batch is 80-95 wt%. The PBT slice has a glass transition temperature of 22-43 ℃, a melting point of 220-230 ℃ and a viscosity of 1.02-1.25 dl/g.
The step two of melting respectively means that the PET slices are melted in a melt pipeline with one side of melting temperature of 260-280 ℃ and cut by a screw; and melting the PBT slices and the PBT master batches in a melt pipeline with the melting temperature of 250-270 ℃ at the other side and cut by a screw. In the third step, the extrusion temperature is 260-270 ℃. Drawing means that the extruded mixed yarn draws the filament bundle to be thin, so that fiber macromolecules in the filament bundle are gradually straightened, and the drawing multiple is 2-6 times; the lateral blowing is cooling and solidifying mixed yarn in a drafting channel, the wind pressure is 50-300 Pa, the wind temperature is 10-50 ℃, the wind speed is 50-80%, and the wind speed is 0.4-0.7 m/s; the heat setting means that the drawn mixed filament is kept at the temperature in a heat setting device for a period of time, so that the fiber structure of the drawn mixed filament is stable, the temperature is 80-150 ℃, and the heat treatment time is 5-30 min.
PET chips were prepared by combining component a: para-aromatic dicarboxylic acid or an ester thereof, component B: aliphatic diols and component C: the meta-aromatic dicarboxylic acid or esters thereof are subjected to esterification reaction, and then the component D: aliphatic polyether polyol, a catalyst and a composite stabilizer are subjected to polycondensation reaction under the conditions of high temperature and high vacuum to obtain the catalyst. The PET slice has a glass transition temperature of 45-65 ℃, a melting point of 230-260 ℃ and a viscosity of 0.46-0.56 dl/g.
The parallel composite spinning device comprises a bracket 1, a first blanking part 21, a second blanking part 22, a pre-crystallization part 23, a first drying part 31, a second drying part 32, a first melting part 41, a second melting part 42, a spinning mechanism, a spinning beam-collecting part, a side blowing part, a first winding part, a heat setting part and a second winding part; the first blanking part 21 and the second blanking part 22 are respectively connected to the support 1, a discharge pipe of the first blanking part 21 is connected with the pre-crystallization part 23, a discharge pipe of the pre-crystallization part 23 is connected with the first drying part 31, a discharge pipe of the second blanking part 22 is connected with the second drying part 32, a discharge pipe of the first drying part 31 is connected with the first melting part 41, a discharge pipe of the second drying part 32 is connected with the second melting part 42, discharge ports of the first melting part 41 and the second melting part 42 are respectively communicated with a feed port of the spinning mechanism, a discharge port of the spinning mechanism is positioned above a spinning convergence part, a bottom opening of the spinning convergence part is positioned above the side blowing part, the first winding part is positioned below the side blowing part, the heat setting part is positioned on one side of the first winding part, and the second winding part is connected to the heat setting part. The pre-crystallization part 23 comprises a drying box and a heater which can circularly introduce hot gas into the drying box, an inlet at the top of the drying box is connected with a discharge pipe of the first blanking part 21 through a valve, the side part of the drying box is connected with an air outlet pipe of the heater, the side part at the other side of the drying box is connected with an air inlet pipe of the heater, and the bottom of the drying box is connected with the first drying part 31 through a pipeline.
The first drying part 31 is a first dryer which can suspend and dry the PBT crystals, the lower part of the first dryer is connected with a hot air duct, the bottom of the first dryer is connected with the first feeding hopper 411 of the first melting part 41 through a duct, the second drying part 42 is a second dryer which can suspend and dry the PET chips, the lower part of the second dryer is connected with a second hot air duct, and the bottom of the second dryer is connected with the second feeding hopper 421 of the second melting part 42 through a duct. The specific structure of the first dryer and the second dryer belongs to the prior art, and thus, will not be described in detail.
The first melting part 41 comprises a first feed hopper 411, a first screw cylinder combination and a first blanking pipe which can feed PBT melt from the first screw cylinder combination into the oven 9, wherein an outlet of the first feed hopper 411 is communicated with an inlet of the first screw cylinder combination, an outlet of the first screw cylinder combination is communicated with the first blanking pipe, and the first blanking pipe is communicated with a first inlet 911 of a spinning mechanism in the oven 9.
The second melting part 42 includes a second feeding hopper 421, a second screw barrel combination, and a second feeding pipe capable of feeding the PET melt from the second screw barrel combination into the oven 9, an outlet of the second feeding hopper 421 is communicated with an inlet of the second screw barrel combination, an outlet of the second screw barrel combination is communicated with the second feeding pipe, and the second feeding pipe is communicated with a second inlet 912 of the spinneret mechanism in the oven 9. The composite fibers exit the oven from the bottom opening 93 of the oven. The specific structure of the first screw barrel combination and the second screw barrel combination belongs to the prior art, and therefore, the detailed description is not provided. As shown in fig. 14, the composite filament PET portion 94 and PBT portion 95 exiting the oven are tightly connected together.
The spinning mechanism comprises a positioning shell 90, a feeding body 91, a connecting body 92, a first stirring sheet 901, a second stirring sheet 902, a third stirring sheet 903, a fourth stirring sheet 904 and a fifth stirring sheet 905 which are sequentially arranged in the positioning shell 90, wherein the top of the feeding body 91 extends out of the top opening of the positioning shell 90, and a first inlet 911 and a second inlet 912 are arranged at the top of the feeding body 91. The connector 92 is provided with two cavities, one cavity is communicated with the first inlet 911, and the other cavity is communicated with the second inlet 912. The two cavities of the connecting body 92 are internally provided with a plurality of layers of filter sheets, and the filter sheets are sequentially a first iron sheet filter sheet 921, a first gauze filter sheet 922, a carborundum filter layer 923, a second gauze filter sheet 924, a second iron sheet filter sheet 925, a third gauze filter sheet 926 and a fourth iron sheet filter sheet 927 from top to bottom.
The spinning and bundling part comprises a cabinet body 5 with an opening at the top and an opening at the bottom and a bundling block arranged in the cabinet body 5, and a guide groove for collecting and passing a plurality of elastic fibers sprayed from the spinning mechanism is vertically arranged on the bundling block.
The side blowing part comprises a first limiting rod 61, a second limiting rod 62, a first blowing device 63 and a second blowing device, the first limiting rod 61 is fixed on the support 1 below the bottom opening 51 of the cabinet body 5, the first blowing device 63 is located on the side portion below the first limiting rod 61, the second limiting rod 62 is located on the side portion below the first blowing device 63, the second limiting rod 62 is fixed with the support 1 below the first limiting rod 61, the first limiting rod 61 is perpendicular to the second limiting rod 62, and the second blowing device is located on the support 1 on one side of the second limiting rod 62. The specific structure of the first and second air blowers 63 and 63 is known in the art and will not be described in detail.
The first winding part comprises a third limiting rod 71 and a winder 7, the third limiting rod 71 is positioned on the bracket 1 below the second air blower, an elastic fiber inlet opening of the winder 7 is positioned below the third limiting rod 71, and elastic fibers entering the winder 7 are wound on a roller body 72 of the winder 7. The specific structure of the winder 7 is prior art and will not be described in detail.
The heat setting part comprises a positioning frame 8, a first stretching roller 81, a heat setting box 82, a false twisting part, a second setting part 83, a second stretching roller 811, an oiling groove 84 and a third stretching roller 85; the first drawing roller 81 is rotatably connected to a positioning frame 8, a guide rod is arranged on the positioning frame 8 above the first drawing roller 81, the guide rod corresponds to a thread inlet of a heat setting box 82, a conduit 821 is arranged at an outlet of the heat setting box 82, an outlet of the conduit 821 corresponds to a false twisting rod of a false twisting part, a guide wheel is arranged on the positioning frame 8 outside the outlet of the false twisting part, a second winding part is arranged on the positioning frame 8 below the false twisting part, a second setting part 83 is arranged on the positioning frame 8 behind the second winding part, the second drawing roller 811 is positioned below the second setting part 83, an upper oil groove 84 is positioned below the second drawing roller 811, a third drawing roller 85 corresponds to the second drawing roller 811, and the third drawing roller 85 is connected in front of the second winding part. The specific construction of the heat setting box 82 and false twister 86 of the false twist section is well known in the art and will not be described in detail.
The positioning frame 8 is provided with a placing rod capable of placing a winding drum wound with the composite fiber and a yarn guide pipe 80 capable of guiding the composite fiber, the yarn guide pipe 80 is connected to the top of the positioning frame 8, and the first drawing roller 81 corresponds to the outlet of the yarn guide pipe 80. The positioning frame 8 above the first stretching roller 81 is provided with a turning rod and a bundling rod, composite fibers passing through the first stretching roller 81 stretch into the heat setting box 82 through the turning rod and the bundling rod, the heat setting box 82 is obliquely arranged relative to the positioning frame 8, and the horizontal distance between the top of the heat setting box 82 and the bundling rod is smaller than the horizontal distance between the bottom of the heat setting box 82 and the bundling rod. The beam-collecting rod is a guide rod with beam-collecting blocks distributed on the cross rod at intervals, and the specific structures of the turning rod and the beam-collecting rod belong to the prior art, so that detailed description is omitted.
The false twisting part comprises a false twister 86, a false twisting guide wheel 87 and a fiber guide block 88, wherein the false twisting guide wheel 87 is arranged at the upper part of the false twister 86, the outlet of a conduit 821 of the heat setting box 82 is positioned above the false twisting guide wheel 87, and the composite fiber after false twisting by the false twister 86 leaves the false twisting part through a vertical guide groove on the fiber guide block 88. The guide wheel is arranged below the fiber guide block 88, the second shaping part 83 comprises heating pipes capable of penetrating the composite fiber and a shaping heater capable of heating the pipeline, and the heating pipes are distributed on the positioning frame 8 behind the second winding part at intervals. The second winding portion includes a winding roller 89, a winding roller holder rotatably connected to the positioning frame 8, the winding roller 89 connected to the winding roller holder, and a guide roller 891 connected to the positioning frame 8 on the front side of the winding roller 89. The second drawing roll 811 is located below the heating pipe, and a pressing roll 841 is provided in the upper oil sump 84 so that the composite fiber is immersed in oil.
The working principle is as follows: functional composite elastic fiber is realized by adding proper amount of functional substances on different components through a parallel composite spinning technology. Wherein the PET component adopts a third monomer and a fourth monomer which are added with long chain fatty acid or alcohol, polyether polyol and the like to obtain a modified low-viscosity PET slice with the viscosity of 0.46-0.56dl/g, and can be dyed at low temperature and normal pressure; the PBT component is a functional master batch prepared by increasing the viscosity to 0.9-1.25dl/g by a liquid phase or solid phase tackifying technology and adding functional substances. The modified PET component and the PBT functional component are respectively placed into respective melt pipelines of parallel composite spinning equipment, functional master batches are injected into the PBT pipelines through injectors, respectively melted and flow into spinneret orifices of a spinneret mechanism along the respective melt pipelines, the functional master batches are jointly extruded at certain extrusion temperature and with the spinneret orifices in aperture proportion, and further the functional master batches are subjected to drawing, cross-blowing, heat setting and winding to form the environment-friendly PBT/PET composite elastic fiber with the functions of low-temperature dyeability, high elasticity, antibiosis, permeation prevention, static resistance and the like. Functional substances are added into the PBT elastic component with smaller apparent viscosity, and the PET component is modified, so that the problems that elastic and unwinding are influenced and tension fluctuation and broken ends occur due to the fact that functional substances are added into the PET component or the two components respectively, and the bilateral phenomenon exists in common PET/PBT fiber dyeing are solved.

Claims (10)

1. A preparation method of PET and PBT composite elastic fiber comprises the following steps,
firstly, respectively manufacturing a PET slice and a PBT slice;
secondly, respectively placing the prepared PET slices and PBT slices into a parallel composite spinning device, and respectively melting the PET slices and the PBT slices through respective melt pipelines and flowing to a spinning mechanism of the parallel composite spinning device along the respective melt pipelines;
thirdly, extruding the molten PET slices and the molten PBT slices out of a spinneret hole of a spinneret mechanism together;
fourthly, drawing, cross-blowing, heat setting and winding the extruded mixed filament;
the method is characterized in that: in the first step, the PBT slice is a PBT slice with the viscosity of 0.9-1.25dl/g formed by liquid-phase tackifying of a polycondensation kettle in the polymerization process or solid-phase tackifying after polymerization;
in the second step, 1-10% by mass of PBT functional master batch is added into a melt pipeline of the PBT slice through an injector;
in the third step, the molten PET slices and the molten PBT slices are extruded together from two spinneret orifices with the aperture ratio of 3.5: 6.5-6.5: 3.5, the PET is adhered to the PBT to be extruded together in the extrusion process, and the PET and PBT composite elastic fiber which can be dyed at the temperature of 90 ℃ under normal pressure, has the dye uptake of 86.2-92.8%, the K/S value of 20.42-23.74 and the curling elastic elongation of more than 30% is obtained through the fourth step after extrusion.
2. The method for preparing an elastic fiber compounded of PET and PBT according to claim 1, characterized in that: the functional PBT master batch is prepared by melting, mixing, stretching and slicing a PBT resin and a functional material, wherein the functional material is one or a mixture of zinc oxide, a silver antibacterial agent, a titanium dioxide anti-penetration agent, an antistatic agent, a flame retardant, far infrared powder, a negative oxygen ion material, magnetic therapy powder and the like.
3. The method for preparing an elastic fiber compounded of PET and PBT according to claim 2, characterized in that: the functional material in the PBT functional master batch is 80-95 wt%.
4. The method for preparing PET and PBT composite elastic fiber according to claim 3, wherein the method comprises the following steps: the PBT slice has the glass transition temperature of 22-43 ℃, the melting point of 220-230 ℃ and the viscosity of 1.02-1.25 dl/g.
5. The method for preparing an elastic fiber compounded of PET and PBT according to claim 1, characterized in that: the step two of melting respectively means that the PET slices are melted in a melt pipeline with one side of melting temperature of 260-280 ℃ and cut by a screw; and melting the PBT slices and the PBT master batches in a melt pipeline with the melting temperature of 250-270 ℃ at the other side and cut by a screw.
6. The method for preparing an elastic fiber compounded of PET and PBT according to claim 1, characterized in that: in the third step, the extrusion temperature is 260-270 ℃.
7. The method for preparing an elastic fiber compounded of PET and PBT according to claim 1, characterized in that: the drawing refers to drawing the extruded mixed yarn to elongate and thin the yarn bundle, so that fiber macromolecules in the mixed yarn are gradually straightened, and the drawing multiple is 2-6 times; the lateral blowing is cooling and solidifying mixed yarn in a drafting channel, the wind pressure is 50-300 Pa, the wind temperature is 10-50 ℃, the wind speed is 50-80%, and the wind speed is 0.4-0.7 m/s; the heat setting means that the drawn mixed filament is kept at the temperature in a heat setting device for a period of time, so that the fiber structure of the drawn mixed filament is stable, the temperature is 80-150 ℃, and the heat treatment time is 5-30 min.
8. The method for preparing an elastic fiber in which PET and PBT are compounded according to claim 1, wherein: the parallel composite spinning device comprises a bracket, a first blanking part, a second blanking part, a pre-crystallization part, a first drying part, a second drying part, a first melting part, a second melting part, a spinning mechanism, a spinning beam-collecting part, a side blowing part, a first winding part, a heat setting part and a second winding part;
the spinning mechanism comprises a support, a first blanking portion, a second blanking portion, a discharging pipe, a pre-crystallizing portion, a discharging pipe, a first melting portion, a second melting portion, a spinning mechanism and a second winding portion, wherein the first blanking portion and the second blanking portion are connected to the support respectively, the discharging pipe of the first blanking portion is connected with the pre-crystallizing portion, the discharging pipe of the pre-crystallizing portion is connected with the first drying portion, the discharging pipe of the second blanking portion is connected with the second drying portion, the discharging pipe of the first drying portion is connected with the first melting portion, the discharging pipe of the second drying portion is connected with the second melting portion, the discharging ports of the first melting portion and the second melting portion are communicated with a feeding port of the spinning mechanism respectively, the discharging port of the spinning mechanism is located above the spinning winding portion, a bottom opening of the spinning winding portion is located above the side blowing portion, the first winding portion is located below the side blowing portion, the heat setting portion is located on one side of the first winding portion, and the second winding portion is connected to the heat setting portion.
9. The method for preparing an elastic fiber compounded of PET and PBT according to claim 8, characterized in that: the spinning mechanism comprises a positioning shell for mounting a spinning piece, and a material feeding body, a connecting body, a first stirring piece, a second stirring piece, a third stirring piece, a fourth stirring piece and a fifth stirring piece which are sequentially arranged in the positioning shell, wherein the top of the material feeding body extends out of an opening in the top of the positioning shell.
10. The method for preparing an elastic fiber compounded of PET and PBT according to claim 8, characterized in that: the heat setting part comprises a positioning frame, a first stretching roller, a heat setting box, a false twisting part, a second setting part, a second stretching roller, an upper oil groove and a third stretching roller;
first drawing roller can connect on the locating rack with rotating, is provided with the guide bar on the locating rack of first stay cord roller top, the guide bar is corresponding with the inlet wire mouth of thermal setting case, the export of thermal setting case is provided with the conduit, the export of conduit is corresponding with the false twist pole of false twist portion be provided with the guide pulley on the locating rack in the export outside of false twist portion, second winding portion sets up on the locating rack of false twist portion below, second winding portion sets up on the locating rack at second winding portion rear, and the second drawing roller is located second winding portion below, it is located the below of second drawing roller to go up the oil groove, third stay cord roller is corresponding with the second drawing roller, the place ahead at second winding portion is connected to the third drawing roller.
CN202210222939.7A 2022-03-09 2022-03-09 Preparation method of PET and PBT composite elastic fiber Pending CN114592248A (en)

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Application publication date: 20220607