CN114592255A - Preparation method of low-temperature dyeable composite elastic fiber - Google Patents
Preparation method of low-temperature dyeable composite elastic fiber Download PDFInfo
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Images
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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
-
- 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
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
Abstract
A preparation method of low-temperature dyeable 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 are respectively melted and flow to a spinning mechanism; co-extruding from a spinneret orifice; the extruded mixed filament is subjected to drafting, cross-blowing, heat setting and winding; when PET slices are prepared, a component C is also added: the distance between the PET macromolecules is increased by the meta-aromatic dicarboxylic acid or the esters thereof, and meanwhile, the PBT slice is a PBT slice which is subjected to liquid phase tackifying through a polycondensation kettle in the polymerization process or solid phase tackifying after polymerization and has the viscosity of 0.9-1.25 dl/g; PET adheres to PBT and is co-extruded during extrusion. The invention has the advantages that: the composite elastic fiber produced by the invention has the characteristics of low-temperature normal-pressure dyeability, uniform coloring, large curling elasticity, uniform color of the prepared elastic fabric and good elasticity retentivity.
Description
Technical Field
The invention relates to the technical field of elastic fiber manufacturing, in particular to a preparation method of low-temperature dyeable composite elastic fiber.
Background
Compared with the homologues of polyethylene terephthalate (PET) and polytrimethylene terephthalate (PTT), the polybutylene terephthalate (PBT) has softer molecular chain and elasticity similar to PTT, has the glass transition temperature of 40-50 ℃ and the melting point of 225-235 ℃, can be dyed at low temperature and normal pressure, and has the glass transition temperature of 67-81 ℃, the melting point of 250-260 ℃, the macromolecular structure of conventional PET is compact, and the molecules lack groups for absorbing ionic dyes, so that the PBT is difficult to dye and needs to disperse and dye at high temperature or under the condition of adding carriers. 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. According to the PBT/PET composite elastic filament, the PET component is arranged on the outer side of the crimp helix, and the PBT component is arranged on the inner side of the crimp helix, due to the potential thermal shrinkage difference obtained in the spinning process, the crimp potential energy is released under post-processing, so that the fiber has a three-dimensional crimp effect, and excellent elasticity and fluffiness are endowed to the fiber.
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 a double-component elastic composite fiber product which is prepared by extruding and compounding a PBT melt and a PET melt at a spinneret micropore to form a single filament bundle, stretching, cooling, solidifying, winding and forming the single filament bundle, stretching, false twisting and deforming the single filament bundle and the PET melt by two groups of metering pumps and two groups of spinning components.
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.
The above published patent applications only specify that conventional PBT/PET self-crimping elastic fibers are realized by PBT of conventional viscosity and conventional PET of low viscosity according to a specific ratio and a general process flow. On the one hand, however, as mentioned above, the glass transition temperature of the conventional PET resin is 67-81 ℃, and the conventional PET resin needs to be dyed by disperse dye at 130 ℃ under high temperature and high pressure; the glass transition temperature of the PBT is 40-50 ℃, and the PBT can be dyed only at 90 ℃ under normal pressure. The difference of the dyeing temperature of the PBT/PET parallel self-crimping composite fiber and the dyeing temperature of the PBT/PET parallel self-crimping composite fiber prepared by the method is about 40 ℃, so that the phenomena of heterochrosis and nonuniform coloring often exist in dyeing, namely, the PBT component is dark in color and the PET component is light in color under the same dyeing condition, so that the color difference exists on two sides of the same filament; after the cloth cover is woven, uneven phenomena such as stripes and the like occur, and defective products are generated; on the other hand, although the color difference between the two components can be flattened by high-temperature dyeing at 130 ℃, the high dyeing temperature can limit the application of the filament in low-temperature dyeing varieties, such as wools, pure cotton fabrics and the like. In addition, in the side-by-side composite spinning, the viscosity matching of the two components must be proper, one component bears most of the spinning tension to obtain high orientation, and the other component adheres thereto to realize a larger amorphous region, so that a better curling elasticity can be obtained, and therefore, the preparation method of the above patent application needs to be improved.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the low-temperature dyeable composite elastic fiber which can be dyed at normal pressure and low temperature below 90 ℃ and has good elasticity aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the low-temperature dyeable 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 together from a spinneret orifice of a spinneret mechanism;
fourthly, drawing, cross-blowing, heat setting and winding the extruded mixed filament;
the method is characterized in that: in step one, the reaction is carried out by reacting component a: para-aromatic dicarboxylic acid or esters thereof and component B: when PET slices are prepared by aliphatic diol esterification reaction, the PET slices are also added with a component C: meta-aromatic dicarboxylic acid or esters thereof to increase the distance between the PET macromolecules, and component A, component B and component C are subjected to esterification reaction and then component D: carrying out polycondensation reaction on aliphatic polyether polyol, a catalyst and a composite stabilizer under the conditions of high temperature and high vacuum to obtain PET slices;
meanwhile, in the first step, the PBT slice is a PBT slice which is tackified by liquid phase of a polycondensation kettle in the polymerization process or tackified by solid phase after polymerization and has the viscosity of 0.9-1.25 dl/g;
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 in the extrusion process and extruded together, and the low-temperature dyeable composite elastic fiber which can be dyed at normal pressure at 90 ℃ and has the dye uptake of 88.7-94.3% is obtained through the fourth step after extrusion.
As a modification, the meta-aromatic dicarboxylic acid or the ester thereof may preferably be one or more of ethylene isophthalate, dihydroxy ethyl isophthalate-5-sodium sulfonate and diethyl isophthalate, and the aliphatic diol is a mixture of ethylene glycol and one or more of 1, 4-butanediol, 1, 3-propanediol and 1, 6-hexanediol.
Further improved, the glass transition temperature of the PET slices can be preferably 45-65 ℃, the melting point is 230-260 ℃, and the viscosity is 0.46-0.56 dl/g.
As an improvement, the glass transition temperature of the PBT slice is preferably 22-43 ℃, the melting point is 220-230 ℃, and the viscosity is 1.02-1.25 dl/g.
Further improvement, the step two of melting respectively preferably means that the PET slices are melted in a melt pipeline with one side 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.
As an improvement, in the third step, the extrusion temperature is preferably 260-270 ℃.
As an improvement, the drawing preferably 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 and 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 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.
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 elastic fiber, thereby enhancing the elasticity and the toughness of the composite elastic fiber, and compared with the fiber produced by the prior art, the tensile allowance of the composite elastic fiber is more than 150 percent. In addition, the composite elastic fiber produced by the invention has the characteristics of low-temperature normal-pressure dyeability, uniform coloring, large curling elasticity, uniform color of the prepared elastic fabric and good elasticity retentivity. According to the invention, the third, fourth and even more monomers are added in the PET polymerization process, so that the distance between PET macromolecules is increased, and disperse dye molecules can effectively enter the molecule, thereby realizing that the fibers and the fabric can be dyed by the disperse dye at low temperature and normal pressure. The modified low-viscosity PET is adopted to replace the conventional low-viscosity PET, and the modified low-viscosity PET and the fiber-grade high-viscosity PBT are subjected to parallel composite spinning, so that the problems of heterochrosis and uneven coloring in the conventional composite elastic fiber during dyeing at low temperature and normal pressure are solved, and the application of the modified low-viscosity PET in low-temperature dyeing varieties is improved. Specifically, the invention is characterized in that a parallel composite spinning technology is adopted, low-viscosity PET obtained by adding a third monomer, a fourth monomer and even more monomers through polymerization modification and high-viscosity PBT obtained by a liquid-phase tackifying or solid-phase tackifying technology are respectively placed into respective melt pipelines of a parallel composite spinning device, are respectively melted and flow to spinneret orifices of a spinneret mechanism along the respective melt pipelines, are extruded together at a certain extrusion temperature and at a certain aperture ratio, and are further subjected to drafting, cross-blowing, oiling, heating, secondary drafting, heat setting and winding to form the PBT/modified PET composite elastic fiber with low-temperature dyeability and high elasticity. The modified PET component can be dyed at low temperature and normal pressure like the PBT component, the problems of uneven coloring and color difference do not exist, and the high-low viscosity matching enables the prepared composite elastic wire to have large curling elasticity, high strength and small elastic loss.
Drawings
FIG. 1 is a perspective view of an embodiment of the present invention with the second winding portion and the heat-set portion removed;
FIG. 2 is a front perspective view of FIG. 1;
FIG. 3 is a perspective view of FIG. 1 at another angle;
FIG. 4 is a perspective view of FIG. 3 at another angle;
FIG. 5 is a bottom view of the bottom opening of the oven of FIG. 4;
FIG. 6 is a perspective view of a second winding section and a heat-set section in the embodiment of the invention;
FIG. 7 is a perspective view of FIG. 6 at another angle;
FIG. 8 is a perspective view of FIG. 7 at another angle;
FIG. 9 is a schematic diagram of the operation of the composite fiber heat setting of FIG. 6;
FIG. 10 is a perspective view of the spinning mechanism of FIG. 1;
FIG. 11 is a top view of FIG. 10;
FIG. 12 is a cross-sectional view taken along line A-A of FIG. 11 with the retaining shell removed;
FIG. 13 is an exploded view of the structure of FIG. 12;
FIG. 14 is a perspective view of FIG. 13 at another angle;
fig. 15 is an exploded view of the configuration of fig. 13 with five stirring blades remaining.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
(1) Carrying out a first-step esterification reaction by using terephthalic acid, ethylene glycol isophthalate, ethylene glycol and 1, 4-butanediol as raw materials, wherein 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 0.47dl/g and is used as a component A.
(2) 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent are adopted 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), granulation and other links, and PBT slices of 1.10dl/g are obtained by a liquid phase tackifying technology to be used as a 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 260, 263, 265, 266 ℃; B. screw temperature 256, 259 ℃) and flowed to parallel spinneret orifices along the respective melt pipelines, and at an extrusion temperature of 264 ℃, the ratio of two hole diameters is 5: 5 extruding spinneret orifices together; and (3) cross air blowing: wind pressure is 200Pa, wind temperature is 22 ℃, rheumatism is 70%, and wind speed is 0.55 m/s; heat setting at 120 deg.c for 20 min; drafting for 5 times, and winding speed is 2500 m/min.
The obtained PBT modified/PET composite elastic fiber has low-temperature dyeability and high elasticity, the fineness is 83dtex/36f, the strength is 2.68cN/dtex, the elongation is 23.82%, the crimp shrinkage is 36.2%, the crimp stability is 85.8%, the boiling water shrinkage is 15.2%, the fiber can be dyed under normal pressure at 90 ℃, the dye uptake is 90%, and the K/S value is 24.32.
Example 2
(1) Carrying out a first-step esterification reaction by using terephthalic acid, dihydroxy ethyl isophthalate-5-sodium sulfonate, isophthalic acid, ethylene glycol and 1, 3-propylene glycol as raw materials, wherein the feeding time is 3.5h, the temperature is 257-258 ℃, 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 0.49dl/g and is used as a component A.
(2) The method comprises the steps of performing 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 the like by adopting 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent, and obtaining PBT slices of 1.15dl/g as a component B by a liquid phase tackifying technology.
(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, 264, 267 ℃; B. screw temperature 252, 254, 256 ℃) and flowing to parallel spinneret orifices along the respective melt pipelines, wherein at extrusion temperature 262 ℃, the ratio of two pore diameters is 4: 6 extruding spinneret orifices together; and (3) cross air blowing: wind pressure is 200Pa, wind temperature is 22 ℃, rheumatism is 70%, and wind speed is 0.55 m/s; heat setting at 130 deg.C for 25 min; the draft was 4 times and the winding speed was 2600 m/min.
The obtained PBT/modified PET composite elastic fiber has low-temperature dyeability and high elasticity, the fineness is 83dtex/36f, the strength is 2.56cN/dtex, the elongation is 22.24%, the crimp shrinkage rate is 34.8%, the crimp stability is 84.7%, the boiling water shrinkage rate is 15.8%, the fiber can be dyed under normal pressure at 90 ℃, the dye uptake is 91%, and the K/S value is 24.64.
Example 3
(1) Terephthalic acid, diethyl isophthalate, sebacic acid, ethylene glycol and 1, 6-hexanediol are used as raw materials to carry out a first-step esterification reaction, the feeding time is 4.0h, the temperature is 255-256 ℃, and the esterification rate is 92-93%; and then adding polytetrahydrofuran diol 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 ℃, the pressure is not higher than 70Pa, so as to obtain a modified low-viscosity polyester slice dyed at low temperature and normal pressure, and the viscosity is 0.54dl/g and is used as a component A.
(2) The method comprises the steps of performing 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 the like by adopting 1, 4-butanediol, terephthalic acid, a catalyst and a polyamide nucleating agent, and obtaining PBT slices of 1.20dl/g as a component B by a liquid phase tackifying technology.
(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 of 200Pa, wind temperature of 40 deg.C (25 deg.C), rheumatism of 60%, and wind speed of 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/modified PET composite elastic fiber has low-temperature dyeability and high elasticity, the fineness is 83dtex/36f, the strength is 2.72cN/dtex, the elongation is 22.6 percent, the crimp shrinkage is 34.2 percent, the crimp stability is 84.2 percent, the boiling water shrinkage is 15 percent, the fiber can be dyed under normal pressure at the temperature of 90 ℃, the dye uptake is 91.8 percent, and the K/S value is 25.14
As shown in fig. 1 to 15, the method for preparing the low temperature dyeable 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 step one, the reaction is carried out by reacting component a: para-aromatic dicarboxylic acid or esters thereof and component B: when the PET slices are prepared by aliphatic diol esterification reaction, the PET slices are also added with a component C: meta-aromatic dicarboxylic acid or esters thereof to increase the distance between the PET macromolecules, and component A, component B and component C are subjected to esterification reaction and then component D: carrying out polycondensation reaction on aliphatic polyether polyol, a catalyst and a composite stabilizer under the conditions of high temperature and high vacuum to obtain PET slices;
meanwhile, in the first step, the PBT slice is a PBT slice with the viscosity of 0.9-1.25 dl/g formed by liquid-phase tackifying of a polycondensation kettle in the polymerization process or solid-phase tackifying after polymerization;
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 in the extrusion process and extruded together, and the low-temperature dyeable composite elastic fiber which can be dyed at normal pressure at 90 ℃ and has the dye uptake of 88.7-94.3% is obtained through the fourth step after extrusion.
The meta-aromatic dicarboxylic acid or the esters thereof are one or more of ethylene isophthalate, dihydroxy ethyl isophthalate-5-sodium sulfonate and diethyl isophthalate, and the aliphatic diol is a mixture of one or more of 1, 4-butanediol, 1, 3-propanediol and 1, 6-hexanediol and ethylene glycol. 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 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. 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; and the heat setting means that the drafted mixed yarn is kept at a temperature in a heat setting device for a period of time, so that the fiber structure of the drafted mixed yarn is stabilized, the temperature is 80-150 ℃, and the heat treatment time is 5-30 min.
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 air into the drying box, the top inlet of the drying box is connected with the discharge pipe of the first blanking part 21 through a valve, the side part of the drying box is connected with the air outlet pipe of the heater, the side part of the other side of the drying box is connected with the 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 crystal, the lower part of the first dryer is connected with a hot air pipeline, the bottom of the first dryer is connected with the first feeding hopper 411 of the first melting part 41 through a pipeline, 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 pipeline, and the bottom of the second dryer is connected with the second feeding hopper 421 of the second melting part 42 through a pipeline. 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 feeding hopper 411, a first screw barrel combination and a first blanking pipe which can feed the PBT melt from the first screw barrel combination into the oven 9, wherein an outlet of the first feeding hopper 411 is communicated with an inlet of the first screw barrel combination, an outlet of the first screw barrel combination is communicated with the first blanking pipe, and the first blanking pipe is communicated with a first inlet 911 of a spinneret mechanism in the oven 9.
The second melting part 42 comprises a second feed hopper 421, a second screw cylinder combination and a second blanking pipe which can feed the PET melt from the second screw cylinder combination into the oven 9, wherein the outlet of the second feed hopper 421 is communicated with the inlet of the second screw cylinder combination, the outlet of the second screw cylinder combination is communicated with the second blanking pipe, and the second blanking pipe is communicated with the second inlet 912 of the spinning 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.
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 part below the first limiting rod 61, the second limiting rod 62 is located on the side part 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. A second drawing roller 811 is located below the heating pipe, and a pressing roller 841 for immersing the composite fiber in oil is provided in the upper oil tank 84
The working principle is as follows: through the parallel composite spinning technology, low-viscosity PET obtained by adding third, fourth and even more monomers through polymerization modification and high-viscosity PBT obtained by liquid-phase tackifying or solid-phase tackifying technology are respectively placed into respective melt pipelines of a parallel composite spinning device, are respectively melted and flow to spinneret orifices of a spinneret mechanism along the respective melt pipelines, are jointly extruded at a certain extrusion temperature and at a certain aperture ratio, and are further subjected to drawing, cross-blowing, oiling, heating, secondary drawing, heat setting and winding to form the PBT/modified PET composite elastic fiber with low-temperature dyeability and high elasticity. The modified PET component can be dyed at low temperature and normal pressure like the PBT component, the problems of uneven coloring and color difference do not exist, and the high-low viscosity matching enables the prepared composite elastic wire to have large curling elasticity, high strength and small elastic loss.
Claims (10)
1. A preparation method of low-temperature dyeable 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 step one, the reaction is carried out by reacting component a: para-aromatic dicarboxylic acid or esters thereof and component B: when the PET slices are prepared by aliphatic diol esterification reaction, the PET slices are also added with a component C: meta-aromatic dicarboxylic acid or esters thereof to increase the distance between the PET macromolecules, and component A, component B and component C are subjected to esterification reaction and then component D: carrying out polycondensation reaction on aliphatic polyether polyol, a catalyst and a composite stabilizer under the conditions of high temperature and high vacuum to obtain PET slices;
meanwhile, in the first step, the PBT slice is a PBT slice with the viscosity of 0.9-1.25 dl/g formed by liquid-phase tackifying of a polycondensation kettle in the polymerization process or solid-phase tackifying after polymerization;
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 in the extrusion process and extruded together, and the low-temperature dyeable composite elastic fiber which can be dyed at normal pressure at 90 ℃ and has the dye uptake of 88.7-94.3% is obtained through the fourth step after extrusion.
2. The method of making a low temperature dyeable composite elastic fiber according to claim 1, wherein: the meta-aromatic dicarboxylic acid or the esters thereof are one or more of ethylene glycol isophthalate, dihydroxy ethyl isophthalate-5-sodium sulfonate and diethyl isophthalate, and the aliphatic diol is a mixture of one or more of 1, 4-butanediol, 1, 3-propanediol and 1, 6-hexanediol and ethylene glycol.
3. The method of making a low temperature dyeable composite elastic fiber according to claim 2, wherein: 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.
4. The method of making a low temperature dyeable composite elastic fiber according to claim 1, wherein: 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 of making a low temperature dyeable composite elastic fiber according to claim 4, wherein: 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 of making a low temperature dyeable composite elastic fiber according to claim 1, wherein: in the third step, the extrusion temperature is 260-270 ℃.
7. The method of making a low temperature dyeable composite elastic fiber according to claim 1, wherein: 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. A method of making a low temperature dyeable composite elastic fiber according to any one of claims 1 to 7, 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 of making a low temperature dyeable composite elastic fiber of claim 8, wherein: 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 of making a low temperature dyeable composite elastic fiber according to claim 8, wherein: 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.
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