CN110438583B - Polyester fiber and preparation method thereof - Google Patents
Polyester fiber and preparation method thereof Download PDFInfo
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- CN110438583B CN110438583B CN201810407521.7A CN201810407521A CN110438583B CN 110438583 B CN110438583 B CN 110438583B CN 201810407521 A CN201810407521 A CN 201810407521A CN 110438583 B CN110438583 B CN 110438583B
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a polyester fiber and a preparation method thereof, wherein polyester is produced under the condition of a titanium catalyst, and then hyperbranched polyester is added for melt spinning to obtain the polyester fiber. After the hyperbranched polyester is added, due to the fact that hyperbranched polyester molecules have a large number of terminal hydroxyl groups, metal atoms of a catalyst are coordinated with oxygen on ester carbonyl in a polyester PET macromolecular chain and are also coordinated with ester carbonyl oxygen in a hyperbranched polyester terminal group, namely the activity of a titanium catalyst is inhibited after the hyperbranched polyester is added, the thermal degradation degree of the polyester in the post-processing spinning process is greatly reduced, and the problems that the viscosity is greatly reduced, small molecules are separated out much, the pre-spinning spinnability is poor and the like caused by large thermal degradation in the post-processing process of the titanium polyester are solved. And meanwhile, the hyperbranched polyester has a function of restraining the main chain macromolecules through coordination with metal atoms of a catalyst and a function of blocking the PET polyester macromolecular chains by a hyperbranched polyester network structure, so that the amorphous area of the obtained fiber is increased, the decrement rate is improved during alkali decrement treatment, and the production energy consumption is reduced.
Description
Technical Field
The invention relates to a fiber, in particular to a polyester fiber and a preparation method thereof.
Background
The polyester fiber is prepared by spinning and post-treating PET polyester, the PET polyester is mainly synthesized by a direct esterification method at present, the direct esterification method takes terephthalic acid (PTA) and Ethylene Glycol (EG) as raw materials, dihydroxy ethyl terephthalate (BHET) is generated by direct esterification and dehydration, and the BHET is further condensed to remove EG to generate PET or generates a dehydration reaction with terminal carboxyl to generate PET.
The reaction rate constants of the catalytic polycondensation and the degradation of different catalysts are different, and the catalytic degradation speed is high while the positive reaction speed of the titanium compound is high. The catalyst has high catalytic activity on the polycondensation reaction, and the coordination ability of titanium and BHET ester carbonyl oxygen is strong, so the catalyst shows very high activity. The titanium compound also facilitates the thermal degradation reaction due to its strong coordination ability to the ester carbonyl oxygen. At present, titanium polyester is melted and then is subjected to the preparation process of products such as filaments, short fibers, films and the like, and due to poor thermal stability, the melt viscosity is greatly reduced, the precipitation of small molecules is more, and the spinnability of pre-spinning is poor during production and processing, which is particularly characterized in that the irregular pulp mass is more during the pre-spinning, so that the frequency of regularly repairing plates is increased, the irregular pulp mass is increased, and the problems of roller winding and the like caused by the pulp mass problem are serious. At present, the heat stabilizer is generally added to solve the problem in the industry for improvement, but the effect is not ideal.
In addition, the traditional polyester fabric has poor moisture absorption and wearability, and no matter the polyester fabric is a common polyester fabric or an ultrafine polyester fabric, all the processed polyester silk-like fabric needs to be subjected to alkali decrement treatment, so that the fabric achieves the hand feeling of silk-like fabric, and the requirements of various indexes such as wearability and the like are met. The alkali deweighting process is to treat the polyester fabric in high-temperature and concentrated caustic soda solution, so that the treated polyester fabric becomes thin, the moisture absorption and moisture regain rate is improved, and the strength is reduced.
The alkali weight reduction treatment brings a plurality of advantages to the polyester fabric, but the COD concentration of the wastewater discharged in the alkali weight reduction process can reach 90000mg/L, the pH value can reach more than 13, and the wastewater contains a large amount of TA (terephthalic acid) or sodium salt thereof and a small amount of polymers with different polymerization degrees. Most of TA can be recovered from the alkali decrement waste water through the treatment processes of acid precipitation and the like, but the alkali decrement waste water still contains TA and macromolecular organic matters, belongs to high-concentration refractory organic waste water, and is mixed with the printing and dyeing waste water to form the alkali decrement printing and dyeing waste water with complex components, high COD concentration, high pH value and poor biodegradability.
At present, the alkali weight reduction processing of the conventional polyester fabric mainly comprises two types: firstly, the high-temperature and high-pressure process has the processing temperature generally higher than 100 ℃ and higher requirements on equipment; the other is a normal pressure process, the processing temperature is generally higher than 95 ℃, and the requirements on alkali liquor concentration and the dosage of the accelerator are higher. It can be seen that the existing alkali reduction processing method has high energy consumption on one hand and serious wastewater pollution generated in the processing process on the other hand.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a polyester fiber and a preparation method thereof aiming at the defects of the prior art, the thermal degradation problem of the obtained titanium polyester in the post-processing process is greatly improved by utilizing the combined action of a titanium catalyst and hyperbranched polyester, the decrement rate of the obtained fiber is improved, the alkali decrement process can be weakened, the energy is saved, the consumption is reduced, and the pollution degree of alkali decrement wastewater to the environment is reduced.
The technical scheme is as follows: a polyester fiber is prepared by adding hyperbranched polyester into polyester produced under the condition of a titanium catalyst for melt spinning.
A process for preparing polyester fibre includes such steps as preparing polyester by direct esterifying method with dibasic acid and dibasic alcohol as main raw materials and titanium catalyst, mixing with hyperbranched polyester, and melt spinning.
Further, the titanium-based catalyst is STIC-01.
Further, the addition amount of the titanium catalyst is 5 to 10mg/kg based on the mass of the raw material polyester.
Further, the titanium-based catalyst is added before or after esterification.
Further, the production process of the polyester comprises esterification reaction, pre-polycondensation reaction and final polycondensation reaction; wherein the esterification temperature is 255-265 ℃, and the pressure is normal pressure; the pre-polycondensation temperature is 270-278 ℃, and the pressure is 2-24 KPa; the final polycondensation temperature is 278-283 ℃, and the pressure is 90-150 Pa; and then granulating and drying to obtain the polyester chip.
Furthermore, the addition amount of the hyperbranched polyester accounts for 1-5% of the mass of the raw material polyester.
Further, adding a delustering agent TiO after esterification reaction2The addition amount of the polyester resin accounts for 0.3 percent of the mass of the raw material polyester.
Further, the preparation process of the FDY filament by adopting the chip indirect spinning comprises the following steps: drying raw material polyester chips, mixing the dried raw material polyester chips with the dried hyperbranched polyester, extruding, melting and plasticizing the mixture, and spinning the mixture through spinning, wherein the hyperbranched polyester is added in the spinning process; the screw temperature is 285-300 ℃, the spinning box temperature is 282-288 ℃, the cooling air temperature is 20-25 ℃, the drafting temperature is 90-95 ℃, the setting temperature is 160-165 ℃, and the winding speed is 4500-4800 m/min.
Further, the hyperbranched polyester is prepared by A2+B3The system is prepared by polycondensation, has an aromatic-aliphatic molecular skeleton structure, is prepared by condensation at the temperature of 120-5000-.
The invention principle is as follows: after the hyperbranched polyester is added, the hyperbranched polyester molecules have a large number of terminal hydroxyl groups
So that the metal atoms of the catalyst are coordinated with the oxygen on the ester carbonyl in the macromolecular chain of the polyester PET and simultaneously coordinated with the ester carbonyl oxygen in the terminal group of the hyperbranched polyester:
Has the advantages that: (1) compared with the pure titanium polyester, the polyester mixture has the following specific expression that the thermal degradation degree is greatly reduced when the polyester mixture is used for processing after melt spinning: the viscosity of the oilless silk is reduced from 0.030dL/g to 0.02-0.01dL/g, and the amplitude is reduced by 33.3-66.6%. Further shown is improved spinnability, specifically: the pre-spun micromolecules are precipitated and the irregular board repair is reduced, the irregular average value is reduced from 6 times/day to 1-4 times/day, and the frequency of the regular board repair is prolonged from 1 time/12 h to 1 time and 24-60 h.
(2) Meanwhile, compared with pure titanium terylene products, the stocking knitted by FDY filaments produced by the mixture polyester has the advantage that the decrement rate can be improved by 14-60% under the same alkali decrement process.
Detailed Description
The technical solution of the present invention is described in detail below, but the scope of the present invention is not limited to the embodiments.
Example (b):
comparative example: firstly, preparing titanium polyester chips, and then preparing FDY filaments, wherein the preparation method specifically comprises the following steps: the polyester raw material used for spinning is produced by a polyester device with a five-kettle process of 3 ten thousand tons/year, the dibasic acid is purified terephthalic acid, the dibasic alcohol is ethylene glycol, the molar ratio of the alcohol acid is 1.1:1, the product type is semi-dull, the catalyst used is a STIC-01 titanium catalyst, the catalyst is added before esterification, and the addition amount is 5mg/kg (relative to the mass of polyester PET); delustering agent TiO2Added after esterification in an amount of 0.3% (based on the mass of the polyester PET). The specific process is that the temperature of the first esterification kettle is 265 ℃, the temperature of the second esterification kettle is 262 ℃, and the esterification process is normal pressure esterification; the temperature of the first pre-shrinking kettle is 273 ℃, the pressure is 24KPa, the temperature of the second pre-shrinking kettle is 278 ℃, and the pressure is 4 KPa; the final polycondensation temperature is 283 ℃, and the pressure is 150 Pa. Then the polyester chips are obtained after being granulated and driedPreparing the slice spinning FDY filament, specifically comprising the following steps: the temperatures of the first zone and the sixth zone of the screw are 285 ℃, 288 ℃, 290 ℃, 293 ℃, 295 ℃ and 300 ℃, the temperature of the spinning box is 288 ℃, the temperature of the cooling air is 23 ℃, and the air speed is as follows: 1.2m/s, a drafting temperature of 95 ℃, a setting temperature of 160 ℃ and a winding speed of 4500 m/min. The viscosity of the oilless silk is reduced to 0.03dL/g, the average irregular plate repair frequency of 24 spinning positions of single threads is 6 times/day, and the regular plate repair period is 1 time/12 hours.
The FDY filaments prepared above were subsequently knitted into a welt on a dye test knitting machine (model KU483B) and then subjected to an alkali deweighting test according to the following alkali deweighting process: the method adopts an impregnation process and sodium hydroxide to carry out alkali reduction processing on the material, and the alkali reduction processing process flow is as follows: preparing sodium hydroxide into a solution with the concentration of 20g/L, then putting the pure titanium sock band into an alkali liquor, wherein the alkali decrement bath ratio is 1:50, heating to 100 ℃ at the heating rate of 3.75 ℃/min, preserving heat for 60min, taking out the sock band after heat preservation, washing the sock band with tap water for 3 times, then placing the sock band in a 60 ℃ blast oven for drying for 1h, heating to 105 ℃ for drying for 4h, then rapidly weighing on an electronic balance, and calculating the decrement rate according to the following formula (1):
example 1: the polymerization, spinning process and alkali decrement processing process routes are the same as those of the comparative example, except that the specific process during polymerization is that the temperature of a first esterification kettle is 265 ℃, and the temperature of a second esterification kettle is 262 ℃; the temperature of the first pre-shrinking kettle is 273 ℃, the pressure is 24KPa, the temperature of the second pre-shrinking kettle is 278 ℃, and the pressure is 4 KPa; the final polycondensation temperature is 283 ℃, and the pressure is 150 Pa. And hyperbranched polyester accounting for 1 percent of the mass of the polyester is added during spinning, and the number average molecular weight of the hyperbranched polyester is 3000. The temperatures of the first zone and the sixth zone of the screw are 285 ℃, 288 ℃, 290 ℃, 293 ℃, 295 ℃ and 300 ℃, the temperature of the spinning box is 288 ℃, the temperature of the cooling air is 25 ℃, and the air speed is as follows: 1.2m/s, a drafting temperature of 95 ℃, a setting temperature of 160 ℃ and a winding speed of 4500 m/min. The viscosity of the oilless filaments is reduced to 0.02dL/g, the number of times of plate repair for 24 spinning positions of single thread in an indefinite period is 4 times/day, and the period of plate repair for a definite period is 1 time/24 hours.
Example 2: the polymerization, spinning process and alkali decrement processing process routes are the same as those of the comparative example, except that the specific process during polymerization is that the catalyst is added after esterification, the temperature of a first esterification kettle is 265 ℃, and the temperature of a second esterification kettle is 261 ℃; the temperature of the first preshrinking kettle is 272 ℃, the pressure is 20KPa, the temperature of the second preshrinking kettle is 277 ℃, and the pressure is 3 KPa; the final polycondensation temperature was 282 ℃ and the pressure was 140 Pa. And (3) adding hyperbranched polyester accounting for 2% of the mass of the polyester during spinning, wherein the number average molecular weight of the hyperbranched polyester is 3500. The temperatures of the first zone and the sixth zone of the screw are 285 ℃, 286 ℃, 288 ℃, 290 ℃, 291 ℃, 295 ℃, the temperature of a spinning box body is 285 ℃, the temperature of cooling air is 23 ℃, the drafting temperature is 95 ℃, the setting temperature is 162 ℃ and the winding speed is 4600 m/min. The viscosity of the oilless filaments is reduced to 0.015dL/g, the average irregular plate repair frequency of 24 spinning positions of a single thread is 3 times/day, and the regular plate repair period is 1 time/36 hours.
Example 3: the polymerization, spinning process and alkali decrement processing process routes are the same as those of the comparative example, except that the specific process during polymerization is that the addition amount of the catalyst is 7mg/kg, the temperature of the first esterification kettle is 263 ℃, and the temperature of the second esterification kettle is 259 ℃; the temperature of the first pre-shrinking kettle is 271 ℃, the pressure is 22KPa, the temperature of the second pre-shrinking kettle is 276 ℃, and the pressure is 3 KPa; the final polycondensation temperature is 280 ℃ and the pressure is 100 Pa. And (3) adding hyperbranched polyester accounting for 3.5 percent of the mass of the polyester during spinning, wherein the number average molecular weight of the hyperbranched polyester is 4000. The temperatures of the first zone and the sixth zone of the screw are 285 ℃, 286 ℃, 287 ℃, 289 ℃, 291 ℃, 293 ℃, the temperature of a spinning box is 285 ℃, the temperature of cooling air is 22 ℃, the drafting temperature is 92 ℃, the setting temperature is 164 ℃, and the winding speed is 4700 m/min. The viscosity of the oilless filaments is reduced to 0.010dL/g, the average irregular board repair frequency of 24 spinning positions of single threads is 2 times/day, and the regular board repair period is 1 time/48 hours.
Example 4: the polymerization, spinning process and alkali decrement processing process routes are the same as those of a comparative example, except that the specific process during polymerization is that the addition amount of a catalyst is 10mg/kg, the temperature of a first esterification kettle is 260 ℃, and the temperature of a second esterification kettle is 255 ℃; the temperature of the first pre-shrinking kettle is 270 ℃, the pressure is 20KPa, the temperature of the second pre-shrinking kettle is 274 ℃, and the pressure is 2 KPa; the final polycondensation temperature was 278 ℃ and the pressure was 90 Pa. And hyperbranched polyester accounting for 5 percent of the mass of the polyester is added during spinning, and the number average molecular weight of the hyperbranched polyester is 5000. The temperatures of the first zone and the sixth zone of the screw are 285 ℃, 286 ℃, 288 ℃, 289 ℃ and 292 ℃, the temperature of a spinning box body is 282 ℃, the temperature of cooling air is 20 ℃, the drafting temperature is 90 ℃, the setting temperature is 165 ℃ and the winding speed is 4800 m/min. The viscosity of the oilless filaments is reduced to 0.010dL/g, the average irregular board repair frequency of 24 spinning positions of single threads is 1 time/day, and the regular board repair period is 1 time/60 hours.
Comparative examples and examples 1-4 fiber preparation and alkali weight loss processing data are given in the following table:
Claims (9)
1. a polyester fiber is characterized in that: polyester is produced under the condition of a titanium catalyst, and then hyperbranched polyester is added for melt spinning to obtain the polyester;
the titanium catalyst is STIC-01;
the number average molecular weight of the hyperbranched polyester is 3000-5000, and the terminal group is hydroxyl.
2. A preparation method of polyester fiber is characterized by comprising the following steps: using dibasic acid and dihydric alcohol as main raw materials, adding a titanium catalyst, producing raw material polyester by adopting a direct esterification method, mixing the raw material polyester with hyperbranched polyester to carry out melt spinning;
the titanium catalyst is STIC-01;
the number average molecular weight of the hyperbranched polyester is 3000-5000, and the terminal group is hydroxyl.
3. The method for preparing polyester fiber according to claim 2, wherein: the adding amount of the titanium catalyst is 5-10mg/kg relative to the mass of the raw material polyester.
4. The method for preparing polyester fiber according to claim 2, wherein: the titanium catalyst is added before or after esterification.
5. The method for preparing polyester fiber according to claim 2, wherein: the production process of the polyester comprises esterification reaction, pre-polycondensation reaction and final polycondensation reaction; wherein the esterification temperature is 255-265 ℃, and the pressure is normal pressure; the pre-polycondensation temperature is 270-278 ℃, and the pressure is 2-24 KPa; the final polycondensation temperature is 278-283 ℃, and the pressure is 90-150 Pa; and then granulating and drying to obtain the polyester chip.
6. The method for preparing polyester fiber according to claim 2, wherein: the addition amount of the hyperbranched polyester accounts for 1-5% of the mass of the raw material polyester.
7. The method for preparing polyester fiber according to claim 2, wherein: adding flatting agent TiO after esterification2The addition amount of the polyester resin accounts for 0.3 percent of the mass of the raw material polyester.
8. The method for preparing polyester fiber according to claim 5, wherein: the preparation process of the FDY filament by adopting the chip indirect spinning comprises the following steps: drying raw material polyester chips, mixing the dried raw material polyester chips with the dried hyperbranched polyester, extruding, melting and plasticizing the mixture, and spinning the mixture through spinning, wherein the hyperbranched polyester is added in the spinning process; the screw temperature is 285-300 ℃, the spinning box temperature is 282-288 ℃, the cooling air temperature is 20-25 ℃, the drafting temperature is 90-95 ℃, the setting temperature is 160-165 ℃, and the winding speed is 4500-4800 m/min.
9. The method for preparing polyester fiber according to claim 2, wherein: the hyperbranched polyester is prepared by A2+B3The system is prepared by condensation polymerization, has an aromatic-aliphatic molecular skeleton structure, takes isophthalic acid and trimethylolpropane as raw materials and p-toluenesulfonic acid as a catalyst, and is prepared by condensation at the temperature of 120-150 ℃.
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| CN111893587A (en) * | 2020-08-12 | 2020-11-06 | 中润科技股份有限公司 | Processing method of PBT (polybutylene terephthalate) polyester fiber for woolen sweater |
| CN114574981B (en) * | 2021-12-07 | 2023-02-28 | 浙江恒逸高新材料有限公司 | Preparation method of polyester staple fiber special for vortex spinning |
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| US20110152456A1 (en) * | 2009-12-17 | 2011-06-23 | E. I. Du Pont De Nemours And Company | Polyester Compositions with Good Melt Rheological Properties |
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