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Preparation method of heat-sensitive copolyester fiber

A technology of copolyester and heat sensitivity, which is applied in the direction of one-component copolyester rayon and one-component polyetherester rayon, etc., which can solve the problems of broken ends, poor thermal stability, and the influence of polyester fiber formation, etc. question

Active Publication Date: 2018-10-16
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The following problems exist in the preparation of existing heat-sensitive polyester materials: 1) in the preparation process of heat-sensitive polyester and its copolyester, the molar ratio of dibasic acid to dibasic alcohol-acid in the existing technical system is far high At a ratio of 1:1, diols undergo self-condensation at a high alkyd molar ratio to generate by-products, which have a greater impact on the fiber-forming properties of polyester. At the same time, high molar ratios require more diol raw materials to be consumed. Increase the cost; 2) for polyester, the esterification stage is directly related to the quality of the final polycondensation product. Although some new monomers have huge application potential advantages, their thermal stability is relatively poor, and the prior art has a high alkyd mole It is necessary to carry out sufficient esterification reaction under the esterification time of more than 3 hours, which is very easy to cause the generation of side reactions in the esterification process; To obtain polyester, the intrinsic viscosity of the precondensation product is generally above 0.25dL / g, which causes the molecular weight distribution of the final product to be wide, and the processing performance is not good, and wool, broken ends, waste 4) At present, the melt transportation of heat-sensitive polyester and its copolyester mainly improves the transportation quality by reducing the transportation temperature, but the low-temperature transportation increases the residence time of the melt in the pipeline, and there are still large Viscosity drops, resulting in poor spinnability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A method for preparing heat-sensitive copolyester fiber, the specific steps are as follows:

[0053] (1) Esterification reaction;

[0054] After mixing and beating terephthalic acid and propylene glycol at a molar ratio of 1:1.05, the titanium-silico-cobalt composite catalyst is added and the guide is carried out at 180°C and 100KPa until the water output reaches 95% of the theoretical water output, and the reaction is terminated. The guide is an esterified product with an esterification rate of 90% formed by the reaction of terephthalic acid and propylene glycol. The addition amount of the guide is 5.0wt% of terephthalic acid, and the addition amount of the titanium silicon cobalt composite catalyst is terephthalic acid The mass of 110ppm, the titanium-silicon-cobalt composite catalyst is compounded by tetrabutyl titanate, silicon dioxide and cobalt acetate at a molar ratio of 1:0.8:0.1;

[0055] (2) Pre-polycondensation reaction;

[0056] Add phosphoric acid to the product o...

Embodiment 2

[0063] A method for preparing heat-sensitive copolyester fiber, the specific steps are as follows:

[0064] (1) Esterification reaction;

[0065] After mixing and beating terephthalic acid and propylene glycol at a molar ratio of 1:1.06, the titanium-silico-cobalt composite catalyst is added and the guide is carried out at 220°C and 150KPa until the water output reaches 95% of the theoretical water output. The reaction is terminated. The guide is terephthalic acid / succinic acid (mass ratio of 2:1) and propylene glycol, and the esterification rate is 95%. The addition amount of the guide is 4.5wt% of terephthalic acid, titanium The addition amount of the silicon-cobalt composite catalyst is 100 ppm of the mass of terephthalic acid, and the titanium-silicon-cobalt composite catalyst is compounded by a molar ratio of 1:2.5:0.5 of metatitanic acid, silicon dioxide and cobalt acetate;

[0066] (2) Pre-polycondensation reaction;

[0067] Add phosphorous acid to the product of step (1) and ...

Embodiment 3

[0074] A method for preparing heat-sensitive copolyester fiber, the specific steps are as follows:

[0075] (1) Esterification reaction;

[0076] After mixing and beating terephthalic acid and butylene glycol at a molar ratio of 1:1.07, add titanium-silicon-cobalt composite catalyst and guide at 230°C and 50KPa until the water output reaches 95% of the theoretical water output. The reaction is terminated. , Where the guide is an esterified product with an esterification rate of 98% produced by the reaction of terephthalic acid and butanediol / pentanediol (mass ratio 1:1), and the addition amount of the guide is 4.0wt of terephthalic acid %, the addition amount of the titanium silicon cobalt composite catalyst is 130 ppm of the mass of terephthalic acid. The titanium silicon cobalt composite catalyst is made of tetrabutyl titanate, silicon dioxide and cobalt acetate at a molar ratio of 1:5.0:4.0. ;

[0077] (2) Pre-polycondensation reaction;

[0078] Add trimethyl phosphate to the pro...

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Abstract

The invention relates to a preparation method of a heat-sensitive copolyester fiber. The preparation method comprises the following steps: mixing terephthalic acid, aliphatic diol I, a guide and a titanium-silicon-cobalt composite catalyst uniformly, then subjecting the mixture to an esterification reaction, a pre-polycondensation reaction and a final polycondensation in sequence to obtain heat-sensitive copolyester, and then preparing the heat-sensitive copolyester fiber by melt direct spinning; the aliphatic diol I is propylene glycol or butylene glycol; the guide is an ester compound generated by a reaction between dibasic acid and aliphatic diol II; the molar ratio of the terephthalic acid to the aliphatic diol I is 1:(1.05-1.10); the titanium-silicon-cobalt composite catalyst is formed by compounding a titanium-silicon composite catalyst and a cobalt catalyst; the titanium-silicon composite catalyst is obtained by loading a titanium-based catalyst with a silicon-based catalyst; and polysiloxane and a copolymerization component are added during the final polycondensation reaction. The preparation method provide by the invention is few in side reactions and high in reaction rate; an obtained product is concentrated in molecular weight distribution and good in quality; and the fiber is prepared with the melt direct spinning.

Description

Technical field [0001] The invention belongs to the field of polyester preparation, and specifically relates to a method for preparing a heat-sensitive copolyester fiber. Background technique [0002] Polyester refers to the general term for polymers obtained by polycondensation of polyols and polyacids. Mainly refers to polyethylene terephthalate (PET), customarily also includes linear thermoplastic resins such as polybutylene terephthalate (PBT) and polyarylate. It is a class of polymers with excellent properties and a wide range of uses. It has been widely used in fiber, plastic, film and other fields. In terms of the application of PET in the fiber field, the output of PET fiber in 2017 exceeded 39 million tons. [0003] Along with the diversified demand for clothing fiber products, more and more attention has been paid to the development of new polyester fiber materials, including new polyesters prepared from new monomers and copolyesters modified by copolymerization of exi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/84D01F6/86C08G77/46C08G77/445C08G77/455C08G63/183C08G63/85
CPCC08G63/183C08G63/85C08G77/445C08G77/455C08G77/46D01F6/84D01F6/86
Inventor 王华平吉鹏王朝生陈向玲陈烨张景春王宇
Owner DONGHUA UNIV
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