Preparation method of hydrolysis-resistant PBT polyester resin

A polyester resin, hydrolysis-resistant technology, applied in the field of polyester resin, can solve the problems of the influence of processing performance and color value, the decrease of product molecular weight, poor hydrolysis resistance, etc. High solution performance and high end-capping efficiency

Active Publication Date: 2020-06-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The invention provides a method for preparing a hydrolysis-resistant PBT polyester resin, the purpose of which is to solve the problem of poor hydrolysis resistance of PBT resins in the prior art, resulting in a decrease in product molecular weight, serious loss of mechanical properties, and limited applications...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A preparation method of hydrolysis-resistant PBT polyester resin, the steps are as follows:

[0046] (1) Preparation of prepolymer:

[0047] 1,4-butanediol and terephthalic acid with a mass ratio of 1:1, the addition amount is 90ppmw (calculated as titanium element) tetratitanate of the polymerization product of terephthalic acid and 1,4-butanediol Butyl ester and 20ppmw magnesium phosphate added as a polymerization product of terephthalic acid and 1,4-butanediol are mixed to form a slurry, added to a polymerization kettle, and subjected to esterification reaction to obtain a prepolymer, wherein, The pressure of esterification reaction is normal pressure (one standard atmospheric pressure), and temperature is 240 ℃, and the time is 150min;

[0048] (2) Prepare PBT polyester resin substrate:

[0049] After the esterification is completed, vacuumize and reduce the pressure to the system pressure of 50Pa. At the same time, the reaction temperature rises to 260°C, and the...

Embodiment 2

[0065] A preparation method of hydrolysis-resistant PBT polyester resin, the steps are as follows:

[0066] (1) Preparation of prepolymer:

[0067] 1,4-butanediol and terephthalic acid with a mass ratio of 1:1, the addition amount is 90ppmw (calculated as titanium element) tetratitanate of the polymerization product of terephthalic acid and 1,4-butanediol Ethylhexyl ester and 10ppmw magnesium phosphate, which is the polymerization product of terephthalic acid and 1,4-butanediol, are mixed to form a slurry, which is added to a polymerization kettle for esterification to obtain a prepolymer. Wherein, the pressure of the esterification reaction is normal pressure, the temperature is 230°C, and the time is 160min;

[0068] (2) Prepare PBT polyester resin substrate:

[0069] After the esterification is completed, the pressure is reduced to 80 Pa, and the reaction temperature is raised to 245 ° C. The melt polycondensation reaction lasts for 115 minutes. After that, the reaction p...

Embodiment 3

[0075] A preparation method of hydrolysis-resistant PBT polyester resin, the steps are as follows:

[0076] (1) Preparation of prepolymer:

[0077]1,4-butanediol and terephthalic acid with a mass ratio of 1:1.2, the addition amount is 85ppmw (calculated as titanium element) tetratitanate of the polymerization product of terephthalic acid and 1,4-butanediol Butyl ester and 16ppmw magnesium phosphate added as the polymerization product of terephthalic acid and 1,4-butanediol are mixed to form a slurry, added to a polymerization tank, and subjected to esterification reaction to obtain a prepolymer, wherein, The pressure of the esterification reaction is normal pressure, the temperature is 240°C, and the time is 170min;

[0078] (2) Prepare PBT polyester resin substrate:

[0079] After the esterification is completed, vacuumize and reduce the pressure to the system pressure of 150Pa, and at the same time, the reaction temperature rises to 248 ° C, and the melt polycondensation r...

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Abstract

The invention relates to a preparation method of hydrolysis-resistant PBT polyester resin. The preparation method comprises the following steps: mixing terephthalic acid, 1, 4-butanediol, an organic titanate compound and magnesium phosphate to prepare slurry; carrying out esterification reaction to obtain a prepolymer; carrying out melt phase polycondensation reaction to obtain a PBT polyester resin substrate; and finally, mixing the PBT polyester resin substrate, an end-capping modifier and an organic phosphate compound in a twin-screw extruder, thereby obtaining the hydrolysis-resistant PBTpolyester resin. 97-99 parts by mass of the PBT polyester resin substrate, 0.5-1 part by mass of the end-capping modifier and 0.01-1 part by mass of the organophosphate compound are added in the mixing process. The end capping modifier is hyperbranched polyester of which the number of terminal hydroxyl groups is 6-100 and a branch unit contains 2, 2-dimethylolpropionic acid. The preparation methodis simple, and the prepared hydrolysis-resistant PBT polyester resin has excellent comprehensive performance.

Description

technical field [0001] The invention belongs to the technical field of polyester resin and relates to a preparation method of hydrolysis-resistant PBT polyester resin. Background technique [0002] Polybutylene terephthalate (PBT) is a thermoplastic polyester formed by polycondensation of terephthalic acid (PTA) and butanediol (BDO). It has excellent mechanical, physical and chemical properties, such as easy processing, High temperature resistance, chemical resistance, oil resistance, good mechanical strength and other properties, have been widely used in the fields of automobiles, machinery, instruments, electronics, household appliances, textiles and civilian use. [0003] PBT resin has excellent hydrolysis resistance under dry and hot conditions, but in many applications, such as underground optical cables, automotive parts, electrical appliances, solar films, etc., PBT resin is very prone to hydrolysis in the case of a large amount of moisture and high temperature aging....

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/91C08G63/78C08G63/85C08G63/83
CPCC08G63/183C08G63/78C08G63/83C08G63/85C08G63/916
Inventor 关震宇张玉梅王华平
Owner DONGHUA UNIV
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