Preparation method of thermal degradation-resistant degradation PBT polyester with high viscosity

A high-viscosity, heat-resistant technology, applied in the field of PBT polyester preparation, can solve the problems of thermal degradation of PBT melt and the addition of multiple chain extenders, etc., to achieve stable properties, reduce the content of terminal carboxyl groups, and increase the esterification rate Effect

Inactive Publication Date: 2016-12-14
WUXI XINGSHENG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Relevant literature reports that the PBT chain extension and viscosity increase technology is to blend PBT slices and chain extenders in the screw to extend the chain, and does not consider the thermal degradation of the PBT melt in the screw. This method may require more chain extenders. The amount of addition can achieve the effect of increasing the viscosity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh the raw material with terephthalic acid and 1,4-butanediol molar ratio of 1:1.05 and put it into the slurry tank for beating for 1 hour, weigh the catalyst tetrabutyl titanate and dissolve it in 1,4-butanediol to prepare the catalyst Disperse in tank for 1 hour, mix the two kinds of slurries and continue beating for 0.5 hours, prepare the reaction slurry and transport it to the esterification reactor; the esterification temperature is 231°C, the esterification pressure is 22kPa, the esterification residence time is 3.5h, After completion, the esterification product is transported to the pre-condensation reactor, and the esterification rate reaches 99.5% at this time; the pre-condensation temperature is 240°C, the pre-condensation pressure is 3kPa, and the residence time is 0.75h. The prepared prepolymers are sequentially prepolymerized filter and prepolymer cooler for filtration and cooling, and then transported to the final polymerization reactor; the final polyco...

Embodiment 2

[0024]Weigh terephthalic acid and 1,4-butanediol molar ratio of 1:1.2 raw materials into the slurry tank for 1.5h, weigh the catalyst tetrabutyl titanate dissolved in 1,4-butanediol in the catalyst Disperse in the preparation tank for 1.5 hours, mix the two kinds of slurry and continue beating for 1 hour, prepare the reaction slurry and transport it to the esterification reactor; the esterification temperature is 240°C, the esterification pressure is 18kPa, the esterification residence time is 4h, and the esterification After completion, the esterification product is transported to the precondensation reactor, and the esterification rate reaches 99.7% at this time; the precondensation temperature is 245°C, the precondensation pressure is 2kPa, and the residence time is 1h. The filter and the prepolymer cooler are filtered and cooled, and then sent to the final polymerization reactor; the final polycondensation temperature is 260°C, the final polycondensation pressure is 0.05kPa...

Embodiment 3

[0027] Weigh the raw material with a molar ratio of terephthalic acid and 1,4-butanediol of 1:1.15 and put it into the slurry tank for beating for 1.2 hours, weigh the catalyst tetrabutyl titanate and dissolve it in 1,4-butanediol in the catalyst Disperse in the preparation tank for 1 hour, mix the two kinds of slurry and continue beating for 0.5 hours, prepare the reaction slurry and transport it to the esterification reactor; the esterification temperature is 210°C, the esterification pressure is 20kPa, and the esterification residence time is 3.8h. After the esterification is completed, the esterification product is transported to the precondensation reactor, and the esterification rate reaches 99.5% at this time; the precondensation temperature is 250 ° C, the precondensation pressure is 5kPa, and the residence time is 0.85h. The polymer filter and the prepolymer cooler are filtered and cooled before being transported to the final polymerization reactor; the final polyconde...

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Abstract

The invention discloses a preparation method of thermal degradation-resistant PBT polyester with the high viscosity. The preparation method comprises the technology process that the thermal degradation-resistant PBT polyester with the specific viscosity of 1.25-1.35 L / g is finally prepared through slurry preparing, negative-pressure esterification reacting, pre-polycondensation reacting, low-viscosity final polycondensation reacting, chain-extension liquid-phase tackifying reacting and discharging and grain-sized dicing in sequence. According to the preparation method, by adopting lower negative pressure and longer esterification retention time in the esterification stage, the esterification rate of the esterification stage is effectively increased and reaches 99.5% or above, and the terminal carbonyl group content in melt of a consequent reaction is decreased; by controlling the reacting time and the melt viscosity in final polycondensation and adding a carboxyl-terminated chain extender in the liquid-phase tackifying stage, the terminal carbonyl group content in the melt is further decreased, the chain extending and tackifying effects are achieved, the effect of quickly achieving tackifying in short time is achieved, and the production efficiency is improved; the chain extender is stable in property, does not influence the product hue, is high in boiling point and cannot be taken away from a reaction system along with liquid-phase tackifying vacuumizing.

Description

technical field [0001] The invention relates to the technical field of PBT polyester preparation, in particular to a method for preparing high-viscosity heat-resistant and degradable PBT polyester, which adopts low-viscosity melt final polycondensation control technology and high-efficiency and rapid chain extension liquid-phase viscosity-increasing technology. Background technique [0002] Polybutylene terephthalate (PBT) fiber is a new type of fiber developed in the 1980s. Its dyeing performance is better than that of polyester, its elasticity is higher than that of nylon, and it is similar to spandex. The products have high elasticity, high crepe, good hand feeling, strong three-dimensional sense, and high-grade quality with unique style. What is particularly prominent is that the PBT fiber after deformation processing is very elastic, no matter it is under low load or wet conditions. Has a high elastic recovery rate. At the same time, the deformed PBT molecules can show...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C08G63/78C08G63/85
CPCC08G63/6856C08G63/78C08G63/85
Inventor 俞盛马健王华平
Owner WUXI XINGSHENG NEW MATERIAL TECH
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