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Homogeneous hyper-viscous polyester and preparation method thereof

A technology of viscous polyester and intrinsic viscosity, applied in the field of homogeneous high-viscosity polyester and its preparation, can solve the problems of high oligomer content and insufficient homogenization, achieve narrow molecular weight distribution width, reduce probability, avoid low The effect of increased polymer content

Pending Publication Date: 2019-01-04
ZHEJIANG UNIFULL IND FIBER +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a homogeneous high-viscosity polyester that can effectively reduce the content of oligomers in the polyester in order to overcome the problems of high oligomer content and insufficient homogenization of the high-viscosity polyester prepared in the prior art and its preparation method

Method used

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  • Homogeneous hyper-viscous polyester and preparation method thereof
  • Homogeneous hyper-viscous polyester and preparation method thereof
  • Homogeneous hyper-viscous polyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The preparation method of homogeneous high viscosity polyester, concrete steps are as follows:

[0052] (1) prepare low-viscosity polyester;

[0053] (1.1) Modulation of ethylene glycol antimony;

[0054]Ethylene glycol antimony and ethylene glycol are mixed uniformly in the catalyst preparation tank 1, and nitrogen gas with a water content of 155ppm is circulated in the mixing process; the catalyst configuration system diagram is as follows figure 2 As shown, the catalyst configuration system includes a catalyst preparation tank 1 and a catalyst supply tank 4. The inside of the catalyst preparation tank 1 is provided with an agitator, and the top and bottom are respectively connected with the outlet of the nitrogen treatment generator 2 and the gas circulation pump 3. 2 is used to generate nitrogen and dry nitrogen at the same time. The nitrogen treatment generator 2 is connected to the inlet of the gas circulation pump 3; after the modulation process is completed, e...

Embodiment 2

[0066] The preparation method of homogeneous high viscosity polyester, concrete steps are as follows:

[0067] (1) prepare low-viscosity polyester;

[0068] (1.1) Modulation of ethylene glycol antimony;

[0069] Antimony ethylene glycol and ethylene glycol are mixed evenly in the catalyst preparation tank, wherein, in the mixing process, helium with a water content of 190ppm is circulated, and the configuration system of the catalyst is basically the same as that of Example 1, except that The device used to generate gas while drying the gas is a helium gas treatment generator;

[0070] (1.2) Carry out esterification reaction and polycondensation reaction between terephthalic acid and ethylene glycol with a molar ratio of 1:1.3, add ethylene glycol antimony when the average degree of polymerization of the intermediate product of the polycondensation reaction reaches 8, and finally obtain low Viscous PET, wherein the temperature of the esterification reaction is 238°C, the tim...

Embodiment 3

[0077] The preparation method of homogeneous high viscosity polyester, concrete steps are as follows:

[0078] (1) prepare low-viscosity polyester;

[0079] (1.1) Modulation of ethylene glycol antimony;

[0080] Ethylene glycol antimony and ethylene glycol are mixed evenly in the catalyst preparation tank, wherein, in the mixing process, the neon gas with a water content of 185ppm is circulated, and the configuration system of the catalyst is basically the same as that of Example 1, the difference is that The device used to generate gas while drying the gas is a neon gas treatment generator;

[0081] (1.2) Carry out esterification reaction and polycondensation reaction between terephthalic acid and ethylene glycol with a molar ratio of 1:1.4, add ethylene glycol antimony when the average degree of polymerization of the intermediate product of the polycondensation reaction reaches 13, and finally obtain low Viscous PET, wherein the temperature of the esterification reaction i...

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Abstract

The invention relates to homogeneous hyper-viscous polyester and a preparation method thereof. The method comprises the following steps of: controlling the mechanism of adding a catalyst during a synthesis process to obtain low-viscous polyester with an intrinsic viscosity of 0.300-0.500 dL / g, and then performing solid phase thickening on the low-viscous polyester to obtain the homogeneous hyper-viscous polyester with an intrinsic viscosity of 0.85-1. 15dL / g, an intrinsic viscosity deviation less than or equal to 0.02dL / g and a molecular weight distribution index of 2.5, wherein the catalyst is added when the average polymerization degree of an intermediate product in a polymerization reaction reaches 8-17; the pre-reaction of the solid-phase thickening is divided into four stages which are a first stage, a second stage, a third stage, and a fourth stage, the corresponding temperatures are 190-195 DEG C,195-210 DEG C, 210-220 DEG C and 220-230 DEG C respectively. The preparation methodof the homogeneous hyper-viscous polyester obviously reduces the content of oligomer in a product, and the prepared polyester has high quality and excellent popularization value.

Description

technical field [0001] The invention belongs to the field of polyester preparation, and relates to a homogeneous high-viscosity polyester and a preparation method thereof. Background technique [0002] High-viscosity polyester has good mechanical properties and excellent physical and chemical properties, and is widely used in industrial fields such as industrial yarns, packaging materials, and engineering plastics, especially in industrial fields that require composite reinforcement materials such as automobiles, safety protection, and ropes. [0003] At present, the common preparation method of high-viscosity polyester is: first prepare low-viscosity polyester with an intrinsic viscosity of about 0.65 dL / g through melt polycondensation, and then prepare tackified polyester through solid-state polycondensation to increase viscosity. The solid state polycondensation process of polyester (solid state polycondensation (SSP) refers to the condensation reaction of the reaction ma...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/86C08G63/183
CPCC08G63/183C08G63/78C08G63/866
Inventor 姬洪张玉梅宋明根蒋权徐龙官陈康邹家熊甘宇
Owner ZHEJIANG UNIFULL IND FIBER
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