Method for preparing linear polyester resin

A linear polyester and polyester resin technology, applied in polyester coatings, coatings, etc., can solve the problems of turbidity, large dosage, and low catalytic efficiency of light-colored coatings, and achieve shortened polycondensation time, good product quality, and production costs. low effect

Inactive Publication Date: 2015-04-01
HENGYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, strong acid catalysts, metal oxides or tetrabutyl titanate are mostly used in the preparation of polyesters by polycondensation of dibasic acids and dibasic alcohols. The use of strong acid catalysts is likely to cause darker color of the product and produce many by-products. Using metal oxides The polyester resin prepared as a catalyst is used as an insulating material to affect the insulating properties of the material. When using a single tetrabutyl titanate as a catalyst, the hydrolysis rate of tetrabutyl titanate is fast, and the catalytic efficiency is low. The large amount of it will cause shallow Color paint becomes cloudy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 621kg of ethylene glycol and 90kg of 1,4-butanediol into a 3000L stainless steel reaction kettle, add 1461kg of adipic acid under stirring, pass in nitrogen to replace the air in the reaction kettle for two times, and pass heat transfer oil into the jacket of the reaction kettle to heat When the material reaches 90-110°C, feed a trace amount of nitrogen into the reactor, turn on the vacuum pump, keep warm, and remove the moisture and air in the system. At this stage, control the pressure in the reactor between -0.055—-0.065 Mpa. After 1 hour, Stop the nitrogen flow, raise the temperature to 140°C, and hold the esterification reaction for 0.8-1.2h. During the esterification reaction, in order to reduce the volatilization of ethylene glycol, a 500-800mm diameter and a height of 5-8 meters are installed on the reactor. The reflux tower is equipped with stainless steel corrugated packing, after the water content in the reflux condensate is measured to be less than 1%, th...

Embodiment 2

[0026] Add 621kg of ethylene glycol and 90kg of 1,4-butanediol into a 3000L stainless steel reaction kettle, add 1461kg of adipic acid under stirring, pass in nitrogen to replace the air in the reaction for two times, and pass heat transfer oil into the jacket of the reaction kettle to heat the material To 95-105 ℃, feed a trace amount of nitrogen into the reaction kettle, turn on the vacuum pump, keep warm, and remove the moisture and air in the system. At this stage, control the pressure in the reaction kettle between -0.055—-0.065 Mpa. After 1 hour, stop Ventilate nitrogen, raise the temperature to 140°C, and keep warm for esterification reaction for 0.8-1.2h. In order to reduce the volatilization of ethylene glycol during the esterification reaction, a reflux with a diameter of 500-800mm and a height of 5-8 meters is installed on the reactor. The tower is equipped with stainless steel corrugated packing. After the water content in the reflux condensate is measured to be les...

Embodiment 3

[0028] Add 590g of ethylene glycol and 180kg of 1,4-butanediol into a 3000L stainless steel reaction kettle, add 1461kg of adipic acid under stirring, pass in nitrogen to replace the air in the reaction for two times, and pass heat transfer oil into the jacket of the reaction kettle to heat the material To, 98-102 ℃, feed a trace amount of nitrogen into the reactor, turn on the vacuum pump, keep warm, and remove the moisture and air in the system. At this stage, the pressure in the reactor is controlled between -0.055—-0.065 Mpa. After 1 hour, Stop the nitrogen flow, raise the temperature to 138-142°C, and hold the esterification reaction for 0.9-1.1h. During the esterification reaction, in order to reduce the volatilization of ethylene glycol, a diameter of 500-800mm and a height of 5-8 The reflux tower is equipped with stainless steel corrugated packing. After the water content in the reflux condensate is measured to be less than 1%, 12kg of new catalyst is added, and the tem...

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Abstract

The invention discloses a method for preparing a linear polyester resin. The method is a polymerization process of synthesizing the linear polyester resin from dibasic acid and dihydric alcohol in the presence of a special catalyst. The production process is as follows: adding adipic acid, ethylene glycol and 1,4-butanediol to a reaction still according to the matching ratio to enable the mixed materials to be subjected to an esterification reaction at a temperature of below 140 DEG C; then, increasing the temperate and reacting for several hours at the presence of a new catalyst; removing the water and excess dihydric alcohol generated during the reaction and measuring the acid value and viscosity of the produced material; cooling the material to an indoor temperature when the fact that the reaction is ended is judged and adding a solvent for dilution; packaging the dilute material to obtain the finished product.

Description

technical field [0001] The present invention belongs to polymer polycondensation reaction, particularly relates to a kind of preparation method of linear polyester resin, is a kind of synthetic polyethylene adipate (butylene adipate) by adipic acid, ethylene glycol, butanediol under the catalysis of catalyst diester). Background technique [0002] The consumption of polyester resin in China is growing at an annual rate of about 20%. The total amount of domestic polyester resin is about 10 million tons, and about 1.3 million tons are imported for supplementary use. Among them, the amount of linear polyester resin for coatings is about 8,000 tons, all of which rely on imports. [0003] Polyester for coatings generally does not form a film alone, and is mainly used to prepare polyester-amino baking varnish, polyester-polyurethane paint, polyester powder coating and unsaturated polyester paint, all of which belong to medium and high-grade coating systems. High gloss, good full...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/85C09D167/02
Inventor 李薇
Owner HENGYANG NORMAL UNIV
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