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A kind of preparation method of high-quality polyester polyol

A polyester polyol, high-quality technology, applied in the field of preparation of high-quality polyester polyol, can solve the problems of product scrap, gel, influence, etc., and achieve the effect of stable moisture content and improved yield

Active Publication Date: 2019-04-16
JIANGSU HUADA NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molecular weight distribution of the product has a great influence on the physical properties of downstream products; the size of the hydroxyl value range affects the formulation stability of the downstream market during product use and thus affects the mechanical properties of the product; the level of chroma has a great impact on downstream products The appearance of the product has an intuitive impact; for the polyurethane reaction system, water can react with isocyanate, so the level of water content will seriously affect the ratio of NCO / OH in the starting material of the downstream formulation, and more side reactions will occur to produce gel etc. leading to product scrapping

Method used

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  • A kind of preparation method of high-quality polyester polyol

Examples

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preparation example Construction

[0011] The preparation method of high-quality polyester polyol of the present invention, it comprises the following steps: (a) add dibasic carboxylic acid and dibasic alcohol in the reactor with rectification column, gradually heat up to 180~200 ℃ under inert gas atmosphere ℃ for esterification and dehydration reaction, and control the temperature at the top of the rectification tower to be 90-110 ℃; (b) add catalyst to the reaction kettle, raise the temperature to 220-250 ℃ at a speed of 5-10 ℃ / 30min, and The polycondensation reaction can be carried out under reduced pressure; the reduced pressure condition is to increase from 0.01MPa to 0.1MPa at a gradient speed of 0.005 to 0.015MPa and keep it for 0.5 to 1 hour after each increase. The quality of the catalyst is as follows: 0.005% to 0.05% of the total mass of dibasic carboxylic acid and glycol. On the one hand, precise control of the temperature at the top of the distillation column can prevent the loss of small molecule ...

Embodiment 1

[0015] The present embodiment provides a kind of preparation method of high-quality polyester polyol, and it comprises the following steps:

[0016] (a) add 146.0kg adipic acid (10.0mol) and 713.0kg ethylene glycol (11.0mol) in the reactor with rectifying tower, heat reaction mixture under nitrogen protection, and control the temperature at the top of rectifying tower The temperature is 95℃~100℃, the specific heating process is: raise the temperature to 130-135℃ at a speed of 5℃ / 30min, keep it for 1.5 hours, continue to heat up to 150-160℃, keep it for 0.5 hours, then raise the temperature to 180℃, keep it for 0.5 hours Hours; continue to heat up to 220-230 ° C constant temperature 2-3 hours.

[0017] (b) Add 0.027kg of catalyst (tetrabutyl titanate) to the reactor with carrier gas, and then keep it at 220°C for 4 hours; carry out polycondensation reaction under reduced pressure, specifically: keep at 0.01Mpa for 0.4h, 0.02Mpa for 0.4h, 0.03Mpa for 0.4h, 0.04Mpa for 0.4h, 0.0...

Embodiment 2

[0019] This example provides a method for preparing high-quality polyester polyol, the preparation process of which is basically the same as that in Example 1, except that the temperature at the top of the rectification tower is controlled at 90-95°C.

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Abstract

The invention relates to a preparation method for high-quality polyester polyol. The method comprises the following steps: (a) adding dicarboxylic acid and dihydric alcohol into a reaction kettle with a rectifying tower and a mechanical stirrer, gradually increasing the temperature to 180-200 DEG C under an inert gas atmosphere, performing esterifying dehydration reaction and controlling the temperature at the top of the rectifying tower at 95-110 DEG C; (b) adding a catalyst into the reaction kettle, increasing the temperature to 220-250 DEG C at the rate of 5-10 DEG C / 30 min, and then performing condensation polymerization under a decompression condition. The decompression condition is that the pressure is gradually increased from 0.01MPa to 0.1MPa at the rate of 0.005-0.015MPa and the pressure is kept for 0.5-1 hour after the gradual increasing at each time and the weight of the catalyst is 0.005-0.05% of the total weight of dicarboxylic acid and dihydric alcohol, so that the stability of molecular weight distribution, hydroxyl value, acid value and chromatic number of the product and the system technique can be guaranteed.

Description

technical field [0001] The invention relates to a preparation method of polyol, in particular to a preparation method of high-quality polyester polyol. Background technique [0002] The main molecular chain of polyester polyol is composed of alkyd ester groups, and the terminal group is hydroxyl group, which can be used as the base material of surfactant or polyurethane material. Polyurethane materials prepared from polyester polyols have high strength, excellent wear resistance, oil resistance, weather resistance and hydrolysis resistance, and also have good biodegradability, and can be used to produce polyurethane elastomers, coatings , adhesives, foam materials, etc., so polyester polyol, as a new type of high-performance polyurethane raw material, has been widely welcomed by manufacturers. The classic production method of polyester polyol is formed by condensation of dibasic acid (anhydride) and dibasic alcohol (polyol). The control of its production process is very imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/16C08G63/85
CPCC08G63/16C08G63/85
Inventor 訾少宝李吉成王晓敏邹晓菲陈伟王玄阳刘少勇
Owner JIANGSU HUADA NEW MATERIAL CO LTD
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