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Preparation method of polyester polyol

A technology of polyester polyols and polyols, applied in the field of organic high-fraction compounds and their preparation, can solve problems such as less catalysts, deactivation, production process and product index stability deterioration, etc., and achieve low catalyst residues and high product quality stable effect

Active Publication Date: 2018-05-04
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One of the reasons is that metal-organic catalysts are easily deactivated by hydrolysis, and the existing process cannot fully remove the residual moisture in the system. If only a small amount of catalyst is added, there will be too little catalyst remaining after hydrolysis, and the low-catalysis reaction cannot be effectively carried out.
The second reason is that the reduction of the amount of catalyst brings great difficulties to accurately weigh and add the catalyst, which makes the production process and the stability of product indicators worse.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Weigh 2.8694kg of adipic acid and 1.9803kg of 1,4-butanediol into a 5L glass reactor equipped with an oil bath jacket, a stirrer, a gas inlet, and a rectification column. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 137°C. Start timing since the observation of the temperature rise at the top of the tower, continuously extract fractions, and control the temperature at the top of the rectifying column to be 96-98°C. After 2 hours of reaction, the temperature was raised to 180°C at a rate of 90°C / h, and the reaction was continued at 180°C for 2 hours, and the temperature at the top of the tower was observed to drop. Use an oil pump to reduce the system pressure to below 1kPa, and raise the temperature to 200°C to continue the reaction for 2 hours. The vacuum was turned off and nitrogen was added to equalize the air pressure. Sampling and measuring acid value 12.37mgKOH / g. Add 1113 mg of a mixture of isopropyl titanate ...

Embodiment 2

[0047] Weigh 2.7639kg of adipic acid and 1.9038kg of 1,4-butanediol into a 5L glass reactor equipped with an oil bath jacket, stirrer, gas inlet, and rectification column. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 138°C. Start counting since the temperature rise at the top of the tower was observed, and fractions were continuously extracted, and the temperature at the top of the rectification column was controlled to be 98-100°C. After 2 hours of reaction, the temperature was raised to 220°C at 80°C / h, and the reaction was continued at 220°C for 2 hours, and the temperature at the top of the tower was observed to drop. Use an oil pump to reduce the system pressure to below 1kPa, and continue the reaction at 220°C for 2 hours. The vacuum was turned off and nitrogen was added to equalize the air pressure. Sampling and measuring acid value 12.27mgKOH / g. Add 1206mg of a mixture of pre-prepared isopropyl titanate and polyadi...

Embodiment 3

[0049] Weigh 2.018kg of adipic acid, 0.496kg of neopentyl glycol, and 1.376kg of 1,6-hexanediol into a 5L glass reactor equipped with an oil bath jacket, a stirrer, a gas inlet, and a rectification column. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 138°C. Start timing since the temperature rise at the top of the tower was observed, and fractions were continuously extracted, and the temperature at the top of the rectification column was controlled to be 96-100°C. After 2 hours of reaction, the temperature was raised to 200°C at 80°C / h, and the reaction was continued at 200°C for 2 hours, and the temperature at the top of the tower was observed to drop. Use an oil pump to reduce the system pressure to below 1kPa, and continue the reaction at 200°C for 2.25 hours. The vacuum was turned off and nitrogen was added to equalize the air pressure. Sampling and measuring acid value 7.3671mgKOH / g. Add 542.0 mg of a mixture of isopr...

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PUM

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Abstract

The invention discloses a preparation method of polyester polyol. The reaction comprises four steps as follows: (1) polybasic acid (anhydride) and polyhydric alcohol react at 120-150 DEG C and under normal pressure, and water produced during the reaction is extracted through rectification; (2) the reaction temperature is increased linearly, and the reaction and extraction of the byproduct water are further promoted; (3) the pressure of the reaction system is reduced slowly and the water content of the system is further reduced; (4) a small quantity of mixture of a catalyst and a polyester polyol product is added, the reaction is continued in a high-temperature and vacuum environment until the product index is qualified, and the product index is adjusted when necessary. The mixture of the catalyst and the polyester polyol is fed, catalyst hydrolysis can be effectively reduced in thermodynamics and kinetics in a ligand change manner, and the dosage of the catalyst can be reduced. The polyester polyol produced with the technology has the advantages of low catalyst residues, low color number, low acid value and stable product quality.

Description

technical field [0001] The invention belongs to the field of organic high-fraction compounds and their preparation, and specifically relates to a synthesis process of polyester polyols, more specifically, to a synthesis process of polyester polyols with low catalyst residue. Background technique [0002] Polyester polyol is one of the important raw materials for producing polyurethane. The production of polyurethane requires black and white materials. The main component of white material is polyol, which can be divided into polyester polyol and polyether polyol. The advantages of polyester polyurethane are high mechanical strength, oil resistance, heat resistance, wear resistance, but hydrolysis resistance, low temperature resistance and oxidation resistance, and the stability to acid and alkali is not as good as polyether polyurethane. At present, polyester polyurethane is mainly used in the production of polyurethane resin, polyurethane sole liquid, polyurethane rigid fo...

Claims

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Application Information

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IPC IPC(8): C08G63/16C08G63/20C08G63/85C08G63/78
CPCC08G63/16C08G63/20C08G63/78C08G63/85
Inventor 孙双翼鞠昌迅黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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