Continuous preparation method of polyester polyol

A polyester polyol and polyol technology, which is applied in the field of organic polymer compounds and their preparation, can solve the problems of poor stability of production process and product indicators, difficulty in weighing and adding catalysts, and inability to sufficiently remove moisture. , to achieve the effect of product quality stability assurance, production time saving and loss reduction

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

The existing process cannot sufficiently 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 to effectively catalyze the reaction.
On the other hand, 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
This leads to the fact that the amount of catalyst actually used in industrial production is still relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Mix adipic acid and 1,4-butanediol evenly in a slurry tank at a mass ratio of 1.45:1. Under continuous and stable conditions, add about 0.75kg of the mixture to a 5L esterification tank per hour. The esterification tank Maintain normal pressure, the reaction temperature is about 180°C, the temperature at the top of the tower is controlled at 96-100°C, and the material in the kettle is 1.5L. The water extraction rate is 0.098kg / h, and the equivalent esterification rate is 90%. The bottom material of the esterification tank is continuously introduced into the 10L flash tank. The reaction in the 10L flash tank maintains a pressure of 18kPa and a temperature of about 200°C. After stabilization, the volume of the material in the tank is about 1L, and the acid value is about 12mgKOH / g. The bottom material of the flash tank is continuously introduced into a 10L polycondensation tank, and 16ppm of isopropyl titanate catalyst (0.012g / h) is added to maintain the reaction tempera...

Embodiment 2

[0049] Mix adipic acid, neopentyl glycol, and 1,6-hexanediol in a slurry tank at a mass ratio of 1:0.246:0.682. Under continuous and stable conditions, add about 0.75kg of the mixture into the 5L esterification tank per hour. The esterification tank maintains normal pressure, the reaction temperature is about 230°C, the temperature at the top of the tower is controlled at 98-100°C, and the volume of the material in the tank is about 2.3L. . The water extraction rate is 0.077kg / h, and the equivalent esterification rate is 80%. After being preheated to 230°C, the bottom material of the esterification tank was continuously introduced into a 10L flash tank. The reaction in the 10L flash tank maintained a pressure of 10kPa, and the reaction temperature was about 230-245°C. After stabilization, the volume of the material in the tank was 1.5L, and the acid value was 18mgKOH / g. The bottom material of the flash tank was continuously introduced into a 10L polycondensation tank, and a ...

Embodiment 3

[0051] Mix dodecanedioic acid and 1,6-hexanediol in a slurry tank at a mass ratio of 1:0.565. Under continuous and stable conditions, add about 0.75kg of the mixture to the 5L esterification tank per hour. The esterification tank maintains normal pressure, the reaction temperature is 200 ° C, the temperature at the top of the tower is controlled at 98-100 ° C, and the volume of the material in the tank is about 1.5 L. The water extraction rate is 0.071kg / h, and the equivalent esterification rate is 95%. The bottom material of the esterification tank is continuously introduced into the 10L flash tank. The reaction in the 10L flash tank was maintained at a pressure of 10kPa, and the reaction temperature was about 200-215°C. After stabilization, the volume of the material in the tank was 1.5L, and the acid value was 5.6mgKOH / g. The bottom material of the flash tank was continuously introduced into a 10L polycondensation tank, and a 1:10 mixture of isopropyl titanate and poly(1,6...

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Abstract

The invention relates to a continuous preparation method of polyester polyol. The method comprises three reaction stages including esterification, flash evaporation and polycondensation. The esterification reaction is performed at 130-260 DEG C, preferably, 180-240 DEG C and more preferably, 200-230 DEG C, the esterification rate is about 50%-95%, and the loss of raw material polyhydric alcohols can be reduced when the esterification reaction is performed at the higher temperature. Small molecules such as water and the like can be removed efficiently and quickly through flash evaporation, thereaction speed can be increased, the production time can be saved, and energy consumption can be reduced. A mixture of a catalyst and 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 and stable product quality.

Description

technical field [0001] The invention belongs to the field of organic macromolecular compounds and preparation thereof, and in particular relates to a continuous preparation method of polyester polyol, more specifically, to a synthesis process of polyester polyol 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, polyure...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/16
CPCC08G63/16C08G63/78
Inventor 孙双翼鞠昌迅黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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