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A high-efficiency polycondensation reaction device with an external circulation system and its production process for polyester polyols

A technology for polycondensation reaction and reaction device, applied in the field of polymer material synthesis device and process, can solve the problems of increased equipment and investment, increased system viscosity, unfavorable production efficiency, etc., and achieves reduction of device investment and land occupation, easy removal , the effect of increasing the rate of gasification and removal

Active Publication Date: 2021-02-02
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional reaction kettle accelerates the removal of small molecules by strengthening stirring or bubbling with inert gas such as nitrogen, but after the molecular weight of polyester polyol increases in the polycondensation stage, the viscosity of the system increases, the effect of the above method becomes worse and energy consumption increase
In addition, downstream applications require polyester polyol products to be free of air bubbles, and it is extremely time-consuming to remove air bubbles from the high-viscosity system before packaging, which is not conducive to the improvement of production efficiency
CN 102432846, CN201611259907.5 and other patents transfer the polycondensation stage into another tower reactor separately to improve the reaction efficiency of the polycondensation stage, but these devices require additional equipment and investment

Method used

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  • A high-efficiency polycondensation reaction device with an external circulation system and its production process for polyester polyols

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Weigh 285kg of adipic acid and 200kg of 1,4-butanediol and add them to the above-mentioned 500L stainless steel reaction kettle. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 137°C. Start timing since the observation of the rise in the tower top temperature, continuously extract fractions, and control the temperature at the top of the rectifying tower to be 96-98°C. After 2 hours of reaction, the temperature was raised to 180°C at a rate of 45°C / h, and the reaction was continued at 180°C for 2 hours. When the temperature at the top of the tower was observed to drop, use an oil pump to pass through the condenser and evacuate from the upper end of the rectification tower. The system pressure was reduced to 4kPa within the same period, and the temperature was raised to 200°C to continue the reaction for 0.5 hours. The vacuum was turned off and nitrogen was added to equalize the air pressure. The acid value measured by sa...

Embodiment 2

[0064] Weigh 150kg of adipic acid, 114kg of isophthalic acid, 76kg of 1,2-propanediol and 96kg of diethylene glycol into the above-mentioned 500L stainless steel reaction kettle. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 149°C. Start timing since the observation of the rise in the tower top temperature, continuously extract fractions, and control the temperature at the top of the rectifying tower to be 96-98°C. After 2 hours of reaction, the temperature was raised to 230°C at a rate of 60°C / h, and the reaction was continued at 230°C for 2 hours. When the temperature at the top of the tower was observed to drop, an oil pump was used to pass through the condenser and evacuate from the upper end of the rectification tower. The pressure of the system was reduced to 5 kPa, and the reaction was continued at 230° C. for 0.5 hour. The vacuum was turned off and nitrogen was added to equalize the air pressure. Sampling and measuri...

Embodiment 3

[0066] Weigh 250kg of adipic acid, 16.2kg of trimethylolpropane, 36kg of ethylene glycol, and 106kg of diethylene glycol, and add them to the above-mentioned 500L stainless steel reaction kettle. Evacuate and pass nitrogen three times. Under nitrogen protection, the reaction temperature was 130°C. Start counting since the rise of the tower top temperature is observed, and fractions are continuously taken out, and the temperature at the top of the rectifying tower is controlled to be 100-102°C. After reacting for 2 hours, raise the temperature to 210°C at a rate of 110°C / h, and continue to react at 210°C for 2 hours. When the temperature at the top of the tower is observed to drop, use an oil pump to pass through the condenser and evacuate from the upper end of the rectification tower. The system pressure was reduced to 10kPa, nitrogen was bubbled through the nitrogen sparger in the reactor, the nitrogen flow rate was 500L / h, and the reaction was continued for 1 hour. The vac...

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Abstract

The invention relates to a high-efficiency polycondensation reaction device with an external circulation system and a process for producing polyester polyol. The device mainly includes a reactor, a rectification tower, a condenser, and a circulation pump. The upper end of the reactor is connected to the bottom of the rectification tower, and the top of the rectification tower is connected to the condenser. The inlet of the circulation pump is connected to the reactor, and the outlet is connected to the rectification tower. A valve is arranged on the pipeline connecting the top of the rectification column with the condenser. In the esterification stage, the rectification tower plays the role of rectification. In the later stage of polycondensation, the material circulates between the reaction kettle and the rectification tower. The rectification tower acts as an evaporator to efficiently remove water and small molecule alcohols. The reactor can simplify the polycondensation reaction device, save the defoaming process, and significantly improve the production efficiency.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis devices and processes, and in particular relates to a polyester polyol synthesis device and process. Background technique [0002] Polyester polyol is one of the important raw materials for the production of polyurethane. The advantages of polyester polyurethane are high mechanical strength, oil resistance, heat resistance and wear resistance, but poor hydrolysis resistance, low temperature resistance and oxidation resistance. At present, polyester polyurethane is mainly used in the production of polyurethane foam, polyurethane adhesive, thermoplastic polyester elastomer and thermosetting polyurethane elastomer. [0003] Generally, polyester polyol is a linear polymer prepared by polycondensation reaction of dibasic acid and dibasic alcohol. Acids and alcohols react to form esters and water, and this reaction is reversible. The production process is usually divided into two stages: este...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/78C08G63/16C08G63/672
CPCC08G63/16C08G63/672C08G63/785
Inventor 孙双翼鞠昌迅李付国黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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