A kind of polycarbonate polyol and its synthesis method and application

A synthesis method, polycarbonate technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve economic disadvantages and other problems

Active Publication Date: 2020-07-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method cannot be realized under normal pressure reaction, and pressurization leads to additional investment in equipment and safety measures, which is economically unfavorable

Method used

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  • A kind of polycarbonate polyol and its synthesis method and application
  • A kind of polycarbonate polyol and its synthesis method and application
  • A kind of polycarbonate polyol and its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] In this embodiment, the preset value of the mass percentage of carbonate contained in the rectification fraction is 32%.

[0070] Weigh 1574g of 1,5-pentanediol and 0.1574g of isopropyl titanate into a glass reaction kettle equipped with an oil bath jacket, a stirrer, a gas inlet, and a rectification column. Vacuumize and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was raised to a reaction temperature of 165° C., and 1700 g (the total amount of carbonate feeds predetermined by stoichiometry) of dimethyl carbonate was slowly added dropwise into the system. Since the temperature rise at the top of the column was observed, distillates were withdrawn continuously at a reflux ratio of 2:1-1:1. During the continuous feeding process of dimethyl carbonate, the adjustment of the reflux ratio is carried out according to the following table 1, to maintain the absolute value of the difference between the mass percentage ...

Embodiment 2

[0078] In this embodiment, the preset value of the mass percentage of carbonate contained in the rectification fraction is 32%.

[0079] Weigh 16261g of 1,5-pentanediol, 18450g of 1,6-hexanediol, and 3.45g of tetrabutyl titanate, and add them to a stainless steel reaction kettle equipped with an oil bath jacket, a stirrer, a gas inlet, and a rectification column middle. Vacuumize and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was raised to a reaction temperature of 156° C., and 35.0 kg (the total amount of carbonate feeds predetermined by stoichiometry) of dimethyl carbonate was slowly added dropwise into the system. Since the temperature rise at the top of the column was observed, fractions were continuously withdrawn at a reflux ratio of 2:1. During the continuous feeding process of dimethyl carbonate, take samples online and record the total fraction mass when sampling, subtract the total fraction mass recorded...

Embodiment 3

[0087] In this embodiment, the preset value of the mass percentage of carbonate contained in the rectification fraction is 32.0%.

[0088] Weigh 494.2 g of neopentyl glycol, 560.7 g of 1,6-hexanediol, and 0.0988 g of isopropyl titanate, and add them into a glass reactor equipped with an oil bath jacket, a stirrer, a gas inlet, and a rectification column. Vacuumize and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was raised to a reaction temperature of 115° C., and 1000 g of dimethyl carbonate (the total amount of carbonate feed in the stoichiometric predetermined amount) was slowly added dropwise into the system. Since the temperature rise at the top of the tower was observed, fractions were continuously withdrawn at a reflux ratio of 1.7:1, and the ratio of methanol:DMC in the fractions fluctuated in the range of 66.1:33.9-66.5:33.5wt%. Since the dimethyl carbonate content in the cuts was monitored to be higher than...

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Abstract

The invention provides a polycarbonate polyol and its synthesis method and application. The synthesis method comprises the following steps: carrying out transesterification reaction between a raw material A containing a polyol or a mixture of a polyol and a lactone and a carbonate to generate the polycarbonate polyol. Carbonate polyol, the raw material A is fed at one time, and the carbonate of the stoichiometrically predetermined total amount of carbonate feed is put into the reaction system by continuous feeding, and the by-products and carbonate are rectified during the reaction. Azeotrope; Sampling and monitoring the mass percentage of carbonate in the fraction during the completion of the stoichiometrically predetermined carbonate feed total amount, controlling the stability of the carbonate content in the fraction composition and / or according to the The content of carbonate is changed to add or reduce carbonate. The method provided by the invention can quickly and stably produce products meeting the requirements of hydroxyl value, and the post-treatment is simpler.

Description

technical field [0001] The invention relates to the technical field of preparation of polycarbonate polyols, in particular to a semi-continuous synthesis method capable of efficiently preparing polycarbonate polyols. Background technique [0002] Polycarbonate polyol is one of the important raw materials for the production of polyurethane. For example, as the soft chain end of polyurethane elastomer, it has excellent properties such as hydrolysis resistance, heat resistance, oil resistance, and aging resistance. Polycarbonate polyols are usually made of small molecule polyols or small molecule alcohols and lactones, and small molecule carbonates are transesterified under a catalyst to generate polycarbonate polyols and small molecule byproducts, by removing small molecule byproducts And promote the reaction to proceed thoroughly, and then obtain the product. [0003] The most important polycarbonate polyol products are homopolymerized or copolymerized polycarbonate diols m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/30C08G18/44
CPCC08G18/44C08G64/30C08G64/305C08G63/64C08G65/2603C08L75/06C09D175/06
Inventor 孙双翼鞠昌迅刘斌赵晶黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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