Polycarbonate polyol, and synthetic method and application thereof

A synthesis method, polycarbonate technology, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve problems such as economic disadvantage

Active Publication Date: 2019-07-02
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method cannot be realized under normal pressure reaction, and pressurization lea

Method used

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  • Polycarbonate polyol, and synthetic method and application thereof
  • Polycarbonate polyol, and synthetic method and application thereof
  • Polycarbonate polyol, and synthetic method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

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

[0070] Weigh 1574 g of 1,5-pentanediol and 0.1574 g of isopropyl titanate and add them to a glass reactor equipped with an oil bath jacket, agitator, gas inlet, and rectification column. Vacuum 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 feed in stoichiometric amount) of dimethyl carbonate was slowly added dropwise to the system. Since the temperature at the top of the tower was observed to rise, fractions were continuously extracted with a reflux ratio of 2:1-1:1. During the continuous feeding process of dimethyl carbonate, adjust the reflux ratio according to the following table 1 to maintain the absolute value of the difference between the mass percentage of carbonate contained in the rectified frac...

Embodiment 2

[0078] In this embodiment, the preset value of the mass percentage of carbonate contained in the rectified 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 reactor equipped with an oil bath jacket, agitator, gas inlet, and rectification column in. Vacuum and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was increased to 156° C., and 35.0 kg (the total amount of carbonate feed in stoichiometry) of dimethyl carbonate was slowly added dropwise to the system. Since the temperature at the top of the tower was observed to rise, distillates were continuously extracted with a reflux ratio of 2:1. During the continuous feeding process of dimethyl carbonate, take online sampling and record the mass of the total fraction at the time of sampling, and subtract the mass of the total fraction recorded during the previous sampling in t...

Embodiment 3

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

[0088] Weigh 494.2 g of neopentyl glycol, 560.7 of 1,6-hexanediol, and 0.0988 g of isopropyl titanate, and add them to a glass reactor equipped with an oil bath jacket, agitator, gas inlet, and rectification column. Vacuum and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was increased to 115° C., and 1000 g of dimethyl carbonate (the total amount of carbonate feed in stoichiometric amount) was slowly added dropwise to the system. Since the temperature rise at the top of the tower was observed, fractions were continuously extracted with a reflux ratio of 1.7:1, and the methanol:DMC ratio in the fraction fluctuated in the range of 66.1:33.9-66.5:33.5wt%. As the content of dimethyl carbonate in the fraction was monitored during the reaction to be higher than the preset value (see Table 3), 16.8 g ...

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Abstract

The invention provides a polycarbonate polyol, and a synthetic method and application thereof. The synthetic method comprises the following step that an ester exchange reaction is carried out on a rawmaterial A containing a mixture of polyhydric alcohol or polyol and lactone with carbonic ester to generate the polycarbonate polyol, wherein the raw material A is fed at one time, the carbonic esterwith a preset stoichiometric amount is fed into the reaction system in a continuous feeding manner, and an azeotrope of by-products and the carbonic ester is rectified in the reaction process. The mass percent of the carbonic ester in a fraction is sampled and monitored in the feeding process of the carbonic ester with the preset total stoichiometric amount, stability of the content of the carbonic ester in the composition of the extracted fraction is controlled, and/or the carbonic ester is supplemented or slightly added according to the change of the content of the carbonic ester in the fraction. The method provided by the invention can be used to rapidly and stably produce a product meeting the hydroxyl value requirement, 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 hydrolysis resistance, heat resistance, oil resistance, and aging resistance. Polycarbonate polyols usually consist of small molecular polyols or small molecular alcohols and lactones, and small molecular carbonates undergo transesterification under a catalyst to generate polycarbonate polyols and small molecular by-products, by removing small molecular by-products And push the reaction to proceed thoroughly, and then obtain the product. [0003] The most important polycarbonate polyol product is a homopolymerized or copolymerized polycarbonate diol with 1,6-hexanedi...

Claims

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Application Information

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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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