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Phthalic anhydride polyester polyol with narrow molecular weight distribution, and preparation method thereof

A technology of phthalic anhydride polyester polyol and phthalic anhydride, applied in the field of polyester polyol, can solve the problems of wide molecular weight distribution, alkyd deviation, high loss, etc., and achieve the effects of narrow molecular weight distribution, excellent flame retardant performance, and low feed ratio

Active Publication Date: 2020-05-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above synthesis method, the small molecular alcohol cannot fully participate in the reaction, and the loss is more at high temperature.
The loss of small molecule alcohol causes the alkyd ratio in the system to deviate from the design value quickly, resulting in a wider molecular weight distribution and an increase in the cost of synthesizing polyols

Method used

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  • Phthalic anhydride polyester polyol with narrow molecular weight distribution, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 10.0kg (67.6mol) of phthalic anhydride and 9.3kg (87.9mol) of ethylene glycol were successively added into a 25L reactor, and the molar ratio of alkyd to acid was 1.3:1. Under the condition of nitrogen protection, raise the temperature of the system to 160°C, and react at this temperature for 0.5h; raise the temperature of the system to 200°C within 1h, and react at this temperature for 1h; raise the temperature of the system within 1h Rise to 230°C, and monitor the acid value and hydroxyl value. When the acid value is lower than 20mgKOH / g, turn on the vacuum system, and the vacuum degree will slowly drop to -0.09MPa within 0.5h to remove the moisture and small molecule alcohol in the system. When the acid value is less than 2mgKOH / g and the hydroxyl value is 108-112mgKOH / g, the vacuum is stopped and the material is discharged. The obtained product is denoted as phthalic anhydride polyester polyol A.

[0028] Product index: acid value 0.8mgKOH / g, hydroxyl value 110.8mg...

Embodiment 2

[0030] 10.0kg (67.6mol) of phthalic anhydride and 9.3kg (87.9mol) of ethylene glycol were successively added into a 25L reactor, and the molar ratio of alkyd to acid was 1.3:1. Under the condition of nitrogen protection, raise the temperature of the system to 170°C, and react at this temperature for 0.5h; raise the temperature of the system to 210°C within 1h, and react at this temperature for 1h; raise the temperature of the system within 1h Raise to 230°C, and monitor the acid value and hydroxyl value, and turn on the vacuum system when the acid value is lower than 20mgKOH / g, and the vacuum degree will slowly drop to -0.09MPa within 0.5h, and remove the moisture and small molecule alcohol in the system. When the acid value is less than 2mgKOH / g and the hydroxyl value is 108-112mgKOH / g, the vacuum is stopped and the material is discharged. The obtained product is denoted as phthalic anhydride polyester polyol B.

[0031] Product index: acid value 0.6mgKOH / g, hydroxyl value 1...

Embodiment 3

[0033] 10.0kg (67.6mol) of phthalic anhydride and 9.3kg (87.9mol) of ethylene glycol were successively added into a 25L reactor, and the molar ratio of alkyd to acid was 1.3:1. Under the condition of nitrogen protection, the temperature of the system is raised to 160°C, and the temperature is kept at this temperature for 1 hour; the temperature of the system is raised to 200°C within 1 hour, and the temperature is kept at this temperature for 2 hours; to 230°C, and monitor the acid value and hydroxyl value, turn on the vacuum system when the acid value is lower than 20mgKOH / g, and slowly reduce the vacuum degree to -0.09MPa within 0.5h, remove the moisture and small molecule alcohol in the system, to When the acid value is less than 2mgKOH / g and the hydroxyl value is 108-112mgKOH / g, the vacuum is stopped and the material is discharged. The resulting product is denoted as phthalic anhydride polyester polyol C.

[0034] Product index: acid value 0.6mgKOH / g, hydroxyl value 110.2...

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Abstract

The invention provides a phthalic anhydride polyester polyol and a preparation method thereof. The phthalic anhydride polyester polyol is synthesized by adopting a conventional polyester polyol device, the alkyd feeding ratio is low, the synthesis process comprises three stages, and the molecular weight distribution of the obtained phthalic anhydride polyester polyol is narrow.

Description

technical field [0001] The invention relates to the field of polyester polyols, in particular to phthalic anhydride polyester polyols with narrow molecular weight distribution and a preparation method thereof. Background technique [0002] Phthalic anhydride polyester polyol is an intermediate widely used in the field of rigid foam, which can partially replace polyether polyol. The existence of benzene ring in its structure can endow rigid foam with good flame retardancy, and has the characteristics that polyether polyol is difficult to Competitive advantage. In addition, phthalic anhydride polyester polyols are also widely used in the fields of coatings, elastomers, adhesives and sealants. [0003] The industrial production methods of polyester polyol mainly include vacuum melt polycondensation method and carrier gas melt polycondensation method, and the synthesis of phthalic anhydride polyester polyol mostly adopts vacuum melt polycondensation method. For example, patent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/668C08G63/181
CPCC08G63/668C08G63/181
Inventor 张存玉孙令民黄岐善
Owner WANHUA CHEM GRP CO LTD
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