Method for preparing polyester polyol/nano-hydrotalcite by in-situ polymerization

A technology of polyester polyol and nano-hydrotalcite, which is applied in the field of polyurethane raw materials, can solve the problems of long reaction time and limited reaction temperature, and achieve the effects of saving reaction time, increasing reaction temperature and improving intercalation effect

Inactive Publication Date: 2018-02-09
SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing polyester polyol / nanometer hydrotalcite by in-situ polymerization, so as to solve the problems of long reaction time and limited reaction temperature in the existing hydrotalcite intercalation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0017] Add hydrotalcite compounds, small molecular polyols, and organic dibasic acids into the reactor, introduce nitrogen to remove the air in the system, raise the temperature to 120-140°C, and react for 5 hours to complete the reaction of organic dibasic acids on hydrotalcites. compound intercalation. Then start to heat up and dehydrate until the system temperature is 180°C, continue to heat up to 220°C, measure the acid value, and start vacuuming until the acid value drops below 1mgKOH / g.

[0018] 1) Intercalation of dibasic acids on hydrotalcite compounds

[0019] First add 1 part of hydrotalcite compound, 24 parts of ethylene glycol and 20 parts of adipic acid. Nitrogen gas was introduced to remove the air in the system, the temperature was raised to 120° C., and the reaction was carried out for 5 hours to complete the intercalation of the organic dibasic acid to the hydrotalcite compound.

[0020] 2) Preparation of polyester polyol / nano hydrotalcite

[0021] Continue...

Embodiment example 2

[0024] 1) Intercalation of dibasic acids on hydrotalcite compounds

[0025] First add 1 part of hydrotalcite compound, 40 parts of 1,4-butanediol and 30 parts of terephthalic acid. Nitrogen gas was introduced to remove the air in the system, the temperature was raised to 140° C., and the reaction was carried out for 5 hours to complete the intercalation of terephthalic acid to the hydrotalcite compound.

[0026] 2) Preparation of polyester polyol / nano hydrotalcite

[0027] Continue to heat up the terephthalic acid / hydrotalcite intercalate prepared in the previous step to remove the moisture generated during the reaction, gradually raise the temperature to 180 °C, measure the acid value to 35 mgKOH / g, and vacuum until the system acid value drops to 1.0 mgKOH / g or less, polyester polyol / nano hydrotalcite is obtained after breaking the vacuum.

[0028] Its hydroxyl value is determined to be: 65 mgKOH / g, and the acid value is 0.76 mgKOH / g.

Embodiment example 3

[0030] 1) Intercalation of dibasic acids on hydrotalcite compounds

[0031] First add 1 part of hydrotalcite compound, 30 parts of ethylene glycol, 30 parts of ethylene glycol, 25 parts of maleic acid and 30 parts of phthalic acid. Nitrogen gas was introduced to remove the air in the system, the temperature was raised to 130° C., and the reaction was carried out for 5 hours to complete the intercalation of maleic acid and phthalic acid to hydrotalcite compounds.

[0032] 2) Preparation of polyester polyol / nano hydrotalcite

[0033] Continue to raise the temperature of the hydrotalcite intercalate prepared in the previous step to remove the moisture generated during the reaction, gradually raise the temperature to 180 °C, measure the acid value to 34 mgKOH / g, and vacuum until the system acid value drops below 1.0 mgKOH / g. The polyester polyol / nanometer hydrotalcite is obtained after breaking the vacuum.

[0034] Its hydroxyl value was determined to be 41 mgKOH / g, and the acid...

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Abstract

The invention provides a method for preparing polyester polyol / nano-hydrotalcite by in-situ polymerization, which comprises the following steps: S1, adding a hydrotalcite-like compound, small molecular polyol and organic dibasic acid into a reactor, wherein a molar mass ratio of all the components is 1: (24 to 60) : (20 to 50); S2, introducing inert gas to remove air in a reaction system, warmingto a temperature of 120 to 140 DEG C, and performing a reaction for 5 hours or longer; S3, carrying out warming dehydration on the reaction system until a temperature of the reaction system is 180 DEGC, and continuously warming to a temperature of 220 DEG C; S4, measuring an acid value of the reaction system, and vacuumizing until the acid value is reduced to a value being equal to or smaller than 1mgKOH / g. According to the method, a reaction temperature of intercalation is raised, dispersion of hydrotalcite in polyester polyol is implemented; in the whole reaction process, intermediate products do not need to be subjected to separation and purification; reaction time is saved; the method has good economic benefits.

Description

technical field [0001] The invention relates to the field of polyurethane raw materials, in particular to a method for preparing polyester polyol / nanometer hydrotalcite by in-situ polymerization. Background technique [0002] Because polyurethane rigid foam has the characteristics of low density, high strength, low thermal conductivity, excellent heat insulation and sound insulation performance, and simple and fast processing and molding, it is widely used in petroleum, chemical industry, construction, refrigeration, refrigerator, aviation, transportation, etc. On the one hand, it is used as thermal insulation material and structural material. However, with the increasing use of polyurethane foam, there is an urgent need to improve the flame retardancy and high temperature resistance of the material. [0003] Adding hydrotalcite compounds into polyurethane foam is a good way to improve the light stability, thermal stability and flame retardancy of rigid polyurethane foam....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/183C08G63/20C08G63/676C08G63/78C08G18/42C08K3/26C08G101/00
CPCC08G18/4213C08G18/4238C08G18/4241C08G18/425C08G63/16C08G63/183C08G63/20C08G63/676C08G63/78C08K3/26C08K2201/011C08G2110/0025
Inventor 张崇印杜鹏飞朱雪艳陈登龙曹晓韩亚刚连爱珍何腾锋堵同亮王钰奉
Owner SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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