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A method for preparing poly(urea-imide) cross-linked and cured by cage-type silsesquioxane

A technology of silsesquioxane and imide, which is applied in the direction of coating, etc., can solve the problem of few high-temperature-resistant materials, and achieve the effects of short reaction cycle, excellent mechanical properties, and improved heat resistance

Active Publication Date: 2017-01-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, the research and development of POSS composite polymer materials have become more and more diversified, and many meaningful results have been produced; however, there are few researches on low-temperature curing high-temperature resistant materials, and there is no patent report in China. Preparation method of poly(urea-imide) high temperature resistant coating material modified by silsesquioxane

Method used

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  • A method for preparing poly(urea-imide) cross-linked and cured by cage-type silsesquioxane
  • A method for preparing poly(urea-imide) cross-linked and cured by cage-type silsesquioxane
  • A method for preparing poly(urea-imide) cross-linked and cured by cage-type silsesquioxane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Weigh 8g of isophorone diisocyanate into a three-necked flask, and add 2mL of N,N-dimethylformamide as a solvent. Weigh 10.53g of amino-terminated polyether (molecular weight 600) and dissolve it in 20mL of N,N-dimethylformamide, add it to the isophorone diisocyanate solution, mix and stir evenly under nitrogen protection, and react at room temperature for 2 hours. Weigh 1.91g of pyromellitic anhydride and add it to the above reaction solution, drop into 9mL of triethylamine catalyst (drop three times, once every 6 hours), raise the temperature to 85°C, react for 24 hours under nitrogen protection, and use saturated lime CO produced by the water detection reaction 2 , to determine whether the reaction is complete. To be free of CO 2 After release, stop the reaction. Take 20g of the reaction solution, add 1.24g of highly reactive octaphenylamino cage silsesquioxane under stirring, continue stirring with a magnetic force for 30min, let it stand for a while, and pour th...

Embodiment 2

[0026] Weigh 8g of isophorone diisocyanate into a three-necked flask, and add 2mL of N,N-dimethylformamide as a solvent. Weigh 10.8g of amino-terminated polyether (molecular weight 600) and dissolve it in 20mL of N,N-dimethylformamide, add it to the isophorone diisocyanate solution, mix and stir evenly under nitrogen protection, and react at room temperature for 2 hours. Weigh 1.96g of pyromellitic anhydride and add it to the above reaction solution, drop into 9mL of triethylamine catalyst (drop three times, once every 6 hours), raise the temperature to 85°C, react for 24 hours under nitrogen protection, and use saturated lime CO produced by the water detection reaction 2 , to determine whether the reaction is complete. To be free of CO 2 After release, stop the reaction. Take 20g of the reaction solution, add 1.3g of highly reactive octaphenylamino cage silsesquioxane under stirring, continue stirring with a magnetic force for 30min, let it stand for a while, and pour the ...

Embodiment 3

[0028] Weigh 8g of isophorone diisocyanate into a three-necked flask, and add 2mL of N,N-dimethylformamide as a solvent. Weigh 35.11g of amino-terminated polyether (molecular weight: 2000) and dissolve it in 70mL of N,N-dimethylformamide, add it to the isophorone diisocyanate solution, mix and stir evenly under the protection of nitrogen, and react at room temperature for 2 hours. Weigh 1.91g of pyromellitic anhydride and add it to the above reaction solution, drop into 9mL of triethylamine catalyst (drop three times, once every 6 hours), raise the temperature to 85°C, react for 24 hours under nitrogen protection, and use saturated lime CO produced by the water detection reaction 2 , to determine whether the reaction is complete. To be free of CO 2After release, stop the reaction. Take 40g of the reaction solution, add 1.01g of highly reactive octaphenylamino cage silsesquioxane under stirring, continue stirring with a magnetic force for 30min, let it stand for a while, and...

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Abstract

The present invention provides a method for preparing cage silsesquioxane cured poly(urea-imide). The present invention utilizes the reaction of polyurea oligomer and pyromellitic anhydride to prepare poly(urea-imide) prepolymer, and then solidifies with octaaniline cage silsesquioxane with high reactivity, and finally prepares A high temperature resistant coating material. The synthesized poly(urea-imide) of this method not only has the excellent processability of polyurea, plasticity, excellent adhesion and excellent dielectric properties, but also has the toughness and strength of polyimide, At the same time has excellent thermal stability. Coating materials with different strength and heat resistance properties can be obtained by adjusting the content of polyurea segment. The method only needs curing at normal temperature, has simple process, low production cost and wide industrialization prospect.

Description

technical field [0001] The invention relates to a method for preparing a poly(urea-imide) high-temperature-resistant coating material by using cage-type silsesquioxane as a crosslinking agent to solidify, and belongs to the technical field of hybrid material preparation. Background technique [0002] In recent years, block copolymers have attracted much attention because they have the characteristics of block units. Polyurea (PU) and polyimide (PI) are two polymer materials with excellent properties, but the disadvantages of PU's poor heat resistance and PI's poor flexibility greatly limit their application in some technical fields. In order to make up for their shortcomings, chemical methods were used to embed PU and PI into the same main chain to prepare poly( Urea-imide) block copolymer (PUI), the structural characteristics of PUI determine that it has the advantages of both polyurea and polyimide, and has excellent performance. By adjusting the content of polyurea soft...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08G18/50C09D179/08
Inventor 李齐方郭志龙周政
Owner BEIJING UNIV OF CHEM TECH