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High-temperature-resistant acetenyl-terminated polyimide material and preparation method thereof

A technology of polyimide and end-imide acid, applied in the direction of adhesives, etc., can solve the problems of brittle material and narrow processing window, and achieve the effect of weakening interaction force, high temperature resistance and lowering softening point.

Pending Publication Date: 2020-05-15
SHEN MA INDUSTRY CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ethynyl-terminated materials have always had defects such as starting to cross-link after melting, the processing window is too narrow, and the material is brittle after cross-linking.

Method used

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  • High-temperature-resistant acetenyl-terminated polyimide material and preparation method thereof
  • High-temperature-resistant acetenyl-terminated polyimide material and preparation method thereof
  • High-temperature-resistant acetenyl-terminated polyimide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation method of the high temperature resistant acetylene group-terminated polyimide material of the present invention, the detailed steps of this preparation method are as follows:

[0048] a. First, under the protection of nitrogen, 50g of N,N-dimethylacetamide was added to a three-necked round-bottomed flask with mechanical stirring, and then 8g of 4-phenoxy m-phenylenediamine was added to fully dissolve;

[0049] b. When 4-phenoxym-phenylenediamine is completely dissolved in step a, add 24.8g of 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and 50g of N,N-dimethylacetamide , and then stirred and reacted at 30°C for 6h;

[0050] c. After the reaction in step b, add 9.36 g of end-capping agent 3-ethynylaniline and N,N-dimethylacetamide, control the solid content of the solution to 20%, and continue the reaction at 30°C for 24 hours to obtain ethynyl-capped Terminal imidic acid solution;

[0051] d. Add 48.48 g of triethylamine and 48.96 g of acetic a...

Embodiment 2

[0055] The preparation method of the high temperature resistant acetylene group-terminated polyimide material of the present invention, the detailed steps of this preparation method are as follows:

[0056] a. First, under the protection of nitrogen, 50g of N-methylpyrrolidone NMP is added to a three-necked round-bottomed flask with mechanical stirring, and then 11.04g of 4-(4'-biphenyloxy) m-phenylenediamine is added, fully dissolved;

[0057] b. When 4-(4'-biphenoxy) m-phenylenediamine is completely dissolved in step a, add 24.8g of 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and 50g of N-methyl Basepyrrolidone NMP, then stirred and reacted at 60°C for 9h;

[0058] c. After the reaction in step b, add 9.36 g of end-capping agent 3-ethynyl aniline and N-methylpyrrolidone NMP, control the solid content of the solution to 20%, and continue the reaction at 60°C for 24 hours to obtain ethynyl-terminated acylidene Amino acid solution;

[0059] d. Add 32.32 g of triethy...

Embodiment 3

[0062] The preparation method of the high temperature resistant acetylene group-terminated polyimide material of the present invention, the detailed steps of this preparation method are as follows:

[0063] a. First, under the protection of nitrogen, 60g of 1,4-dioxane was added to a three-necked round-bottomed flask with mechanical stirring, and then 8g of 4-phenoxy m-phenylenediamine was added to fully dissolve;

[0064] b. When 4-phenoxym-phenylenediamine is completely dissolved in step a, add 24.8g of 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and 60g of 1,4-dioxane, Then the reaction was stirred and reacted at 40°C for 8h;

[0065] c. After the reaction in step b, add 9.36 g of end-capping agents 3-ethynylaniline and 1,4-dioxane, control the solid content of the solution to 15%, and continue the reaction at 40°C for 12 hours to obtain ethynyl end-capping imidic acid solution;

[0066] d. Add 48.48 g of triethylamine and 100.08 g of trifluoroacetic anhydride dr...

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Abstract

The invention discloses a high-temperature-resistant acetenyl-terminated polyimide material and a preparation method thereof. The preparation method comprises the steps: firstly, adding a diamine monomer into an organic solvent for fully dissolving under the protection of nitrogen; then adding 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and an organic solvent, and carrying out a reaction;after the reaction, adding an end-capping reagent 3-acetenyl aniline and an organic solvent, and carrying out a reaction to obtain an acetenyl end-capped imide acid solution; adding a catalyst and adehydrating agent into the ethynyl-terminated imide acid solution to carry out a chemical imidization dehydration reaction; and washing, drying and crushing the solution obtained after the reaction tofinally obtain the powdery acetenyl-terminated polyimide prepolymer. The obtained thermosetting polyimide material has low requirements on the temperature of equipment in the molding process, and theprepared material has high temperature resistance and has potential application value in the fields of preparation of high-performance advanced resin-based composite materials, high-temperature-resistant adhesives and the like.

Description

[0001] 1. Technical field: [0002] The invention relates to the technical field of high-performance polyimide materials, in particular to a high-temperature-resistant ethynyl-terminated polyimide material and a preparation method thereof. [0003] 2. Background technology: [0004] As an important member of the high-performance polymer family, polyimide materials can be made into films, fibers, adhesives, profiles and advanced Composite materials and other products are widely used in microelectronics, machinery manufacturing, national defense and aerospace and other fields. According to different types, polyimide materials can be divided into thermoplastic polyimide and thermosetting polyimide. Thermosetting polyimide is a prepolymer with low molecular weight and active groups first synthesized, and then processed for crosslinking and curing reaction to obtain high molecular weight polyimide material. [0005] The crosslinking temperature of phenylethynyl-terminated thermose...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08C09J179/08
CPCC08G73/1071C08G73/1007C08G73/1046C08L79/08C09J179/08C08L2201/08
Inventor 王巍宇平窦晓勇薛敏钊汤荇牛乐朋刘燕刚吕建夫
Owner SHEN MA INDUSTRY CO LTD
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