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Preparation method of copolymerization modified thermosetting polyimide material

A polyimide and copolymerization modification technology, which is used in the preparation of copolymerization modified thermosetting polyimide materials, can solve problems such as complex curing mechanism, and achieve the advantages of low price, improved market competitiveness and low melt viscosity. Effect

Inactive Publication Date: 2020-06-05
SHEN MA INDUSTRY CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phenylacetylene phthalic anhydride mainly forms a polyene structure and a cyclic olefin structure during the high-temperature cross-linking curing process. The curing mechanism is relatively complicated, and there is no conclusion yet.

Method used

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  • Preparation method of copolymerization modified thermosetting polyimide material
  • Preparation method of copolymerization modified thermosetting polyimide material

Examples

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Effect test

Embodiment 1

[0033] The preparation method of the copolymerized modified thermosetting polyimide material of the present invention, the detailed steps of the preparation method are as follows:

[0034] a. First, under the protection of nitrogen, add 30g of N-methylpyrrolidone NMP into a three-necked round-bottomed flask with mechanical stirring, and then add 10g of 3,4'-diaminodiphenyl ether and stir to fully dissolve it;

[0035] b. After the 3,4'-diaminodiphenyl ether in step a is completely dissolved, add 4.36g pyromellitic dianhydride PMDA and 6.2g 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride a-ODPA and 30g N-methylpyrrolidone NMP, then react at room temperature, the reaction time is 6h;

[0036] c. Step b. After the reaction is over, add 4.96g of end-capping agent 4-phenylacetylene phthalic anhydride and N-methylpyrrolidone NMP, control the solid content of the solution to 20%, continue to stir and react at room temperature for 24h, and obtain polyamide Acid solution

[0037] d. Heat...

Embodiment 2

[0040] The preparation method of the copolymerized modified thermosetting polyimide material of the present invention, the detailed steps of the preparation method are as follows:

[0041] a. First, under the protection of nitrogen, add 30g of N-methylpyrrolidone NMP into a three-necked round-bottomed flask with mechanical stirring, and then add 10g of 4,4'-diaminodiphenyl ether and stir to fully dissolve;

[0042] b. After the 4,4'-diaminodiphenyl ether in step a is completely dissolved, add 4.36g pyromellitic dianhydride PMDA and 6.2g 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride a-ODPA and 30g N-methylpyrrolidone NMP, then react at room temperature, the reaction time is 5h;

[0043] c. Step b: After the reaction is over, add 4.96g of the end-capping agent 4-phenylacetylene phthalic anhydride and N-methylpyrrolidone NMP, control the solid content of the solution to 20%, continue to stir and react at room temperature for 10 hours, and obtain polyamide after the reaction Acid...

Embodiment 3

[0047] The preparation method of the copolymerized modified thermosetting polyimide material of the present invention, the detailed steps of the preparation method are as follows:

[0048] a. First, under the protection of nitrogen, add 30g of N-methylpyrrolidone NMP into a three-necked round-bottomed flask with mechanical stirring, and then add 10g of 3,4'-diaminodiphenyl ether and stir to fully dissolve it;

[0049] b. After the 3,4'-diaminodiphenyl ether in step a is completely dissolved, add 2.18g pyromellitic dianhydride PMDA and 9.3g 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride a-ODPA and 30g N-methylpyrrolidone NMP, then react at room temperature, the reaction time is 6h;

[0050] c. Step b. After the reaction is over, add 4.96g of end-capping agent 4-phenylacetylene phthalic anhydride and N-methylpyrrolidone NMP, control the solid content of the solution to 20%, continue to stir and react at room temperature for 24h, and obtain polyamide Acid solution

[0051] d. Heat...

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Abstract

The invention discloses a preparation method of a copolymerization modified thermosetting polyimide material. The preparation method comprises the following steps: firstly, adding an organic solvent into a reaction vessel, and then adding diaminodiphenyl ether for fully dissolving; then adding pyromellitic dianhydride, 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and an organic solvent, and carrying out a reaction at room temperature; after the reaction is finished, adding an end-capping reagent and an organic solvent, controlling the solid content of the solution, and continuously reacting at room temperature to obtain a polyamide acid solution; and carrying out a high-temperature thermal imidization reaction or a chemical imidization reaction on the obtained polyamide acid solution to obtain the copolymerization modified thermosetting polyimide material. The thermosetting polyimide material prepared through copolymerization modification has the advantage of being low in cost,the melting processability and temperature resistance of the material are balanced, and the thermosetting polyimide material can be used for preparing special profiles such as high-temperature-resistant bearings, mechanical parts, pipes and bars through mold pressing.

Description

[0001] 1. Technical Field: [0002] The invention belongs to the field of special engineering plastics and their preparation, and particularly relates to a preparation method of a copolymerized modified thermosetting polyimide material. [0003] 2. Background technology: [0004] Polyimide materials are a class of high-performance polymers that have been successfully used in the past decades. Due to the excellent comprehensive properties of polyimide, it has been well applied in many high-tech fields. According to the structural characteristics, polyimide can be divided into thermoplastic polyimide and thermosetting polyimide. Thermoplastic polyimide has a linear structure, a long molecular chain, and exhibits high melt viscosity and poor Solubility, difficult to process and shape. The thermosetting polyimide is a low-molecular-weight prepolymer containing active end-capping groups before cross-linking. The molecular chain has weak force and is not easy to entangle. It exhibits low ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12
CPCC08G73/127
Inventor 王巍宇平窦晓勇薛敏钊汤荇刘燕刚吕建夫
Owner SHEN MA INDUSTRY CO LTD
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