A kind of imide side chain-containing cage silsesquioxane/polyimide nanocomposite material and preparation method thereof

A nanocomposite material and technology of silsesquioxane are applied in the field of imide side chain cage-type silsesquioxane/polyimide nanocomposite materials and their preparation, and can solve the problem of copolymerized POSS polyimide The problems of high production cost of amines, difficult productization, phase separation and agglomeration, etc., achieve the effects of excellent antigenic oxygen performance, reduced preparation cost, and high yield

Active Publication Date: 2020-03-27
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved in the present invention is that the production cost of copolymerized type POSS polyimide is high, the difficulty of commercialization and the problems of phase separation and agglomeration easily occur between POSS nanoparticles and matrix in the preparation process of blended type POSS polyimide, for Therefore, the invention provides a cage-type silsesquioxane / polyimide nanocomposite material containing imide side chains and a preparation method thereof

Method used

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  • A kind of imide side chain-containing cage silsesquioxane/polyimide nanocomposite material and preparation method thereof
  • A kind of imide side chain-containing cage silsesquioxane/polyimide nanocomposite material and preparation method thereof
  • A kind of imide side chain-containing cage silsesquioxane/polyimide nanocomposite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Dissolve 1.153g octaaminophenyl POSS in 10.4g N-methylpyrrolidone (NMP) at room temperature and under nitrogen protection, and stir for 15 minutes to obtain octaaminophenyl POSS solution 1; add 1.185g in 3 times Phthalic anhydride continued to react for 12 hours; N-methylpyrrolidone (NMP) was removed by distillation under reduced pressure to obtain POSS1 containing amic acid branch;

[0025](2) At room temperature and under the protection of nitrogen, add 2.002g 4,4'-diaminodiphenyl ether into 18g NMP, stir for 15 minutes to obtain 4,4'-diaminodiphenyl ether solution; add 3.042g in 3 times 3,3,4',4'-biphenyltetraacid dianhydride, add 27.4g NMP, stir and polymerize for 12 hours to obtain polyamic acid 1;

[0026] (3) Dissolve 0.504g of POSS1 containing amic acid branched chain in 4.5g NMP, stir for 15 minutes to obtain the POSS1 solution containing amic acid branched chain; slowly add the POSS1 solution containing amic acid branched chain to the poly Stir in the ami...

Embodiment 2

[0037] (1) Dissolve 1.072g of octaaminopropyl POSS in 20.4g of N,N-dimethylacetamide (DMAc) at room temperature and under the protection of nitrogen, and stir for 30 minutes to obtain octaaminopropyl POSS solution 2; Add 1.185g phthalic anhydride once, continue reaction 24 hours; Underpressure distillation removes DMAc, obtains the POSS2 containing amic acid branch;

[0038] (2) At room temperature and under nitrogen protection, add 2.002g of 4,4'-diaminodiphenyl ether into 38g of DMAc and stir for 30 minutes to obtain a 4,4'-diaminodiphenyl ether solution; add 3.016 g 3,3,4',4'-biphenyltetraacid dianhydride, add 57.3gDMAc, stir and polymerize for 24 hours to obtain polyamic acid 2;

[0039] (3) 0.105g POSS2 containing amic acid branch was dissolved in 2g DMAc, and stirred for 30 minutes to obtain the POSS2 solution containing amic acid branch; the POSS2 solution containing amic acid branch was slowly added to the polymer in 15 minutes. Stir in the amic acid 2 solution for 16...

Embodiment 3

[0042] (1) Dissolve 1.153g of octaaminophenyl POSS in 10.4g of N,N-dimethylformamide (DMF) at room temperature and under the protection of nitrogen, and stir for 15 minutes to obtain octaaminophenyl POSS solution 3; Add 1.185g of phthalic anhydride for 3 times, continue to react for 12 hours; remove DMF by distillation under reduced pressure, and obtain POSS3 containing amic acid branch;

[0043] (2) At room temperature and under the protection of nitrogen, 4.105g of 2,2-bis[4-(4-aminophenoxy)phenyl]propane was added to 36.9g of NMP and stirred for 15 minutes to obtain 2,2-bis[ 4-(4-aminophenoxy)phenyl]propane solution; 2.255g of pyromellitic dianhydride was added in 3 times, 20.3g of NMP was added, stirred and polymerized for 12 hours to obtain polyamic acid 3;

[0044] (3) Dissolve 0.318g of POSS1 containing amic acid branched chains in 2.86g NMP, stir for 15 minutes to obtain a POSS3 solution containing amic acid branched chains; slowly add the POSS3 solution containing ami...

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Abstract

The invention provides an imide side chain containing polyhedral oligomeric silsesquioxane / polyimide nano composite and a preparation method thereof, and belongs to the field of preparation of polyimide. The imide side chain containing polyhedral oligomeric silsesquioxane / polyimide nano composite comprises a dispersing phase and a continuous phase, wherein the dispersing phase is imide side chain containing polyhedral oligomeric silsesquioxane; the continuous phase is polyimide. The preparation method comprises the following steps: reacting phthalic anhydride and octaamino polyhedral oligomeric silsesquioxane to obtain amido acid branch chain containing polyhedral oligomeric silsesquioxane; mixing amido acid branch chain containing polyhedral oligomeric silsesquioxane and polyamide acidbased on ratio under solution; and performing thermal imidization to obtain the imide side chain containing polyhedral oligomeric silsesquioxane / polyimide nano composite. The imide side chain containing polyhedral oligomeric silsesquioxane / polyimide nano composite is outstanding in anti-atomic oxygen performance, easy to prepare, high in yield and low in synthesizing cost.

Description

technical field [0001] The invention relates to the field of polyimide preparation, in particular to a cage-type silsesquioxane / polyimide nanocomposite material containing imide side chains and a preparation method thereof. Background technique [0002] Low earth orbit is an important orbit for aircraft, ranging from 200 to 700 kilometers in outer space. Aircraft such as space stations and high-resolution earth observation systems operate in this orbit, and hazardous environmental factors such as atomic oxygen, plasma, ultraviolet radiation, thermal cycles, high vacuum, and space debris affect the normal operation of aircraft. Among them, atomic oxygen is known as "the most dangerous factor". Atomic oxygen has the characteristics of high-temperature oxidation and high-speed collision, and erodes the polymer materials outside the spacecraft. The Kapton polyimide material produced by DuPont of the United States is widely used in the outermost layer of the multi-layer heat ins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08L83/04C08G77/38C08G73/10
CPCC08G73/1071C08G77/045C08L79/08C08L2201/08C08L83/04
Inventor 陈春海王春博赵晓刚王大明周宏伟
Owner JILIN UNIV
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