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Method of preparing polyimide/inorganic nano hybridization material

A technology of polyimide and inorganic nanometers, which is applied in the field of preparation of polyimide/inorganic nanometer hybrid materials, can solve the problems of difficult particle modification and unsatisfactory dispersion method research, and achieve the solution of nanoparticle dispersion problems, uniform distribution, and improved heat resistance

Inactive Publication Date: 2007-10-24
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the surface of nanopowder is modified, the modifier is often coated with an aggregate of multiple particles, not a single particle, and it is difficult to completely modify the particle.
Therefore, the research of many decentralized methods is not very ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Phenylacetylene-terminated polyimide / nano-SiO 2 Preparation method of hybrid material:

[0024] 1. Synthesis of phenylethynyl imine cyclosilane:

[0025] (1) Phenylacetylene phthalic anhydride was added to the dimethyl sulfoxide solution of equimolar aminosilane in 4 times, and reacted at room temperature for 45 hours to obtain a phenylacetylene amic acid silane solution;

[0026] (2) Use acetic anhydride and triethylamine as an anhydride reagent for dehydration, add it to the phenylethynyl amic acid silane solution and react for 5 hours, the molar ratio of acetic anhydride to aminosilane is 3:1, acetic anhydride and triethylamine The mol ratio is 1: 0.2, and the phenylethynyl imine cyclosilane solution is obtained, and its weight ratio with dimethyl sulfoxide is 10: 90;

[0027] (3) Drop the phenylethynylimine cyclosilane solution into methanol to form a yellow precipitate, which is filtered, washed and dried to obtain a yellow powder of the phenylethynyl imine c...

Embodiment 2

[0033] (1) Norbornene-terminated polyimide / nano Al 2 o 3 Preparation method of hybrid material:

[0034] 1. Synthesis of norbornenyl imine cyclosilane:

[0035] (1) adding norbornene diacid anhydride to the dimethyl sulfoxide solution of equimolar aminosilane in 5 times, and reacting at room temperature for 50 hours to obtain a norbornene amic acid silane solution;

[0036] (2) Use acetic anhydride and triethylamine as an anhydride reagent for dehydration, add it to the norbornenyl amic acid silane solution and react for 4 hours, the molar ratio of acetic anhydride to aminosilane is 2:1, acetic anhydride and triacetic acid The molar ratio of amine is 1: 0.3, and the norbornenyl imine cyclosilane solution is obtained, and its weight ratio with dimethyl sulfoxide is 15: 85;

[0037] (3) Drop the norbornenyl imine cyclosilane solution into methanol to form a yellow precipitate, which is filtered, washed, and dried to obtain norbornenyl imine cyclosilane yellow powder, and prep...

Embodiment 3

[0043] (1) Polyimide / nano-TiO 2 Preparation method of hybrid material:

[0044] 1. Synthesis of norbornenyl imine cyclosilane (same as the second embodiment).

[0045] 2. Add titanium alkoxide to the alcohol solvent adjusted to pH 3.5 with hydrochloric acid, react at 30-35°C for 3 hours, hydrolyze and condense the alkoxide to form inorganic oxide colloidal particles, add the above-mentioned synthetic norbornene imine The N-methyl-2-pyrrolidone solution of cyclosilane is reacted at 30-35°C for 2 hours to hydrolyze the synthesized norbornenyl imine cyclosilane and condense with the hydroxyl group of the colloidal particles to form a covalent bond. Organic-inorganic composite nanoparticles are obtained, the organic phase contains a synthetic norbornenyl imine ring group, and the inorganic phase is TiO 2 Nanoparticles.

[0046] 3. Add the above-mentioned organic-inorganic composite nanoparticles to the polyamic acid solution synthesized by pyromellitic dianhydride and 4,4'-diam...

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Abstract

The invention provides a method preparing for a polyimide or an inorganic nanometer hybridized material, which comprises the following steps: synthesizing an imidogen cyclic silane adapting to the inorganic nanometer particle modifier; preparing for the inorganic oxidate nanometer particle with the sol-gel processing; adding the modifier-imidogen cyclic silane in the sol-gel reacting process; getting the organic and inorganic complex nanometer particle; making the organic and inorganic complex nanometer particle uniformly dispersing in the polyamic acid solution; getting the polyimide or the inorganic nanometer hybridized material. The invention dissolves the problem of dispersing the nanometer particles, which shows every property sufficiently.

Description

(1) Technical field [0001] The invention relates to chemical material preparation technology, in particular to a preparation method of polyimide / inorganic nanometer hybrid material. (2) Background technology [0002] At present, polyimide is the organic polymer material with the highest heat resistance level for industrial applications, and is widely used in aerospace, electrical and microelectronics industries and other fields. With the development of science and technology and the improvement of material performance requirements in application fields, polyimide / inorganic nano-hybrid materials with higher mechanical properties and heat resistance have emerged as the times require. Polyimide / inorganic nano-hybrid materials combine the advantages of polyimide, inorganic materials, and nano-materials, and economically and effectively utilize the unique optical, electrical, thermal, magnetic, force, chemical activity, and catalytic properties of nanoparticles. , has been highl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K11/00
Inventor 张春红高丽丽王震盛楠卓世强江溪
Owner HARBIN ENG UNIV
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