Method for preparing high-strength high-modulus organosilicone modified PI/SiO2 hybridization film

A high-strength, high-modulus, organosilicon technology, which is applied in the field of preparation of high-strength and high-modulus organosilicon modified PI/SiO2 hybrid films, can solve the problems of polyimide material voids, difficulty in meeting high-strength and high-modulus, affecting mechanical properties, etc. , to achieve the effect of good uniformity and accuracy, excellent comprehensive performance, and large molecular weight of the product

Inactive Publication Date: 2014-01-01
SOUTH CHINA NORMAL UNIVERSITY
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Problems solved by technology

[0003] Due to the rigidity of the polyimide molecular chain itself and the strong interaction between molecules, ordinary polyimide neither melts nor dissolves until the decomposition temperature, which makes its processing difficult.
In addition, during the high-temperature imidization process, a large amount of water molecules are released, resulting in voids in the internal structure of the polyimide material, which affects its final mechanical properties, and it is difficult to meet the requirements of high strength and high modulus.

Method used

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  • Method for preparing high-strength high-modulus organosilicone modified PI/SiO2 hybridization film
  • Method for preparing high-strength high-modulus organosilicone modified PI/SiO2 hybridization film

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preparation example Construction

[0031] High-strength and high-modulus organosilicon modified PI / SiO 2 The preparation method of the hybrid thin film is characterized in that the specific preparation steps are as follows:

[0032] (1) Add the aromatic dianhydride into the organic solvent, control the temperature at 20-30°C, dissolve under stirring, add the aminosilane coupling agent, keep the temperature and stir, and react for 3-8 hours;

[0033] (2) Add the aromatic diamine into the organic solvent, control the temperature at 20-30°C, dissolve under stirring, add the aromatic dianhydride and the system of step (1), then add ethyl orthosilicate, control the temperature Keep stirring at 30-40°C, and react for 4-6 hours to obtain a silicone-modified polyamic acid resin solution;

[0034] (3) Dilute the silicone-modified polyamic acid resin solution in the above step (2) with an organic solvent to a suitable coating viscosity, spread the film on a clean support after defoaming, and control the film thickness t...

Embodiment 1

[0047] Under the protection of a nitrogen atmosphere, add 0.004mol of pyromellitic dianhydride to 10ml of N,N-dimethylacetamide, control the temperature at 20°C, stir and dissolve, then add an equimolar amount of γ-aminopropyltriethoxy base silane, stirred at constant temperature, and reacted for 3 hours to obtain N, N-dimethylacetamide solution of organosilicon-modified aromatic dianhydride monomer;

[0048] Under the protection of nitrogen atmosphere, add 0.104mol 4,4-diaminodiphenyl ether into 250ml N,N-dimethylacetamide, control the temperature at 20°C, stir and dissolve, then add the above silicone modified aromatic dianhydride Monomer N,N-dimethylacetamide solution and 0.1mol pyromellitic dianhydride, then add 0.00312mol ethyl orthosilicate, control the temperature at 30°C, stir and react for 4 hours to obtain a viscosity of 3050Pa. The organosilicon-modified polyamic acid resin solution of s;

[0049] Dilute the silicone-modified polyamic acid resin solution with N,N-d...

Embodiment 2

[0053] Under the protection of a helium atmosphere, add 0.01mol of biphenyltetracarboxylic dianhydride to 10ml of N,N-dimethylformamide, control the temperature at 30°C, stir and dissolve, then add an equimolar amount of γ-aminopropyltrimethoxy base silane, stirred at constant temperature, and obtained the N,N-dimethylformamide solution of organosilicon-modified aromatic dianhydride monomer after reacting for 8 hours;

[0054] Under the protection of a helium atmosphere, add 0.11mol of p-phenylenediamine to 250ml of N,N-dimethylformamide, control the temperature at 30°C, stir and dissolve, then add the N of the above silicone-modified aromatic dianhydride monomer , N-dimethylformamide solution and 0.1mol biphenyltetracarboxylic dianhydride, then add 0.0088mol ethyl orthosilicate, control the temperature at 40°C, stir and react for 6 hours to obtain a viscosity of 2950Pa. The organosilicon-modified polyamic acid resin solution of s;

[0055] Dilute the silicone-modified polyam...

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Abstract

The invention discloses a method for preparing a high-strength high-modulus organosilicone modified PI / SiO2 hybridization film. The method includes the following steps that firstly, aminosilane coupling reagents are fully reacted with aromatic anhydride in a solvent; secondly, the aromatic anhydride is dissolved in the solvent and made into a solution, the system, the aromatic anhydride and tetraethyl orthosilicate in the first step are added into the solution, and a polymerization reaction is performed to obtain an organosilicone modified polyamide acid solution; the organosilicone modified polyamide acid solution obtained in the second step is diluted, arranged on a supporting body in a coating mode and roasted, and the film is obtained; fourthly, the film undergoes temperature rising, dehydration and crosslinking, and a product is obtained. According to the method for preparing the high-strength high-modulus organosilicone modified PI / SiO2 hybridization film, the prepared hybridization film is high in stretching strength and modulus of elasticity, and the defect that a large amount of water is brought to the system by conventionally adding sol-gel state silicon dioxide is overcome. The method for preparing the high-strength high-modulus organosilicone modified PI / SiO2 hybridization film can well control the reaction evenness and the reaction accuracy and is short in experimental period, simple in technology and suitable for industrial production.

Description

technical field [0001] The invention relates to a high-strength and high-modulus organosilicon modified PI / SiO 2 Preparation method of hybrid film. Background technique [0002] Polyimide (Polyimide, abbreviated as PI) refers to a class of polymers containing imide rings in the main chain, among which polymers containing phthalimide structures are particularly important. Its structure determines that polyimide polymer materials have excellent heat resistance, wear resistance, radiation resistance, chemical resistance, good electrical insulation, toughness and flexibility, and also have high Gas permeability, so it is widely used in high-tech fields such as aviation, aerospace, electrical, microelectronics and automobiles, and the demand is increasing year by year. [0003] Due to the rigidity of the polyimide molecular chain itself and the strong interaction between the molecules, ordinary polyimide neither melts nor dissolves until the decomposition temperature, which mak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08C08K3/36C08J5/18
Inventor 石光陈银珊黄雨鸣陈建平
Owner SOUTH CHINA NORMAL UNIVERSITY
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