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Preparation method of polyimide/ladder-like polysiloxane double-sided anisotropic composite thin film

A polysiloxane and composite film technology, applied in the field of polymer materials, can solve the problems of low mechanical properties and heat resistance, film brittleness, etc., and achieve the effects of high stability, low volume parameters, and cheap and easy-to-obtain raw materials

Active Publication Date: 2011-11-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polyimide / ladder polysiloxane composite film prepared by the present invention has two-sided anisotropy, that is, the upper surface of the composite film has good hydrophobicity, and the matrix of the composite film still maintains the characteristics of polyimide, which solves the problem of Low mechanical properties and heat resistance of the existing polyimide / siloxane composite film and brittleness of the film

Method used

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  • Preparation method of polyimide/ladder-like polysiloxane double-sided anisotropic composite thin film
  • Preparation method of polyimide/ladder-like polysiloxane double-sided anisotropic composite thin film
  • Preparation method of polyimide/ladder-like polysiloxane double-sided anisotropic composite thin film

Examples

Experimental program
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Effect test

Embodiment 1

[0044] 1) Add 0.01mol (2g) 4,4-ODA and 40mlDMAc into a three-necked flask, stir and dissolve, then add 0.0101mol PMDA (2.2g), and continue the reaction at room temperature for 1 hour to obtain a polyamide with a solid content of 10% acid solution;

[0045]2) Add 0.0001mol (0.0163g) γ-aminopropyltriethoxysilane to the polyamic acid, and stir the reaction at room temperature for 1 hour. After capping the polyamic acid, add 0.105g of trapezoidal phenyl polysilicon Oxane powder and 0.0003mol (0.0054g) of an acidic aqueous solution with a pH value of 3 were stirred at room temperature for 3 hours to obtain a polyamic acid / trapezoidal phenylpolysiloxane solution;

[0046] 3) After defoaming the polyamic acid / ladder polysiloxane solution, scrape-coat it on a glass plate to form a film, let it stand at room temperature for 0.5 hours, put it in an oven for 10 hours at 80°C, and then transfer it to a curing oven. Curing was performed at 80°C for 30 minutes, at 100°C for 120 minutes, at...

Embodiment 2

[0048] 1) Add 0.01mol (2g) 4,4'-ODA and 18ml DMAc into a three-necked flask, stir and dissolve, then add 0.0101mol PMDA (2.2g), after the addition, continue to react at room temperature for 3 hours to obtain the solid content 20% polyamic acid solution;

[0049] 2) Add 0.0001mol (0.0163g) γ-aminopropyltriethoxysilane to the polyamic acid, and stir the reaction at room temperature for 6 hours. After capping the polyamic acid, add 0.105g of trapezoidal phenyl polysilicon Oxane powder and 0.0006mol (0.0108g) an acidic aqueous solution with a pH value of 3, stirred at room temperature for 10 hours to obtain a polyamic acid / trapezoidal phenyl polysiloxane solution;

[0050] 3) After defoaming the polyamic acid / ladder polysiloxane solution, scrape-coat it on a glass plate to form a film, let it stand at room temperature for 2 hours, put it in an oven for 10 hours at 80°C, and then transfer it to a curing oven. Curing was performed at 80°C for 30 minutes, at 100°C for 120 minutes, a...

Embodiment 3

[0052] 1) Add 0.01mol (2g) 4,4'-ODA and 66.7ml DMAc into a three-necked flask, stir and dissolve, then add 0.0101mol PMDA (2.2g), after the addition is complete, continue to react at room temperature for 2 hours to obtain the solid content 6% polyamic acid solution;

[0053] 2) Add 0.0001mol (0.0163g) γ-aminopropyltriethoxysilane to the polyamic acid, and stir and react at room temperature for 4 hours. After capping the polyamic acid, add 0.63g of trapezoidal phenyl polysilicon Oxane powder and 0.0004mol (0.0072g) an acidic aqueous solution with a pH value of 3, stirred at room temperature for 6 hours to obtain a polyamic acid / trapezoidal phenyl polysiloxane solution;

[0054] 3) After defoaming the polyamic acid / ladder polysiloxane solution, scrape-coat it on a glass plate to form a film, let it stand at room temperature for 2 hours, put it in an oven for 10 hours at 80°C, and then transfer it to a curing oven. Curing was performed at 80°C for 30 minutes, at 100°C for 120 mi...

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Abstract

The invention relates to a preparation method of a polyimide / ladder-like polysiloxane double-sided anisotropic composite thin film, which belongs to the field of polymer materials. The existing polyimide / organic siloxane composite thin film is prepared by introducing a poly-linear siloxane chain segment into a polyimide substrate through the copolymerization method or the doping method, and the prepared thin film has low mechanical property, low thermal resistance and great brittleness. The preparation method comprises the steps of using gamma-aminopropyltriethoxysilane and polyamic acid for carrying out reaction, utilizing hydrolytic condensation of the gamma-aminopropyltriethoxysilane for introducing ladder-like polysiloxane into the polyamic acid, and carrying out curing for preparing the polyimide / ladder-like polysiloxane double-sided anisotropic composite thin film. Compared with the prior art, the method can simultaneously maintain the mechanical property of the thin film while preparing the double-sided anisotropic composite thin film, and also solve the brittleness problem of the thin film and the obvious decline problem of the thermal performance. Simultaneously, the preparation method has the advantages of simple reaction steps, strong operationability, no toxicity, no pollution, easy industrialization and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of a polyimide / ladder polysiloxane double-sided heterosexual composite film. Background technique [0002] Polyimide (PI) is an excellent high-temperature-resistant material with excellent mechanical properties, dielectric properties, and radiation resistance, especially in high-temperature conditions with excellent comprehensive properties. Therefore, it is widely used in many fields such as machinery, electronics, and aviation. However, its high hygroscopicity and high surface energy limit its application in electrical insulating varnishes, cushioning materials, and interlayer packaging materials. [0003] At present, polyorganosiloxanes have been widely used due to their outstanding physical properties, such as excellent thermal stability, low capacitance parameter, high stability in oxygen atom plasma environment, good hydrophobicity and low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L83/00C08L79/08C08G73/10
Inventor 武德珍冯玉仲齐胜利吴战鹏马卉
Owner BEIJING UNIV OF CHEM TECH
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