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A solvent-resistant polyimide film with low thermal expansion coefficient and preparation method thereof

A technology of polyimide film and low thermal expansion coefficient, which is applied in the field of solvent-resistant and low thermal expansion coefficient polyimide film and its preparation, and can solve problems such as application troubles, high thermal expansion coefficient, and poor solvent resistance of the film , to achieve the effect of good application prospects

Active Publication Date: 2019-05-14
YANCHENG XIANGYUAN ENVIRONMENTAL PROTECTION EQUIP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Recently, with the development of high-tech industries, easy-to-process soluble polyimides and fluorine-containing polyimides have received extensive attention and development. The introduction of flexible segments and trifluoromethyl groups provides polyimide films More characteristics such as low dielectric properties and good solubility bring convenience to subsequent processing, but a prominent problem is that the solvent resistance of the final film becomes worse, and the thermal expansion coefficient becomes higher, which is difficult for specific applications. caused a lot of trouble

Method used

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  • A solvent-resistant polyimide film with low thermal expansion coefficient and preparation method thereof
  • A solvent-resistant polyimide film with low thermal expansion coefficient and preparation method thereof
  • A solvent-resistant polyimide film with low thermal expansion coefficient and preparation method thereof

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Effect test

Embodiment 1

[0036] In this embodiment, the polyimide resin material has the following structural formula:

[0037]

[0038] The specific preparation method is:

[0039] (1) Under nitrogen protection, mix 4.0 mmol) of 4,4-oxodiphthalic anhydride, 3.0 mmol of 2,2′-bis(trifluoromethyl)-4,4′-diaminobiphenyl , 0.98 mmol of 2,6-diaminobenzonitrile, 0.04 mmol of 4-aminobenzonitrile and 15 ml of m-cresol were added to a 50 mL reaction flask, then 0.1 ml of isoquinoline was added, and the reaction was heated and stirred at 190 °C After 8 hours, a viscous polyimide solution was obtained. When the reaction temperature dropped to 70°C, it was diluted with 20 milliliters of m-cresol and precipitated in 400 milliliters of ethanol. After suction filtration, the ethanol was refluxed and washed twice. Put into oven and dry, make polyimide resin;

[0040] (2), the prepared polyimide resin is configured into a solution with a concentration of 10% by weight with N,N-dimethylacetamide, and the solution i...

Embodiment 2

[0045] In the present embodiment, the ratio of diamine-containing nitrile group is increased, and the polyimide resin material has the following structural formula:

[0046]

[0047] The specific preparation method is:

[0048] (1) Under the protection of nitrogen, 4.0 mmol of 4,4-oxydiphthalic anhydride, 2.0 mmol of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl, Add 1.98 mmol of 2,6-diaminobenzonitrile, 0.04 mmol of 4-aminobenzonitrile and 15 ml of m-cresol into a 50 mL reaction flask, then add 0.1 ml of isoquinoline, heat and stir at 190 °C for 8 hours , to obtain a viscous polyimide solution. When the reaction temperature drops to 80°C, dilute it with 20 ml of m-cresol and precipitate it in 400 ml of ethanol. Oven drying, obtained polyimide resin;

[0049] (2), the prepared polyimide resin is configured into a solution with a concentration of 10% by weight with N,N-dimethylacetamide, and the solution is evenly coated on a clean glass plate by casting method, The thic...

Embodiment 3

[0052] In this embodiment, the polyimide resin material has the following structural formula:

[0053]

[0054] The specific preparation method is:

[0055] (1) Under the protection of nitrogen, 4.0 mmol of 4,4-oxydiphthalic anhydride, 2.0 mmol of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl, Add 1.99 mmol of 2,6-bis(3-aminobenzyl)benzonitrile, 0.02 mmol of 2-trifluoromethyl-4-aminobenzonitrile and 15 ml of m-cresol into a 50 mL reaction flask, and then Add 0.1 ml of isoquinoline, heat and stir at 200°C for 9 hours to obtain a viscous polyimide solution. When the reaction temperature drops to 60°C, dilute with 20 ml of m-cresol and precipitate in 400 ml of ethanol , after suction filtration, ethanol reflux, boil and wash twice, put into an oven to dry, and obtain polyimide resin;

[0056] (2), the prepared polyimide resin is configured into a solution with a concentration of 10% by weight with N,N-dimethylacetamide, and the solution is evenly coated on a clean glass pla...

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Abstract

The invention discloses a solvent-resistant polyimide thin film with low thermal expansion coefficient. The polyimide thin film is characterized in that the polyimide thin film is obtained by cross-linking polyimide with the following basic structural units. A preparation method comprises the following steps of preparing a viscous polyimide solution under the protection of nitrogen, diluting the viscous polyimide solution with metacresol, performing precipitation in ethanol, performing suction filtration to obtain polyimide resin, preparing a solution from the prepared polyimide resin by virtue of N,N-dimethylacetamide, uniformly coating a clean glass plate with the solution by virtue of a tape casting method, placing the glass plate in a drying box to obtain a polyimide thin film, and performing thermal treatment on the polyimide thin film to obtain the solvent-resistant polyimide thin film with low thermal expansion coefficient. The polyimide thin film has the advantages of solvent resistance, low thermal expansion coefficient and the like.

Description

technical field [0001] The invention belongs to the field of polyimide and its preparation, in particular to a solvent-resistant polyimide film with low thermal expansion coefficient and a preparation method thereof. Background technique [0002] Polyimide is the most important variety of aromatic heterocyclic polymers developed in the past half century, and it is also a type of polymer material with the highest service temperature. It has high mechanical strength, high temperature resistance, chemical stability, and creep resistance. With excellent comprehensive performance, it has been widely used in aviation, aerospace, electrical, mechanical, microelectronics, chemical industry and other fields. [0003] Recently, with the development of high-tech industries, easy-to-process soluble polyimides and fluorine-containing polyimides have received extensive attention and development. The introduction of flexible segments and trifluoromethyl groups provides polyimide films Mor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
Inventor 尤耀康
Owner YANCHENG XIANGYUAN ENVIRONMENTAL PROTECTION EQUIP CO LTD