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Alicyclic-containing polyimide film and preparation method thereof

A polyimide film and alicyclic technology, which is applied in the field of polyimide film and its preparation, can solve the problems of low reactivity, high cost, and obstacles to popularization and application, and achieve mild reaction conditions, simple operation, and convenient source Effect

Inactive Publication Date: 2009-11-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Its shortcoming is: (1) used raw material 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride monomer is extremely expensive, causes the cost of film product to be very high, has seriously hindered its further popularization and application; ( 2) Due to the low reactivity of 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride monomer and aromatic dibasic primary amine, it is difficult to prepare high molecular weight polyimide resin, Therefore, the overall performance of its film products is greatly reduced, especially its mechanical properties.
[0011] The molecular structure and preparation method of the alicyclic polyimide film disclosed by the present invention have not yet been published in the literature or patent reports

Method used

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  • Alicyclic-containing polyimide film and preparation method thereof
  • Alicyclic-containing polyimide film and preparation method thereof
  • Alicyclic-containing polyimide film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] 23.8 grams (0.1 moles) of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane (DMDC), 41.0 grams (0.1 moles) of 2,2-bis[4-(4-amino Phenoxy) phenyl] propane (NJXBAPP) and 510 milliliters of N, N-dimethylacetamide were put into the reaction kettle, stirred at room temperature, after completely dissolving, 104.1 grams (0.2 moles) of 2,2-bis [4-(3,4-dicarboxyphenoxy)phenyl]propane dianhydride (BPADA), stirred at room temperature, after completely dissolving, the reaction was maintained for 1 hour to obtain homogeneous transparent viscous alicyclic poly Amic acid solution.

[0077] Utilize N,N-dimethylacetamide solvent to adjust the viscosity of the polyamic acid solution so that it is between 30 seconds and 60 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Remove organic solvent (recovery and reuse) and carry out dehydration thermal imidization reaction, wherein, the specific dehydration thermal imidization process is: heating from room te...

Embodiment 2

[0082]23.8 g (0.1 mole) of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane (DMDC), 54.7 g (0.1 mole) of 2,2-bis[4-(2-tri Fluoromethyl-4-aminophenoxy group) phenyl] propane (BAPP-2TF) and 910 milliliters of N, N-dimethylformamide are put into reaction kettle, stir at room temperature, after dissolving completely, add 104.1 grams ( 0.2 mol) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propanedianhydride (BPADA), stirred at room temperature, after completely dissolving, the reaction was maintained for 3 hours to obtain a homogeneous Transparent viscous polyamic acid solution containing alicyclic ring.

[0083] Utilize N,N-dimethylformamide solvent to adjust the viscosity of the polyamic acid solution so that it is between 30 seconds and 60 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Remove organic solvent (recovery and reuse) and carry out dehydration thermal imidization reaction, wherein, the specific dehydration thermal imidization process...

Embodiment 3

[0088] 23.8 g (0.1 mole) of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane (DMDC), 65.4 g (0.1 mole) of 2,2-bis[4-(2-tri Fluoromethyl-4-aminophenoxy)phenyl]hexafluoropropane (BAPFP-2TF) and 773 ml of N-methyl-2-pyrrolidone were put into the reaction kettle, stirred at room temperature, after completely dissolving, 104.1 g of (0.2 moles) of 2,2-bis[4-(3,-dicarboxyphenoxy)phenyl]propane dianhydride (BPADA), stirred at room temperature, and after completely dissolving, the reaction was maintained for 2 hours to obtain a homogeneous Transparent viscous polyamic acid solution containing alicyclic ring.

[0089] Use N-methyl-2-pyrrolidone solvent to adjust the viscosity of the polyamic acid solution so that it is between 30 seconds and 60 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Organic solvent (recovery and reuse) and dehydration heat imidization reaction, wherein, the specific dehydration heat imidization process is: heating from room ...

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Abstract

The invention relates to an alicyclic-containing polyimide film. The molecular structure general formula of the film is the right formula, wherein, -CA- is a bivalence connection group of an alicyclic dibasic primary amine, -Ar- is a bivalence connection group of an aromatic dibasic primary amine, and -R- is a bivalence connection group of an aromatic dibasic estolide. The preparation thereof includes: the alicyclic dibasic primary amine and the aromatic dibasic primary amine are dissolved in non-proton organic solvent with strong polarity, the aromatic dibasic estolide is added, the non-proton organic solvent with strong polarity is used for regulating the viscosity of the alicyclic-containing polyamic acid resin solution after reaction for 1-3 hours, forming is carried out in a curtain coating machine, and dehydration fever imidization, cooling and demoulding are carried out so as to obtain the film. The preparation method has mild reaction condition and low cost and is environmentally friendly; and meanwhile, the alicyclic-containing polyimide film has excellent mechanic property and heat resistant property and low water absorption, and the visible light transmission thereof is as high as more than 97%. The film has good application prospect in the fields of optical waveguide material, photorefractive material and photoelectric material in optical communication field and direct action membrane material in the liquid crystal display field and the like.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to an alicyclic polyimide film and its preparation method. Background technique [0002] Polyimide film is a kind of polymer material with excellent comprehensive properties. It has particularly excellent heat resistance, low temperature resistance, flame retardancy, electrical properties and mechanical properties. It is widely used in electronic microelectronics, aerospace , laser, photoelectric and other high-tech fields. [0003] However, traditional polyimide films, such as the KAPTON film produced by the American DUPONT company and the domestic H film, have a molecular structure of pyromellitic dianhydride, that is, the main monomer raw material is pyromellitic acid di Anhydride and 4,4'-diaminodiphenyl ether have low transmittance of visible light (wavelength 400nm-700nm), a large amount of absorption occurs at a wavelength of 500nm, and it is absorbed by 100...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10G02B1/04G02B23/00G02F1/1337G02F1/361
Inventor 虞鑫海阿尔斯兰·麦麦提敏
Owner DONGHUA UNIV
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