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All-aromatic fluorine-containing colorless transparent polyimide film and preparation method thereof

A technology of transparent polyimide and transparent film, which is applied in the field of fully aromatic fluorine-containing colorless transparent polyimide film and its preparation, can solve the problem that it is difficult to obtain high molecular weight polyimide resin, which has not yet been disclosed. The problems such as the literature or patent reports, and the decline of the comprehensive performance of the film products, achieve the effects of excellent dimensional stability, low cost, and convenient source.

Inactive Publication Date: 2012-02-01
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 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.
[0012] The molecular structure and preparation method of the all-aromatic fluorine-containing colorless transparent polyimide film disclosed by the present invention have not yet been published in the literature or patent reports

Method used

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  • All-aromatic fluorine-containing colorless transparent polyimide film and preparation method thereof
  • All-aromatic fluorine-containing colorless transparent polyimide film and preparation method thereof
  • All-aromatic fluorine-containing colorless transparent polyimide film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] At room temperature, 42.8 g (0.1 mol) of 1,3-bis(2-trifluoromethyl-4-aminophenoxy)benzene (DARes-2TF) and 285 ml of N,N-dimethylacetamide were put Put it into the reaction kettle, stir, after completely dissolving, cool in an ice-water bath to below 5°C, add 52.0 g (0.1 moles) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propane Dianhydride (BPADA), stirred at a temperature range of 5°C-10°C, and after being completely dissolved, the reaction was maintained for 3 hours to obtain a homogeneous transparent viscous fluorine-containing aromatic polyamic acid solution.

[0065] Use N,N-dimethylacetamide solvent to adjust the viscosity of the polyamic acid solution so that it is between 100 seconds and 110 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Remove the organic solvent (recycle and reuse) and carry out dehydration thermal imidization reaction, cooling, and stripping to obtain a tough and transparent colorless all-aromatic fluorin...

Embodiment 2

[0071] At room temperature, 42.8 g (0.1 mol) of 1,3-bis(2-trifluoromethyl-4-aminophenoxy)benzene (DARes-2TF), 65.4 g (0.1 mol) of 2,2-bis [4-(2-Trifluoromethyl-4-aminophenoxy)phenyl]hexafluoropropane (BAPFP-2TF) and 850 ml of N-methyl-2-pyrrolidone were put into the reaction kettle, stirred and dissolved completely Finally, the ice-water bath was cooled to below 5°C, and 62.0 grams (0.2 moles) of 3,3',4,4'-tetracarboxydiphenyl ether dianhydride (ODPA) was added, and stirred within the temperature range of 5°C-10°C After completely dissolving, the reaction was maintained for 3 hours to obtain a homogeneous transparent viscous fluorine-containing aromatic polyamic acid solution.

[0072] Use N-methyl-2-pyrrolidone solvent to adjust the viscosity of the polyamic acid solution so that it is between 100 seconds and 110 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Organic solvent (recycling) and thermal imidization reaction for dehydration,...

Embodiment 3

[0077] At room temperature, 42.8 g (0.1 mol) of 1,3-bis(2-trifluoromethyl-4-aminophenoxy)benzene (DARes-2TF), 65.4 g (0.1 mol) of 2,2-bis [4-(2-trifluoromethyl-4-aminophenoxy)phenyl]hexafluoropropane (BAPFP-2TF) and 850 milliliters of N,N-dimethylformamide were put into the reaction kettle, stirred, completely After dissolving, the ice-water bath was cooled to below 5°C, and 104.1 grams (0.2 moles) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propanedianhydride (BPADA) (BPADA) was added in 5 Stir in the temperature range of ℃-10 ℃, after completely dissolving, keep the reaction for 3 hours to obtain a homogeneous transparent viscous fluorine-containing aromatic polyamic acid solution.

[0078] Utilize N,N-dimethylformamide solvent to adjust the viscosity of the polyamic acid solution so that it is between 100 seconds and 110 seconds (No. 4 viscosity cup), form a film in a casting machine, and heat up to remove Remove the organic solvent (recycle and reuse) and carry out dehydrat...

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Abstract

The invention relates to a fully aromatic fluorine-containing colorless transparent polyimide film, the general formula of its molecular structure is as shown in the figure: wherein: -R 1- is a divalent residue of a fluorine-containing aromatic dibasic primary amine, -R 2- is a divalent linking group of an aromatic dibasic acid anhydride molecule; its preparation includes: adding a fluorine-containing aromatic dibasic primary amine and a strong polar aprotic organic solvent into a polymerization bottle, stirring at room temperature, and after completely dissolving , adding the aromatic dibasic acid anhydride, stirring, and reacting for 3 hours to obtain a homogeneous, transparent and viscous fluorine-containing aromatic polyamic acid resin solution; adjust the above-mentioned fluorine-containing aromatic polyamic acid with a strong polar aprotic organic solvent. The viscosity of the amic acid resin solution is obtained by forming a film, heating, dehydrating thermal imidization reaction, cooling, and removing the film. The preparation method has mild reaction conditions, simple operation, low cost and environmental friendliness; and the fully aromatic fluorine-containing colorless transparent polyimide film has excellent mechanical properties and heat resistance, and its visible light transmittance is as high as 95%.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to an all-aromatic fluorine-containing colorless and transparent polyimide film and a preparation method thereof. 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 occ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10
Inventor 虞鑫海
Owner DONGHUA UNIV