Full aromatic fluorine containing transparent polyimide film and preparation method thereof

A transparent polyimide and transparent film technology, which is applied in the field of all-aromatic fluorine-containing colorless transparent polyimide film and its preparation, can solve the problem that it is difficult to prepare high-molecular-weight polyimide resin, which has not yet been published The literature or patent reports, the decline of the comprehensive performance of film products and other problems, achieve the effect of excellent dimensional stability, low cost, and fewer types of use

Inactive Publication Date: 2009-12-09
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 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.
[0015] 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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  • Full aromatic fluorine containing transparent polyimide film and preparation method thereof
  • Full aromatic fluorine containing transparent polyimide film and preparation method thereof
  • Full aromatic fluorine containing transparent polyimide film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] 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 placed Put it into the reaction kettle, stir, after it is completely dissolved, cool it to below 5°C in an ice-water bath, add 52.0 g (0.1 mole) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propane The dianhydride (BPADA) was stirred in the temperature range of 5°C-10°C, and after being completely dissolved, the reaction was maintained for 3 hours to obtain a homogeneous, transparent and viscous fluorine-containing aromatic polyamic acid solution.

[0069] Use N,N-dimethylacetamide solvent to adjust the viscosity of the polyamic acid solution to make it between 100 seconds and 110 seconds (viscosity cup No. 4), form a film in a casting machine, and heat up to remove Remove the organic solvent (recycle and reuse), carry out dehydration thermal imidization reaction, cool and remove the film to obtain a tough and transparent colorless ...

Embodiment 2

[0075] 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 reactor, stirred and completely dissolved After that, the ice water bath was cooled to below 5°C, 62.0 g (0.2 mol) of 3,3',4,4'-tetracarboxydiphenyl ether dianhydride (ODPA) was added, and the temperature was stirred in the range of 5°C to 10°C. , after the complete dissolution, the reaction was maintained for 3 hours to obtain a homogeneous transparent and viscous fluorine-containing aromatic polyamic acid solution.

[0076] Use N-methyl-2-pyrrolidone solvent to adjust the viscosity of the polyamic acid solution to make it between 100 seconds and 110 seconds (viscosity cup No. 4), form a film in a casting machine, and heat up to remove Organic solvent (recycled and reused) and dehydration thermal imidization reac...

Embodiment 3

[0081] 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,N-dimethylformamide were put into the reactor, stirred, and completely After dissolving, the ice-water bath was cooled to below 5°C, and 104.1 g (0.2 mol) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propane dianhydride (BPADA) was added to the solution at 5 Stir in the temperature range of ℃-10 ℃, after the complete dissolution, the reaction is maintained for 3 hours to obtain a homogeneous transparent and viscous fluorine-containing aromatic polyamic acid solution.

[0082]Use N,N-dimethylformamide solvent to adjust the viscosity of the polyamic acid solution to make it between 100 seconds and 110 seconds (viscosity cup No. 4), form a film in a casting machine, and heat up to remove Remove the organic solvent (recycle and reuse), carry out dehydration t...

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Abstract

The invention relates to a full aromatic fluorine containing transparent polyimide film. Structural formula of molecule thereof is shown above, wherein -R1 is a divalent residue of fluorine containing aromatic binary primary amine, and -R2 is a divalent connecting group of aromatic binary anhydride molecule. The preparation method thereof comprises steps of adding the fluorine containing aromatic binary primary amine and strongly polar non-protonic organic solvent into a polymerizing bottle, stirring at room temperature, after being completely dissolved, adding the aromatic binary anhydride, stirring, after 3 hours reaction, obtaining transparent and thick fluorine containing aromatic polyamide acid resin solution having homogeneous phase; and using the strongly polar non-protonic organic solvent to regulate viscosity of the fluorine containing aromatic polyamide acid resin solution, forming film, heating, carrying out dehydrating hot-imidization reaction, cooling, demoulding, thus obtaining the full aromatic fluorine containing transparent polyimide film. The preparation method has mild reaction condition, simple operation and low cost and is environment friendly. The full aromatic fluorine containing transparent polyimide film has excellent mechanical property and heat tolerance and visible light transmission thereof is up to 95%.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to a fully aromatic fluorine-containing colorless 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, optoelectronics and other high-tech fields. [0003] However, traditional polyimide films, such as the KAPTON film produced by DUPONT in the United States and the domestic H film, have a molecular structure of the pyromellitic dianhydride type, that is, the main monomer raw material is pyromellitic acid Anhydride and 4,4'-diaminodiphenyl ether have low transmittance of visible light (wavelength 400nm-700nm), and a large amount of absor...

Claims

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Application Information

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