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Colorless transparent polyimide composite film and its production method

一种聚酰亚胺、复合薄膜的技术，应用在该复合薄膜的制备领域，能够解决不能适用、薄膜不良表面平滑度、薄膜不良可塑性等问题，达到优良耐热性和机械性能的效果

Active Publication Date: 2009-08-19
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, this production method is prone to the following problems: layered silicate can migrate in the resin due to the high fluidity of the resin resulting from high-temperature imidization reaction, resulting in aggregation of layered silicate and insufficient transparency of the film
Thus, this method causes problems that the resulting film tends to exhibit poor surface smoothness due to the formation of white spots, blemishes, etc. on the surface of the film, the resulting film exhibits poor plasticity and the thickness of the film is difficult to control
Furthermore, disadvantageously, the film cannot be used in optical devices that require a colorless and transparent film because polyimide itself has a maroon color
[0009] Similar to the case of the composite material described in Patent Document 1, the composite material explicitly described in Patent Document 2, that is, a composite material using a polyimide formed from an aromatic tetracarboxylic anhydride cannot exhibit sufficient water vapor barrier sex

Method used

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  • Colorless transparent polyimide composite film and its production method
  • Colorless transparent polyimide composite film and its production method
  • Colorless transparent polyimide composite film and its production method

Examples

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preparation example Construction

[0038] The colorless transparent polyimide composite film of the present invention contains the polyimide (A) that has the repeating unit represented by formula (1) and by treating with the organic onium ion represented by formula (2) or (3) The obtained organically treated layered silicate (B). The preparation method of the colorless and transparent polyimide composite film of the present invention comprises: by the layered silicate (B) that contains polyimide (A), organic treatment and have the organic solvent (C) of specific SP value The three-component liquid mixture of is extruded or applied on a carrier to form a film-form mixture; the organic solvent (C) is subsequently removed from the film-form mixture.

[0039] The polyimide (A) having a repeating unit represented by formula (1) used in the present invention is obtained by a reaction between an aliphatic tetracarboxylic acid or a derivative thereof and a diamine.

[0040] Examples of the aliphatic tetracarboxylic ac...

Embodiment

[0088] The present invention will be described in detail below by means of examples, and it should not be understood that the present invention is limited to these examples.

[0089] The physical properties of polyimides, two-component liquid mixtures (each containing an organically treated layered silicate and an organic solvent) and polyimide composite films obtained in Examples and Comparative Examples were measured by the following methods .

[0090] Evaluation method of polyimide

[0091]

[0092] Polyimide (0.1 g) was dissolved in N-methyl-2-pyrrolidone (20 ml), and at 30° C., the inherent viscosity of polyimide was measured by a Canon-Fenske viscometer . The inherent viscosity (μ) was calculated by using the following formula.

[0093] μ=[ln(t s / t o )] / C

[0094] t o : Solvent flow time

[0095] t s : dilute polymer solution flow time

[0096] C: 0.5 g / dl

[0097]

[0098]

[0099] The turbidity of a two-component liquid mixture containing an organical...

preparation Embodiment 1

[0114]

[0115] Oxydianiline (20.12 g, 0.1 mol) and an organic solvent, namely, γ-butyrolactone (51.65 g) with an SP value of 12.6 and N, N-dimethylacetamide (12.92 g) with an SP value of 10.8 ) into a 500-milliliter five-neck flask equipped with a thermometer, a stirrer, a nitrogen introduction tube and a condenser with a fractionator, followed by dissolving oxydianiline in an organic solvent. The solution obtained above was cooled to 5°C by means of an ice-water bath. While keeping the solution at the same temperature as above, 1,2,4,5-cyclohexanetetracarboxylic dianhydride (22.62 g, 0.1 mol) and triethylamine (0.50 g , 0.005 mol) were added to the above solution together. After the addition was complete, the resulting mixture was heated to 180°C and refluxed for three hours, the distillate was removed if necessary, then heated to 200°C to complete the reaction. After air cooling until the internal temperature was 100°C, N,N-dimethylacetamide (107.6 g) serving as a dilue...

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Abstract

The present invention provides a colorless and transparent polyimide composite film containing polyimide (A) having a specific repeating unit and an organically treated layered film obtained by treating with an organic onium ion having a specific structure. Silicate (B), so that the layered silicate (B) of described organic treatment is dispersed in polyimide (A); Also provide the preparation method of colorless and transparent polyimide composite film, The process involves forming on a support a three-component liquid mixture comprising polyimide (A), organically treated layered silicate (B) and an organic solvent (C) with a specific SP value The mixture in the form of a film; the organic solvent (C) is subsequently removed from the mixture in the form of a film. The polyimide composite film of the present invention is a colorless transparent film containing polyimide (A) and an organically-treated layered silicate (B) dispersed very uniformly in polyimide, which exhibits It has excellent heat resistance and mechanical properties and exhibits flexibility.

Description

technical field [0001] The present invention relates to a colorless and transparent polyimide composite film containing layered silicate (hereinafter referred to as "layered silicate") treated with organic onium ions having a specific structure, and to a method for preparing the composite film . Background technique [0002] A polyimide resin is a heat-resistant resin generally obtained by cyclizing a polyamic acid synthesized by a condensation reaction of an aromatic tetracarboxylic anhydride and an aromatic diamine. Due to its molecular chain rigidity, resonance stability, and strong chemical bonds, polyimide resins exhibit excellent thermal decomposition resistance, high resistance to chemical changes (eg, oxidation or hydrolysis), and excellent mechanical and electrical properties. In addition, polyimide resins also exhibit flexibility. Thus, polyimide resins have been widely used as films, coating agents, molded parts, and insulating materials in, for example, electri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08J5/18C08K3/34C08K9/04
CPCC08J3/205Y10T428/31721C08J5/18C08J3/212C08J2379/08C08L79/08C08K9/04C08J3/215
Inventor 牧野嶋高史木原秀太
Owner MITSUBISHI GAS CHEM CO INC
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