Matte insulating polyimide black film and preparation method thereof

A technology of polyimide and polyimide powder, which is applied in the field of matte insulating polyimide black film and its preparation, can solve the problems of limited effect, poor compatibility between carbon black and polyimide system, etc. Achieve performance improvement, good appearance, and good affinity

Pending Publication Date: 2021-09-17
ANHUI GUOFENG PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN105482115B uses non-conductive carbon black to reflux through concentrated sulfuric acid for 2 hours to make its surface modified and grafted with -COOH, and uses a silane coupling agent to improve the affinity of carbon black and polyimide, improving the carbon black in the The dispersion effect in polyimide, but when the carbon black is added in a large proportion (such as the preparation of ultra-thin polyimide black film), the effect of this method is relatively limited
Chinese patent CN103160123B uses polyimide powder with an average particle size of 0.5-15 μm as a matting agent. Compared with known inorganic matting agents, it has high insulation and has a high affinity with polyimide systems. However, the problem of poor compatibility between carbon black and polyimide systems as an opacifying agent has not been resolved.

Method used

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  • Matte insulating polyimide black film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Preparation of silane coupling agent modified polyimide powder:

[0047] (a), under a nitrogen atmosphere, dissolve 0.5mol ODA in a DMF solvent, then add 0.525mol PMDA, stir and react at 20°C for 3h, to obtain a polyamic acid solution with a solid content of 1%wt and excess anhydride;

[0048] (b) Add 0.1mol N-β-(aminoethyl)-γ-aminopropyl-trimethoxysilane to the polyamic acid solution with excess anhydride, stir and react at 60°C for 12h, then add 1mol ethyl Anhydride and 0.75mol isoquinoline were stirred and reacted at 80°C for 12h. After the reaction was completed, the reaction system was kept at 130°C for 10h, cooled, filtered, and the obtained solid matter was washed 3 times with ethanol solution and dried in vacuum Dry it in an oven at 100°C for 12 hours, and grind it to an average particle size of 3 μm.

[0049] Preparation of carbon black slurry:

[0050] Add blue phase channel carbon black with a primary particle size of 20nm into the DMF solvent, use a high-spe...

Embodiment 2

[0056] Preparation of silane coupling agent modified polyimide powder:

[0057] (a), under a nitrogen atmosphere, dissolve 0.5mol PDA in DMAc solvent, then add 0.55mol PMDA, stir and react at 25°C for 2h, to obtain a polyamic acid solution with a solid content of 1wt% and excess anhydride;

[0058] (b) Add 0.125mol N-β-(aminoethyl)-γ-aminopropyl-triethoxysilane to the polyamic acid solution with excess anhydride, stir and react at 60°C for 12h, then add 1.25 mol acetic anhydride and 1mol isoquinoline, stirred and reacted at 80°C for 12h, after the reaction was completed, the reaction system was kept at 130°C for 10h, cooled, filtered, and the obtained solid matter was washed 3 times with ethanol solution, and placed in a vacuum Dry in a drying oven at 100°C for 12 hours, and pulverize until the average particle size is 3 μm.

[0059] Preparation of carbon black slurry:

[0060] Add blue phase channel carbon black with a primary particle size of 30nm into the DMF solvent, use...

Embodiment 3

[0066] Preparation of silane coupling agent modified polyimide powder:

[0067] (a) Under a nitrogen atmosphere, dissolve 0.4mol ODA and 0.1mol PDA in NMP solvent, then add 0.55mol BPDA, stir and react at 25°C for 2h, and obtain a polyamic acid with an anhydride excess of 3wt% solid content solution;

[0068] (b) Add 0.125mol N-β-(aminoethyl)-γ-aminopropyl-methyldimethoxysilane to the polyamic acid solution with excess anhydride, stir and react at 70°C for 10h, and then Add 1.25mol acetic anhydride and 1mol isoquinoline, stir and react at 90°C for 10h, after the reaction is complete, keep the reaction system at 140°C for 8h, cool, filter, and wash the obtained solid matter with ethanol solution 3 times, place Dry it in a vacuum oven at 100°C for 12 hours, and grind it to an average particle size of 4 μm.

[0069] Preparation of carbon black slurry:

[0070] Add blue phase channel carbon black with a primary particle size of 30nm into DMAc solvent, use a high-speed shear dis...

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Abstract

The invention discloses a preparation method of a matte insulating polyimide black film, which comprises the following steps: S1, in an inert atmosphere, reacting an aromatic dianhydride with an aromatic diamine of which the molar weight is excessive relative to that of the aromatic dianhydride in an aprotic polar solvent to obtain a polyamide acid solution of which the amine is excessive; s2, adding silane coupling agent modified polyimide powder and carbon black color paste into the polyamide acid solution with excessive amine, uniformly dispersing, and then adding an aromatic dianhydride for reaction to obtain a polyamide acid mixed solution; s3, subjecting the polyamide acid mixed solution to film forming and imidization, and obtaining the matte insulating polyimide black film. The polyimide black film prepared by the method has the characteristics of good appearance, low glossiness, high insulating strength and the like, and the tensile strength, the elongation at break, the thermal shrinkage rate and other properties of the polyimide black film are improved.

Description

technical field [0001] The invention relates to the technical field of film preparation, in particular to a matte insulating polyimide black film and a preparation method thereof. Background technique [0002] Polyimide film is widely used as the base material or cover film material of flexible circuit boards due to its excellent heat resistance, excellent insulation properties and mechanical properties. However, the traditional polyimide film has high transparency and high gloss. During the application process, glare or astigmatism caused by light reflection will occur. In addition, there is also the problem that the circuit design distribution may be interpreted and copied by competitors. In order to solve the above problems, matte polyimide black film came into being, which has the characteristics of low light transmittance and low gloss. Low light transmittance can cover the electronic circuits covered by it to prevent reverse engineering; low gloss can solve the proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10C08K3/04
CPCC08J5/18C08G73/1071C08G73/1067C08G73/1042C08J2379/08C08K3/04
Inventor 孙善卫史恩台方超潘成陈铸红
Owner ANHUI GUOFENG PLASTIC
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