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Matte polyimide black film with low heat shrinkage rate, and preparation method thereof

A technology of polyimide and shrinkage rate, which is applied in the field of low thermal shrinkage matte polyimide black film and its preparation, can solve the problem of uneven dispersion of matting agent particle agglomeration, poor storage stability of slurry, low solid content, etc. problems, to achieve the effect of good dimensional stability, low visible light transmittance, and low surface gloss

Active Publication Date: 2020-02-21
ANHUI GUOFENG PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is glare or astigmatism caused by light reflection on the surface of traditional bright polyimide black film, which causes visual discomfort and makes eyes tired when watching for a long time. Therefore, in recent years, matte film with better shielding effect and better appearance Polyimide black film has gradually become the focus of the cover film market, and the black film with a gloss range of 25-60GU is usually called matte polyimide black film
[0004] At present, the thermal shrinkage range of the black film used for conventional cover films in the market is ≤0.15%. For customers with higher requirements, the black film cannot be well applied
In the traditional black polyimide black film preparation process, the carbon black slurry is mainly prepared by ultrasonic dispersion or high-speed dispersion with a solvent and a coupling agent. The storage stability of the slurry is poor and the solid content is low.
[0005] In addition, for the matte black film, the current method of adding matting agent is mainly to mix the matting agent with the solvent through high-speed dispersion, and then disperse it with the synthesized resin in the form of dispersion liquid. The viscosity of the resin solution is quite different, and it is inevitable that there will be uneven dispersion and agglomeration of matting agent particles when mixing again, which will affect various properties of film products.

Method used

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  • Matte polyimide black film with low heat shrinkage rate, and preparation method thereof
  • Matte polyimide black film with low heat shrinkage rate, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A kind of preparation method of low heat shrinkage matte polyimide black film, comprises the steps:

[0052] S1. Preparation of polyamic acid resin solution: In nitrogen atmosphere, add 2.47kg of 3,3-4,4-diaminodiphenyl ether and 0.82kg of p-phenylenediamine to 40kg of N,N'-dimethylacetamide Dissolved to obtain an aromatic diamine solution; add 0.56 kg of coupling agent-modified silica with an average particle size of 4 μm to the aromatic diamine solution and mix evenly, then add 3.78 kg of pyromellitic dianhydride at a uniform speed for 10 times, Stirring and reacting at 40° C. for 4 h to obtain a polyamic acid resin solution, wherein the solid content of the polyamic acid resin solution is 15 wt %;

[0053]S2. Preparation of black slurry: Dilute 1.44 kg of the polyamic acid resin solution obtained in S1 with N,N'-dimethylacetamide to a solid content of 5 wt% to obtain solution A, and add 0.09 kg of polyurethane under high-speed stirring Mix with similar dispersants, ...

Embodiment 2

[0057] A kind of preparation method of low thermal shrinkage matte polyimide black film, comprises the steps:

[0058] S1. Preparation of polyamic acid resin solution: In a nitrogen atmosphere, add 3.64kg of 3,3-4,4-diaminodiphenyl ether and 0.85kg of 2,5-dimethylacetamide to 45kg of N,N'-dimethylacetamide Dissolve aminotoluene to obtain an aromatic diamine solution; add 0.4 kg of coupling agent-modified aluminum oxide with an average particle size of 4 μm to the aromatic diamine solution, mix well, and then add 4.68 kg of pyromellitic acid at a uniform speed for 12 times Dianhydride, stirring and reacting at 45° C. for 6 hours to obtain a polyamic acid resin solution, wherein the solid content of the polyamic acid resin solution is 16.9 wt %;

[0059] S2. Preparation of black slurry: Dilute 1.28kg of the polyamic acid resin solution obtained in S1 with N,N'-dimethylacetamide to a solid content of 6wt% to obtain solution A, and add 0.14kg of polyurethane under high-speed stirr...

Embodiment 3

[0063] A kind of preparation method of low thermal shrinkage matte polyimide black film, comprises the steps:

[0064] S1. Preparation of polyamic acid resin solution: In a nitrogen atmosphere, add 3.77kg of 3,3-4, 4-diaminodiphenyl ether and 0.62kg of p-phenylenediamine are dissolved to obtain an aromatic diamine solution; adding 0.53kg of an average particle diameter to the aromatic diamine solution is a coupling agent modified silica of 6 μm and mixes evenly, and then Add 0.62kg of 3,3'-4,4'-biphenyltetracarboxylic dianhydride and 3.85kg of pyromellitic dianhydride in 12 times at a uniform speed (the 3,3'-4,4'-biphenyltetracarboxylic dianhydride is added first in order) acid dianhydride), stirred and reacted at 50°C for 5h to obtain a polyamic acid resin solution, wherein the solid content of the polyamic acid resin solution was 18wt%;

[0065] S2. Preparation of black slurry: Dilute 2.01 kg of the polyamic acid resin solution obtained in S1 with N,N'-dimethylformamide to ...

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Abstract

The invention discloses a preparation method of a matte polyimide black film with a low heat shrinkage rate. The method comprises the following steps: S1, preparing a polyamide acid resin solution: adding a matting agent into an aromatic diamine solution in an inert gas atmosphere, mixing until uniformity, adding aromatic dianhydride, and carrying out a stirring reaction to obtain the polyamide acid resin solution, wherein the aromatic diamine contains rigid aromatic diamine, and the rigid aromatic diamine is at least one of p-phenylenediamine, 2,5-diaminotoluene, 1,5-naphthalenediamine, 2,5-naphthalenediamine and 2,6-naphthalenediamine; S2, preparing a black slurry; and S3, preparing the matte polyimide black film with the low heat shrinkage rate. The invention further discloses the mattepolyimide black film with the low heat shrinkage rate. The matte polyimide black film with the low heat shrinkage rate is prepared through the preparation method of the matte polyimide black film with the low heat shrinkage rate. The matte polyimide black film with the low heat shrinkage rate has the advantages of low shrinkage rate, matt effect, maintenance of mechanical properties and electrical properties, good dimensional stability, low visible light transmittance and low surface gloss.

Description

technical field [0001] The invention relates to the technical field of polyimide films, in particular to a low heat shrinkage matte polyimide black film and a preparation method thereof. Background technique [0002] Polyimide films are widely used in electrical, electronics, aerospace and other fields due to their excellent mechanical, thermal and electrical properties. Electronic-grade polyimide cover film is mainly used to protect flexible printed circuit boards. Due to the needs of various processing processes such as downstream glue coating and etching, the dimensional stability of the cover film is required to be high. [0003] Because of its opacity, black PI film can cover electronic materials such as flexible circuits, electronic components, and lead frames of integrated circuit packages to prevent visual inspection, tampering, and plagiarism, and the market demand is high. There is glare or astigmatism caused by light reflection on the surface of traditional brigh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08K9/06C08K3/36C08K3/22C08K3/04C08G73/10
CPCC08J5/18C08G73/1071C08G73/1042C08G73/105C08K2003/2227C08K2201/011C08J2379/08C08K9/06C08K3/36C08K3/04
Inventor 江朝阳
Owner ANHUI GUOFENG PLASTIC
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