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Method for preparing matt black polyimide film

A black polyimide film preparation technology, applied in the field of polyimide film manufacturing, can solve the problems of reducing the mechanical properties of PI film, uneven melting, complicated manufacturing process, etc., to eliminate the internal stress of the film and enhance the tear resistance Crack performance, surface quality improvement effect

Inactive Publication Date: 2018-04-27
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the chemical conversion temperature must exceed 250°C during the preparation of polyimide films, none of the above organic compounds can withstand temperatures of 250°C or higher.
When such organic compounds are added to the polyimide film as a matting agent, it will cause defects such as cracks or holes in the film, or uneven color spots due to uneven melting
[0009] At present, the main production technology of matte black PI film is divided into two categories: one is to add black pigment and matting agent filler to PI resin, and then undergo chemical imidization or thermal imidization to synthesize a film with low light transmittance and Low-gloss PI film, this method is easy to operate and the effect is obvious, but due to the addition of a large amount of fillers, the mechanical properties of the PI film are greatly reduced; the other is to coat one or both sides of the PI base film Coated with a PI film containing black pigment and matting effect
Though this kind of method can make polyimide film present desired black effect preferably, and can guarantee the certain mechanical performance of polyimide film, but the black resin of additional coating usually increases manufacturing process and cost, and Detrimental effect on the properties of polyimide film
In addition, polyimide films are prone to performance degradation when exposed to thermal stress due to the poor heat resistance of the resin coating layer
There are many patent applications related to the manufacture of low-gloss black polyimide films, but they are difficult to implement due to defects such as complex manufacturing processes, high production control precision requirements, and high manufacturing costs.

Method used

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  • Method for preparing matt black polyimide film
  • Method for preparing matt black polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Ⅰ. Preparation of polyamic acid resin solution

[0050] In a nitrogen atmosphere, the temperature of the synthesis system is controlled to be 12°C, and 2.39 kg of aromatic diamine 4,4'-diaminodiphenyl ether (4,4 '-ODA) was stirred and dissolved. After 4,4'-ODA was completely dissolved, 2.61kg of aromatic dianhydride pyromellitic acid diacid (PMDA) was added at a constant speed in 8 times at a molar ratio of 1:1 to the aromatic diamine. , and stirred at 1200r / min, synthesized by polycondensation reaction for 12h to obtain a polyamic acid resin solution with a solid content of M=5kg, that is, a solid content ratio of 10wt%;

[0051] Ⅱ. Black slurry preparation

[0052] According to the 20wt% of the solid content M in the polyamic acid resin solution gained in step 1, get carbon black 1kg and add solvent N, N'-dimethylacetamide (DMAC) 2kg, mix and stir to obtain carbon black content 30% black Slurry; the average particle size of carbon black in this example is 0.01 μm. ...

Embodiment 2

[0064] Ⅰ. Preparation of polyamic acid resin solution

[0065] In a nitrogen atmosphere, control the temperature of the synthesis system at 22°C, add 6.38kg of aromatic diamine 2,2'-bis(trifluoromethyl)benzidine to 37.5kg of N,N'-dialkylcarboxamide solvent and stir Dissolve, after it is completely dissolved, add 5.99 kg of aromatic dianhydride 3,3',4,4'-biphenyl tetracarboxylic acid dianhydride (BPDA ), and stirred at 1000r / min, synthesized by polycondensation reaction for 8h to obtain a polyamic acid resin solution with a solid content of M=12.4kg, that is, a solid content ratio of 25wt%;

[0066] Ⅱ. Black slurry preparation

[0067] 16wt% of the solid content M in the polyamic acid resin solution obtained by step 1 gets iron black 2kg and adds solvent N, mixes and stirs in 18kg of N'-dimethylsulfoxide (DMSO) and obtains the black slurry of iron black content 10%. Material; the average particle size of iron black in this example is 0.8 μm.

[0068] The mixing and stirring ...

Embodiment 3

[0077] Ⅰ. Preparation of polyamic acid resin solution

[0078] In a nitrogen atmosphere, the temperature of the synthesis system is controlled at 50°C, and 7.92kg of aromatic diamine 3,4'-diaminodiphenyl ether (3,4'-ODA) is added to 25kg of N-methylpyrrolidone (NMP) solvent to carry out Stir to dissolve, and after it is completely dissolved, add 17.23 kg of aromatic dianhydride 2,2-bis(3,4-dicarboxylic acid phenyl)hexafluoro at a uniform speed of 5 times at a molar ratio of 1.02:1 to the aromatic diamine Propane dianhydride (6FDA), stirred at 1000r / min, synthesized by polycondensation for 8 hours to obtain a solid content M = 25.15kg, that is, a polyamic acid resin solution with a solid content ratio of 50wt%;

[0079] Ⅱ. Black slurry preparation

[0080] 4wt% of the solid content M in the polyamic acid resin solution obtained by step 1 gets acetylene black 1kg and adds in solvent N-methylpyrrolidone (NMP) 5.6kg and mixes and stirs to obtain the black slurry of acetylene blac...

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Abstract

The invention discloses a method for preparing a matt black polyimide film. The method comprises I, preparing a polyamic acid resin solution through a conventional method, II, preparing black slurry of which the use amount is 2-20 wt% the solid content M of the polyamic acid resin solution, III, preparing a matting agent dispersion liquid of which the use amount is 2-20wt% M, IV, preparing a black polyamic acid resin solution through blending the polyamic acid resin solution, the black slurry and the matting agent dispersion liquid through stirring, and carrying out defoaming for next use, and V, carrying out curtain coating, drawing, imidization and setting on the black polyamic acid resin solution through conventional processes, wherein after biaxial drawing, imidization or setting, thefilm is subjected to surface treatment at a high temperature of 640-800 DEG C for 5-120s so that the matt black polyimide film is obtained. The black pigment and the matting agent have moderate average particle sizes. In the resin solution curtain coating, the high temperature surface treatment is used. The film has improved light transmittance, gloss and physical and mechanical properties.

Description

technical field [0001] The invention relates to a polyimide film manufacturing technology, in particular to a method for preparing a matte black polyimide film. Background technique [0002] Flexible printed circuit board (FPC) is widely used in 3C products, optical lens modules, liquid crystal display (LCD) modules and solar cells and other products, and polyimide film (Polyimide Film, referred to as PI film) is often used as its substrate Or cover film material, due to the high surface flatness of the traditional PI film in the application process, the surface of the film reflects most of the incident light and produces high gloss. The high-gloss film surface has glare or astigmatism caused by light reflection, which causes visual discomfort and easily fatigues the eyes when watching for a long time. Especially for high-gloss PI film polyimide films with black, white, blue, red and other colors, the reflected light on the surface has a more significant impact on vision. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J7/00C08L79/08C08K3/04C08K3/36C08K3/22C08G73/10
CPCC08J5/18C08G73/1039C08G73/105C08G73/1064C08G73/1067C08G73/1071C08J7/08C08J2379/08C08K3/04C08K3/36C08K2003/2227C08K2003/2237C08K2003/2241C08K2201/003
Inventor 任小龙蒋耿杰冯羽风马纪翔
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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