Preparation method of black polyimide thin film with matte surface

A black polyimide film preparation technology, applied in the field of polyimide film manufacturing, can solve problems such as low gloss, increased manufacturing process and cost, and complicated manufacturing process, so as to enhance tear resistance and reduce replacement The effect of increasing the number of times and improving the filtration efficiency

Inactive Publication Date: 2018-05-04
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the content is large, the problem of uneven dispersion of additives will also occur; adding a large amount of matting agent will also lead to deterioration of the performance of the polyimide film, easy to be brittle, and a large amount of additives are prone to sedimentation and agglomeration in the polyamic acid resin. It will also increase the production cost of the film
[0008] At present, the main production technology of black low-gloss 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 number of fillers, the mechanical properties of the PI film are greatly reduced; the other type is on one or both sides of the PI base film Apply a layer of PI film with 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
In the early days, some people tried to directly prepare black and low-gloss PI membranes by using pigments with micron-sized and large particle sizes, but the pigments with larger particles easily blocked the filtration system, resulting in the inability to continuously form membranes, so they had to give up trying
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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  • Preparation method of black polyimide thin film with matte surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Ⅰ. Preparation of polyamic acid resin solution

[0036] In a nitrogen atmosphere, the temperature of the synthesis system is controlled to be 22°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 M=5kg, that is, a solid content ratio of 10wt%;

[0037] Ⅱ. Black slurry preparation

[0038] 20wt% of the solid content M in the polyamic acid resin solution gained by step 1 gets carbon black 1kg and adds solvent N, N'-dimethylacetamide (DMAC) 2.33kg and mixes and stirs to obtain carbon black content 30% Black slurry; the average particle size of carbon black in this example is 0.01 μm.

[0039] T...

Embodiment 2

[0046] Ⅰ. Preparation of polyamic acid resin solution

[0047] 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=12.40kg, that is, a solid content ratio of 25wt%;

[0048] Ⅱ. Black slurry preparation

[0049] According to the 16wt% of the solid content M in the polyamic acid resin solution gained in step 1, get iron black 2kg and add solvent N, mix and stir in 18kg of N'-dimethyl sulfoxide (DMSO) to obtain iron black content 10% black Slurry; the average particle size of iron black in this example is 0.8 μm.

[0050] The mixing and stirring after ...

Embodiment 3

[0056] Ⅰ. Preparation of polyamic acid resin solution

[0057] In a nitrogen atmosphere, the temperature of the synthesis system is controlled at 60°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), and stirred at 1000r / min, synthesized by polycondensation for 8h to obtain a solid content M = 25.15kg, that is, a solid content ratio of 50wt% polyamic acid resin solution;

[0058] Ⅱ. Black slurry preparation

[0059] 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 black conten...

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Abstract

The invention provides a preparation method of a black polyimide thin film with a matte surface. The preparation method comprises the following main steps: I, preparing a polyamic acid resin solutionaccording to a conventional method; II, preparing black slurry, wherein the amount of a black pigment is 2 to 20 weight percent of solid content M in the polyamic acid resin solution; III, preparing ablack polyamic acid resin solution; blending and stirring the polyamic acid resin solution, the black slurry and an agglomeration agent, and de-foaming for later use; IV, after enabling the black polyamic acid solution to pass through a filtering system, treating a conveying pipeline through a magnetic field or ultrasonic waves; finishing magnetic field and ultrasonic agglomeration treatment on the resin solution; then conventionally preparing the black polyimide thin film with the matte surface. According to the preparation method provided by the invention, the average grain diameter of theblack pigment is 0.01 to 0.8mu m; the agglomeration agent is added in a polyamic acid resin condensation polymerization synthesis process; the light transmittance, the glossiness and the physical andmechanical properties of the thin film are remarkably improved.

Description

technical field [0001] The invention relates to a polyimide film manufacturing technology, in particular to a method for preparing a black polyimide film with a matte surface. 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 impa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08L33/26C08L71/02C08L79/02C08L23/06C08J5/18C08G73/10
CPCC08J5/18C08G73/1007C08G73/1067C08G73/1071C08J2379/08C08J2423/06C08J2433/26C08J2471/02C08J2479/02C08K3/04C08K5/42
Inventor 任小龙马纪翔陈志平蒋耿杰
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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