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Production of black polyamide thin film

A technology of black polyimide and polyamic acid, applied in the field of aromatic dianhydride and 4, can solve the problems of brittle film performance and complex production conditions

Active Publication Date: 2007-11-21
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of the prior art is that the polyimide molding can be solidified at low temperature and in a short time, and the workability and productivity are good. The disadvantage is that high temperature is required when the film is used for blister molding or thermocompression molding, the production conditions are complicated, and the film The performance is brittle, so the existing technology must be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Preparation of black slurry

[0018] 150g carbon black is filled in 1000ml dimethylacetamide, then add 33g logarithmic reduced viscosity and be the polyamic acid solution of 1.0 deciliter / gram (hereinafter referred to as polydiphenyl ether tetracarboximide precursor solution) , the polyamic acid solution is generated by the reaction of 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride and 4,4'-diaminodiphenyl ether; Pulverize into a black slurry with a carbon black particle diameter of 4.9 μm.

[0019] (2) Preparation of polyamic acid solution

[0020] 217g (0.7 mol) 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride and 65g (0.3 mol) pyromellitic dianhydride and 184g (1 mol) 4,4'-diaminodiphenyl ether React in 1600 ml of dimethylacetamide at 35° C. for 4 hours to obtain a polyamic acid solution with a eggplant viscosity of 18 minutes.

[0021] (3) Mixing of black slurry and polyamic acid solution.

[0022] Stir the black slurry at high speed for 1.5 hr, th...

Embodiment 2

[0026] During the preparation of the black slurry, 100g of carbon black was removed, the stirring speed was 2800 rpm, and 55g of polydiphenyl ether tetracarboximide precursor solution was added, the stirring temperature was 20°C, and the logarithmic viscosity was 1.2 dl / g. Other formulations and steps are the same as in Example 1 except that the carbon black particle diameter is 4.8 μm.

[0027] In the preparation of the polyamic acid solution, except that the reaction temperature was 45° C., the reaction time was 3 hours, and the eggplant viscosity of the polyamic acid solution was 10 minutes, other formulations and steps were the same as in Example 1.

[0028] The mixing of the black slurry and the polyamic acid solution, except that the black slurry was first stirred for 1 hr, then 120 g of the black slurry was added and stirred for 2 hours, other formulations and steps were the same as in Example 1.

[0029] The obtained black polyimide film has a thickness of 25 μm, a bla...

Embodiment 3

[0031] In the process of black slurry preparation, carbon black removal is 200g, and the stirring speed is 6000 rpm. When 5g is added, the reduced viscosity is 1.1 dl / g. The polydiphenyl ether tetracarboximide precursor solution is stirred at 50°C to form Except for the black paste with a black particle diameter of 4.7 μm, other formulations and steps are the same as in Example 1.

[0032] In the preparation of the polyamic acid solution, except that the reaction temperature is 20°C, the reaction time is 4.5Hr, and the eggplant viscosity of the polyamic acid solution is 25 minutes. Other formulas and steps are the same as in Example 1.

[0033] In the mixing of the black slurry and the polyamic acid solution, except that the black slurry was first stirred for 2 minutes, 600 g of the black slurry was added, and after stirring at a speed of 150 rpm for 3 hours, other formulas and steps were the same as in Example 1.

[0034] The prepared black polyimide film has a thickness of ...

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Abstract

Production of black polyimide thin film is carried out by high-speed agitating while crushing for carbon black methyl acetamino solution 10-20 wt% with poly(diphenyl ether) tetramethyl-imide precursor solution at 2800-6000 / min below 20-50 degree to obtain black slurry with granular diameter <5mum, reacting of aromatic dianhydride and aromatic diamino in dimethyl acetamide solution at 20-45 degree for 3-4.5 hrs to obtain polyamide acid solution, high-speed agitating for black slurry for 1-2 hrs, adding into polyamide acid solution with viscosity 10-25 mins, agitating at 150 / min for 2-3 hrs to obtain black solution with viscosity 10-25 mins, doctor blade casting or latex dipping and filming. The thickness is 25-125mum, the extensibility is 18-20%, tensile strength is 140-160 MPa, and dielectric strength is 20-30 MV / m.

Description

technical field [0001] The present invention relates to a kind of preparation method of black polyimide film, relate to 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride-based aromatic dianhydride and 4,4'- The invention discloses a method for preparing black polyimide film by reacting diaminodiphenyl ether. Background technique [0002] Black polyimide film has high thermal conductivity, antistatic performance and good electrical conductivity as well as excellent adhesive performance. Has been widely used in the electronics industry, optical fields. Specific applications include: audio voice coil bobbins, flexible printed circuit board substrates, mobile phone shielding materials, thermal protection materials, light-shielding materials and optical filters, etc. [0003] Prior art JP02-138340, 28.05.1990 discloses pyromellitic dianhydride and 4,4'-diaminodiphenyl ether reacted in N-methylpyrrolidone to make polyimide precursor solution, optional one Additives such as c...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08K5/17
Inventor 项志度王伟民冯介骅邬显德费祯田
Owner SHANGHAI PLASTICS RES INST CO LTD
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