Preparation method of uniform polyimide film
A technology of polyimide film and polyamic acid film, which is applied in the field of preparation of uniform polyimide film, can solve the problems of uneven surface of polyimide film, uneven polyamic acid solution, wide molecular weight distribution, etc. , to achieve the effects of easy and stable control of the processing process, reduction of film defects, and narrow molecular weight distribution
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Embodiment 1
[0049] 1. Stock solution preparation: Add 1.0814kg (10mol) p-phenylenediamine (PDA) and 35.39kg N,N-dimethylacetamide (water content 180ppmw) into the reaction kettle,2 Protect and stir until the monomer is completely dissolved, add 2.8773kg (9.78mol) 3,3′,4,4′-biphenyltetraacid dianhydride (BPDA) powder at a rate of 1.4kg / h, and continue to heat at 25°C after the addition is complete. N 2 Stirring under protection for 2 hours at a stirring speed of 250 rpm, a uniform transparent viscous polyamic acid solution was obtained. After testing, the apparent viscosity of the polyamic acid solution at 25°C was 21Pa·s, the number average molecular weight was 167000, and the molecular weight distribution was 1.37. foreign body. The polyamic acid solution is filtered through 5 μm and 0.5 μm filter materials, and then degassed under reduced pressure to obtain a polyamic acid film-forming stock solution.
[0050] 2. Cast film formation: the polyamic acid stock solution is controlled by a...
Embodiment 2
[0056] 1. Stock solution preparation: Add 2.0024kg (10mol) 4,4'-diphenyl ether diamine (ODA) and 21.98kg N,N-dimethylacetamide (water content 460ppmw) into the reaction kettle, 2 Protect and stir until the monomer is completely dissolved, add 2.8773kg (9.78mol) 3,3',4,4'-biphenyltetraacid dianhydride (BPDA) powder at a rate of 0.96kg / h, and continue at 0°C after the addition is complete N 2 Stirring for 4 hours under protection at a stirring speed of 200 rpm, a uniform transparent viscous polyamic acid solution was obtained. After testing, the polyamic acid solution has an apparent viscosity of 74Pa·s, a number average molecular weight of 172000, and a molecular weight distribution of 1.41 at 25°C. After passing the solution through a 2μm glass fiber filter membrane, the filter screen is exposed to ultraviolet fluorescent lamps. No foreign matter. The polyamic acid solution is filtered through 8 μm and 1 μm filter materials, and then degassed under reduced pressure to obtain...
Embodiment 3
[0060] 1. Preparation of stock solution: Add 1.0012kg (5mol) 4,4'-diphenyl ether diamine (ODA) and 22.16kg N,N-dimethylacetamide (water content 460ppmw) into the reaction kettle, at 20°C N 2 Stir under protection, after completely dissolving, add 1.4416kg (4.9mol) 3,3′,4,4′-biphenyltetraacid dianhydride (BPDA) powder at a rate of 2.88kg / h, continue to heat at 20°C after the addition is complete N 2 Stir for 1 h under protection at a stirring speed of 400 rpm to obtain a uniform transparent viscous polyamic acid solution. After testing, the polyamic acid solution has an apparent viscosity of 60Pa·s, a number average molecular weight of 163000, and a molecular weight distribution of 1.20 at 25°C. After passing the solution through a 2μm glass fiber filter membrane, the filter screen is exposed to ultraviolet fluorescent lamps. No foreign matter. The polyamic acid solution is filtered through 10 μm and 1 μm filter materials, and then degassed under reduced pressure to obtain a...
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Abstract
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