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
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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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