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
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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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