Preparation method of polyimide fibers
A polyimide fiber and polyimide technology, applied in the field of fiber, can solve problems such as unreported research
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[0031] The invention provides a kind of preparation method of polyimide fiber, comprises the following steps:
[0032] Polymerizing monomer dianhydride and monomer diamine to obtain a polyamic acid solution;
[0033] mixing the light stabilizer solution with the polyamic acid solution to obtain a polyamic acid spinning stock solution;
[0034] Spinning the polyamic acid spinning dope to obtain polyamic acid fibers;
[0035] Imidating polyamic acid fibers to obtain polyimide primary fibers;
[0036] hot drawing polyimide primary fibers to obtain polyimide fibers;
[0037] The monomer dianhydride is selected from at least one of the structures of formula (I) and formula (II) and a mixture of at least one of the structures of formula (III) and formula (IV);
[0038] Formula (I); Formula (II);
[0039] Formula (III); Formula (IV);
[0040] The monomer diamine is selected from one or more of the structures of formula (V) and formula (VI);
[0041] Formula (V); For...
Embodiment 1
[0077] Dissolve 43.26g (0.400mol) of p-phenylenediamine, 131.16g (0.500mol) of 2,5-bis(4-aminophenyl)pyrimidine and 10.81g (0.100mol) of m-phenylenediamine in 4000mL of N-methylpyrrolidone Add 264.80g (0.9mol) 4,4'-biphenyl dianhydride and 40.23g (0.1mol) 3,4'-triphenylene dianhydride under stirring at 15°C, and keep the temperature for 7 hours. Dissolve 4.90g of GW-783 (GW-944 and GW-622 at a weight ratio of 1:1) in 200mL of N-methylpyrrolidone, add it into the polyamic acid solution under stirring, and continue stirring for 2 hours to obtain a polyamic acid stock solution .
[0078] After the above-mentioned polyamic acid stock solution is filtered and vacuum defoamed, it is spun into shape by using the dry spray wet spinning technology route. After the spinning slurry at room temperature is accurately measured by a metering pump, it is extruded from the spinneret hole and enters through the air layer. In the coagulation bath of N-methylpyrrolidone and water with a volume r...
Embodiment 2
[0084] 32.44g (0.300mol) of p-phenylenediamine, 52.46g (0.200mol) of 2,5-bis(4-aminophenyl)pyrimidine and 78.69g (0.300mol) of 2,4-bis(4-aminophenyl) Dissolve pyrimidine in 3800mL N,N'-dimethylacetamide, add 132.40g (0.45mol) 3,4'-biphenyldianhydride, 132.40g (0.450mol) 4,4'- Biphenyl dianhydride and 40.23g (0.1mol) 3,4'- triphenyl diether dianhydride, keep this temperature for 7 hours, 2.605g (poly-{[6-[(1,1,3,3- Tetramethylbutyl)-imino]-1,3,5-triazine-2,4-diyl][2-(2,2,6,6-tetramethyl-4-piperidinyl)- Nitrilo]-hexamethylene-[4-(2,2,6,6-tetramethyl-4-piperidinyl)-nitrilo]}) (GW-944) dissolved in 180mL N,N-di Methyl acetamide was added into the polyamic acid solution under stirring, and the stirring was continued for 2 hours to obtain the polyamic acid stock solution.
[0085] After the above-mentioned polyamic acid stock solution is filtered and vacuum defoamed, it is spun and formed by wet spinning technology. After the spinning slurry at room temperature is accurately measu...
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