Polyamide acid fibrid, polyimide fibrid and preparation method of polyamide acid fibrid
A technology of precipitating fibers and polyamic acid, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, single-component synthetic polymer rayon, etc., which can solve the mechanical and insulating properties that limit the mass production of polyimide paper products and other issues, to achieve the effect of improving mechanical strength and insulation performance, low dielectric loss, and high wave-transmitting performance
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[0014] On the one hand, the invention provides a kind of preparation method of polyamic acid fibrid, the method comprises:
[0015] (1) react amine monomer and acid anhydride monomer in polar solvent to generate polyamic acid product;
[0016] (2) Dilute the product obtained in step (1) until the polyamic acid concentration is 1-14% by weight and the viscosity is less than 500cp, and then inject the diluted solution into the precipitant under stirring conditions;
[0017] Wherein, the precipitating agent is at least one of water, ethanol, methanol, acetone and toluene.
[0018] According to the method of the present invention, in step (1), the amine monomers are various amines in the art, such as diamines and / or triamines, preferably diamines, more preferably At least one of hexafluorodiamine, biphenylenediamine, 3,4-diaminodiphenyl ether, 4,4'-diamino-4"-hydroxytriphenylmethane, which can significantly improve the obtained polyamide The specific surface area of acid preci...
Embodiment 1
[0041] This example is used to illustrate the polyamic acid fibrids and polyimide fibrids of the present invention and their preparation methods.
[0042] (1) Dissolve 3,4-diaminodiphenyl ether in a mixed solvent of N,N-dimethylacetamide and xylene with a volume ratio of 6:1, and then add acid anhydride monomers (acid anhydride monomers The composition is: 2,3,3',4'-biphenyl tetra-acid dianhydride, 3,3',4,4'-benzophenone tetra-acid dianhydride and 3,3',4,4'-biphenyl tetra-acid dianhydride Phenyl ether tetra-acid dianhydride, the weight ratio is 1:1:5), the molar ratio of 3,4-diaminodiphenyl ether and acid anhydride monomer is controlled to be 1:0.95, and the solid content in every liter of mixed solvent is 200g , stirring and reacting at 10°C for 2h to generate polyamic acid product;
[0043] (2) Add the above-mentioned mixed solvent to the polyamic acid product obtained in step (1) until the content of polyamic acid is 5% by weight, and the solution viscosity is 200cp, and t...
Embodiment 2
[0046] This example is used to illustrate the polyamic acid fibrids and polyimide fibrids of the present invention and their preparation methods.
[0047] (1) Hexafluorodiamine is dissolved in N, N-dimethylacetamide and xylene in a mixed solvent with a volume ratio of 7:1, and then an acid anhydride monomer is added (the composition of the acid anhydride monomer is: 2 , 3,3',4'-biphenyl tetraacid dianhydride, 3,3',4,4'-benzophenone tetraacid dianhydride and 3,3',4,4'-diphenyl ether tetraacid di Anhydride, the weight ratio is 1:2:2), the molar ratio of hexafluorodiamine and acid anhydride monomer is controlled to be 1:1, and the solid content in each liter of mixed solvent is 240g, and the reaction is stirred at 25°C for 1h to form poly Amic acid products;
[0048] (2) Add the above-mentioned mixed solvent to the polyamic acid product obtained in step (1) until the content of polyamic acid is 7% by weight, and the solution viscosity is 250cp, and then inject it at 50°C and 800...
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