Polyimide ultra-short fiber and preparation method thereof
A technology of ultra-short fiber and polyimide, applied in the field of polyimide ultra-short fiber and its preparation, to achieve good insulation effect
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[0029] The preparation method of polyimide ultra-short fiber of the present invention is specifically realized by the following steps:
[0030] Step 1. Diamine and acid anhydride monomers are reacted in a polar solvent to generate polyamic acid, and a polyamic acid nonwoven fabric with a nanometer or micrometer fiber diameter is obtained by electrospinning or solution jetting; or , The diamine and acid anhydride monomers are reacted in a polar solvent to generate polyamic acid, and the polyamic acid continuous fiber with a fiber diameter of micrometers is obtained by dry, wet or dry-jet wet spinning; diamine and The molar ratio of acid anhydride monomers is: (0.95-1):1.
[0031] Preferably, the polar solvent is selected from: dimethylformamide (DMF), dimethylacetamide (DMAc), N,N-dimethylpyrrolidone (NMP), dimethyl sulfoxide (DMSo), tetrahydrofuran ( THF) one or more of them.
[0032] Preferably, the diamine is selected from: 4,4'-diaminodiphenyl ether (ODA), p-phenylenediamine (PP...
Example Embodiment
[0045] Example 1
[0046] 1mol of ODA, 0.8mol of PMDA, 0.18mol of HQDPA, 0.04mol of phthalic anhydride, react in DMAc to form a polyamic acid solution; this solution is electrospinning to obtain a polyamic acid nonwoven fabric, and then subjected to 200℃ Treated for 10 minutes to obtain a non-woven fabric with a fiber diameter of about 0.5 μm and not completely imidized. The non-woven fabric is mechanically broken into a uniform sheet-like distribution, a slurry is prepared, the slurry concentration is 1%, the solvent is deionized water and ethanol, and the dispersant is polyacrylate sodium salt. After the prepared slurry is uniformly stirred, it is repeatedly processed by a decomposer and then concentrated and washed, the solvent is filtered out, and dried at 90° C. to obtain block fiber flocs. The agglomerate is subjected to mechanical pulverization treatment and imidized at 320°C to become a polyimide segmented fiber flocculation. Then, the above polyimide agglomerates were ...
Example Embodiment
[0047] Example 2
[0048] 1mol of ODA, 0.7mol of PMDA, 0.3mol of BPDA, react in NMP to form a polyamic acid solution; the solution is wet-spinning to obtain polyamic acid fibers, and then treated at 190°C for 20 minutes to obtain fiber diameter About 15μm, not completely imidized fiber. The fiber is chopped, the chopped strand length is 4mm, the slurry is prepared, the slurry concentration is 15%, the solvent is deionized water and methyl ethyl ketone, and the dispersant is PEO. After the prepared slurry is uniformly stirred, it is repeatedly processed by a disc mill and then concentrated and washed, the solvent is filtered out, and it is dried at 110°C to obtain a cake-like fiber flocculent aggregate. The agglomerate is mechanically pulverized and imidized at 360°C to become a polyimide granular fiber flocculation. Then the above polyimide agglomerates are subjected to ball milling and sieved by different meshes to obtain ultra-short polyimide fibers with a fiber length of 70-...
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