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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

Active Publication Date: 2018-02-09
JIANGXI XIAN CAI NANOFIBERS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In particular, there has not been any report on the preparation of polyimide fiber products with nanometer fiber diameter and micrometer length in batches.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] A kind of preparation method of polyimide ultra-short fiber of the present invention is specifically realized through the following steps:

[0030] Step 1, reacting diamine and acid anhydride monomers in a polar solvent to generate polyamic acid, and obtaining a polyamic acid nonwoven fabric with a fiber diameter of nanometer or micrometer by electrospinning or solution spraying; or , react diamine and acid anhydride monomers in a polar solvent to generate polyamic acid, and obtain continuous polyamic acid fibers with a fiber diameter of microns by dry method, wet method or dry spray wet spinning method; 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), dimethylsulfoxide (DMSo), tetrahydrofuran ( One or more of THF).

[0032] Preferably, the diamine is selected from: 4,4'-diaminodiphenyl ether (ODA), p-phenylen...

Embodiment 1

[0046] 1 mol of ODA, 0.8 mol of PMDA, 0.18 mol of HQDPA, and 0.04 mol of phthalic anhydride were reacted in DMAc to generate a polyamic acid solution; the solution was electrospun to obtain a polyamic acid nonwoven fabric, and then subjected to 200°C After treatment for 10 minutes, a non-woven fabric with a fiber diameter of about 0.5 μm and incomplete imidization was obtained. The non-woven fabric is mechanically crushed into a uniform sheet-like distribution, and a slurry is prepared, the concentration of the slurry is 1%, the solvent is deionized water and ethanol, and the dispersant is polyacrylic acid sodium salt. After the prepared slurry is evenly stirred, it is repeatedly processed by a deflaker, then concentrated, washed, filtered to remove the solvent, and dried at 90°C to obtain a block-shaped fiber floc aggregate. The agglomerate was mechanically pulverized and imidized at 320° C. to become a segmented polyimide fiber flocculation aggregate. Then the above-mention...

Embodiment 2

[0048] 1mol of ODA, 0.7mol of PMDA, and 0.3mol of BPDA are reacted in NMP to form a polyamic acid solution; the solution is wet-spun to obtain polyamic acid fibers, and then treated at 190°C for 20 minutes to obtain the fiber diameter Around 15 μm, not fully imidized fibers. The fibers were chopped, and the length of the chopped strands was 4 mm. A slurry was prepared with a slurry concentration of 15%. The solvents were deionized water and methyl ethyl ketone, and the dispersant was PEO. After the prepared slurry is uniformly stirred, it is repeatedly treated by disc grinding, then concentrated, washed, filtered to remove the solvent, and dried at 110°C to obtain a cake-shaped fiber floc aggregate. The agglomerate was mechanically pulverized and imidized at 360°C to become a polyimide granular fiber floc aggregate. Then, the above-mentioned polyimide aggregates are ball milled, and sieved by different meshes to obtain ultra-short polyimide fibers with a fiber length of 70-80...

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Abstract

The invention discloses a polyimide ultra-short fiber and a preparation method thereof and relates to the field of fiber preparation. According to the preparation method disclosed by the invention, batch preparation of polyimide fiber products with a fiber diameter nanoscale and a length micro scale can be realized. For the polyimide ultra-short fiber disclosed by the invention, the length of thefiber is 2 to 500mu m, the diameter of the fiber is 0.1 to 50mu m, and specific area is 2 to 30m<2> / g. By utilizing the physical and chemical properties at different heat treatment temperatures in thepreparation process of the polyimide fiber, dispersion and ultrashort properties of the fiber are realized more easily by adopting physical and mechanical methods in a state that the polyimide fiberis incompletely imidized; then complete imidization of the polyimide fiber is realized by high-temperature treatment; finally, the polyimide ultra-short fiber is obtained by a method of mechanical pulverization, lapping and shifting. The polyimide ultra-short fiber obtained by the preparation method disclosed by the invention has the characteristics of high and low temperature resistance, ultraviolet irradiation resistance, good insulating property and the like, and can be used for preparing a slurry coating solution, reinforcing resin, rubber and the like, forming pulp and the like.

Description

technical field [0001] The invention relates to the technical field of fiber preparation, in particular to a polyimide ultra-short fiber and a preparation method thereof. Background technique [0002] Polyimide fiber is currently an organic fiber with a higher temperature. Compared with other high-performance fibers (such as aramid fibers and polyphenylene sulfide fibers), it has better heat resistance, aging resistance, oxidation resistance, UV resistance, and water absorption. Therefore, polyimide fibers are widely used in environmental protection, aerospace, special and high temperature insulation, civil textiles and other fields. Ultra-short polyimide fiber not only has the excellent properties of polyimide fiber, but more importantly, it can be made into slurry coating liquid, or used as filler for resin, rubber, etc., or used as special paper pulp The use of materials, etc., has greatly expanded the application field of polyimide fibers. [0003] At present, it is qu...

Claims

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Application Information

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IPC IPC(8): D01F6/94D01F1/10D06C7/00D02J13/00
CPCD01F1/10D01F6/94D02J13/00D06C7/00
Inventor 付饶谭洪艳侯豪情欧阳文于暴韩京成
Owner JIANGXI XIAN CAI NANOFIBERS TECH
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