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Preparation method of polyacrylonitrile precursor

A technology of polyacrylonitrile spinning and polyacrylonitrile, which is applied in the direction of spinning solution preparation and wet spinning, which can solve the problems of poor performance of raw silk and achieve the effects of excellent performance, easy operation and cost reduction

Active Publication Date: 2013-09-25
WEIHAI TUOZHAN FIBER +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the filament solidifies quickly, and the above-mentioned skin-core structure is easily formed, and the obtained raw filament has poor performance.
[0004] In view of this, in order to overcome the shortcomings of the prior art in the production process of polyacrylonitrile precursors, the filaments solidify too fast and form a skin-core structure, resulting in poor performance of the precursors, to find a polypropylene with a dense structure and excellent performance. The preparation method of nitrile precursor is very necessary

Method used

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  • Preparation method of polyacrylonitrile precursor
  • Preparation method of polyacrylonitrile precursor
  • Preparation method of polyacrylonitrile precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1, the preparation of polyacrylonitrile precursor

[0038] With the 45wt% sodium thiocyanate solution that contains 17wt% acrylonitrile-itaconic acid-methyl acrylate terpolymer (wherein, the molar percentage composition of each monomer is respectively 95%, 1% and 4%), adopt Dry-jet wet spinning, after the spinning solution leaves the spinneret hole, it is coagulated in a n-butanol coagulation bath at 2°C for about 1.0 min to obtain primary gel filaments. The obtained primary gel filaments are further coagulated through a 30 wt % sodium thiocyanate aqueous solution coagulation bath at 50° C. to obtain coagulated filaments. After the coagulated filaments are taken out of the sodium thiocyanate aqueous solution coagulation bath, they are washed with water at a temperature of 60°C. After washing with water, the washed silk is dried in a blast drying oven at 80°C for 1 hour to obtain a polyacrylonitrile raw silk. The SEM photograph of gained polyacrylonitrile pr...

Embodiment 2

[0039] Embodiment 2, the preparation of polyacrylonitrile precursor

[0040]With the 50wt% sodium thiocyanate solution that contains 17wt% acrylonitrile-itaconic acid-methyl acrylate terpolymer (wherein, the molar percentage composition of each monomer is respectively 96%, 2% and 2%), adopt Dry-jet wet spinning, after the spinning solution leaves the spinneret hole, the aliphatic alcohol coagulation bath composed of n-butanol and 30wt% sodium thiocyanate aqueous solution (wherein, n-butanol and 30wt% sodium thiocyanate The mass fraction ratio of the aqueous solution is 4:1), and the primary gel filaments are obtained after coagulating for about 10.0 min. The obtained primary gel strands are then passed through the first-stage coagulation bath of 25wt% sodium thiocyanate aqueous solution at 30°C and the second-stage coagulation bath of 15wt% sodium thiocyanate aqueous solution at 20°C, and are further coagulated to obtain Solidified strands. After the solidified filaments are...

Embodiment 3

[0041] Embodiment 3, the preparation of polyacrylonitrile precursor

[0042] With the 65wt% nitric acid aqueous solution that contains 30wt% acrylonitrile-itaconic acid binary copolymer (wherein, the molar percentage composition of each monomer is 98% and 2% and respectively), adopt dry-jet wet spinning method to spin, spin The silk liquid leaves the spinneret hole, and first coagulates in a coagulation bath composed of isobutanol and 60% nitric acid aqueous solution (wherein, the mass fraction ratio of isobutanol and 60% nitric acid aqueous solution is 97:3) at 25 ° C for about 6 minutes to obtain primary Gel strands. The resulting primary gel strands are then passed through the first stage coagulation bath of 50wt% nitric acid aqueous solution at 50°C, the second stage coagulation bath of 30wt% nitric acid aqueous solution at 30°C and the 15wt% nitric acid aqueous solution at 20°C The third coagulation bath is further coagulated to obtain coagulated filaments. After the co...

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Abstract

The invention discloses a preparation method of a polyacrylonitrile precursor. The method comprises the following steps: (1) spinning a polyacrylonitrile spinning stock solution, injecting the stock solution into a fatty alcohol coagulation bath and solidifying to obtain a primary gel fibre filament; (2) adding the primary gel fibre filament into at least one stage of inorganic salt aqueous coagulation bath and solidifying to obtain a polyacrylonitrile solidified filament; (3) washing the polyacrylonitrile solidified filament and drying to obtain the polyacrylonitrile precursor. Without changing a prior art, the method merely adds a segment of the coagulation bath consisting of fatty alcohol and inorganic salt to obtain the polyacrylonitrile precursor with more compact structure and more excellent performances.

Description

technical field [0001] The invention relates to a method for preparing carbon fiber precursors, in particular to a method for preparing polyacrylonitrile precursors. Background technique [0002] At present, almost all carbon fibers used in industry are formed by carbonization of organic fibers while maintaining their original shape. Therefore, the quality of carbon fibers depends largely on the quality of raw silk. The coagulation process is one of the most important process steps that affect the properties of the precursor. When the polyacrylonitrile spinning solution enters the coagulation bath, a double diffusion process occurs in which the precipitant diffuses into the filament and the solvent in the filament diffuses into the coagulation bath. The double diffusion first occurs on the surface of the filament. If the coagulation is too fast, the filament will A dense skin layer will be formed on the surface of the strip, which hinders the double diffusion process of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01D1/02D01D5/06D01F9/22
Inventor 李书乡徐坚余晓兰张小莉赵宁
Owner WEIHAI TUOZHAN FIBER
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