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Fibre spinning method for polyacrylonitrile solution

A technology of polyacrylonitrile and solution, which is applied in the direction of feeding solution to spinneret, preparation of spinning solution, single-component synthetic polymer rayon, etc. Poor performance and other problems, to achieve the effect of improved spinnability, uniform flow field, and elimination of radial velocity difference

Active Publication Date: 2016-05-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the technical problem of poor sealing of the spinning assembly, high spinning pressure and many broken filaments of the primary fiber in the coagulation bath in the prior art

Method used

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  • Fibre spinning method for polyacrylonitrile solution
  • Fibre spinning method for polyacrylonitrile solution
  • Fibre spinning method for polyacrylonitrile solution

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Preparation of stock solution: Add acrylonitrile, itaconic acid and methyl methacrylate to the polymerization kettle, then add initiator and dimethyl sulfoxide, react at a temperature of 40°C for 10 hours, and then remove Unreacted monomers and the bubbles generated by the reaction obtain the spinning dope, the initiator is azobisisoheptanonitrile, the mass ratio of acrylonitrile and comonomer is 98.5:1.5, and the mass percent of the initiator accounting for the total monomer is 0.08%, and the total monomer concentration is 15%. After filtration, high-performance polyacrylonitrile copolymer spinning stock solution is obtained. The spinning stock solution has a particle weight of 110,000, a molecular weight distribution of 2.0, and a viscosity of 90 Pa·S at 60°C. The spinning dope temperature was 60°C.

[0046] (2) Conveying, filtering and distributing of raw liquid: adopt embedded spinneret, the heat preservation temperature of pipeline, filter and spinning assembly...

Embodiment 2

[0050] (1) Preparation of stock solution: Add acrylonitrile, ammonium itaconate and methacrylic acid to the polymerization kettle, then add initiator and dimethyl sulfoxide, react at a temperature of 60°C for 24 hours, and then remove untreated The reacted monomer and the bubbles generated by the reaction are used to obtain the spinning dope, the initiator is azobisisobutyronitrile, the mass ratio of acrylonitrile and comonomer is 90:10, and the mass percentage of the initiator in the total monomer is 0.25 %, the total monomer concentration is 25%, and the high-performance polyacrylonitrile copolymer spinning dope is obtained through filtration. The temperature of silk stock solution is 60°C.

[0051] (2) Conveying, filtering and distributing of the raw liquid: the embedded spinneret is used, and the heat preservation temperature of the pipeline, filter and spinning assembly is 65°C; 10, the filter mesh of the first filter layer is 1600, and the filter mesh of the second filt...

Embodiment 3

[0055] (1) Stock solution preparation: add acrylonitrile and itaconic acid to the polymerization kettle, then add initiator and dimethyl sulfoxide, react at a temperature of 65°C for 30 hours, and then remove unreacted monomers and Bubbles generated by the reaction were used to obtain the spinning dope, the initiator was azobisisobutyronitrile, the mass ratio of acrylonitrile and comonomer was 95:5, the mass percentage of the initiator accounting for the total monomer was 0.2%, and the total monomer The concentration of the polyacrylonitrile copolymer is 20%, and the high-performance polyacrylonitrile copolymer spinning stock solution is obtained through filtration. The spinning stock solution has a particle weight of 80,000, a molecular weight distribution of 15, a viscosity of 60 Pa·S at 60°C, and a spinning stock solution temperature of 60°C. ℃.

[0056] (2) Conveying, filtering and distributing of the raw liquid: the embedded spinneret is used, and the heat preservation te...

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Abstract

The invention relates to a fibre spinning method for a polyacrylonitrile solution, and mainly solves the technical problems in the prior art that a fibre spinning assembly has poor sealing property, fiber spinning pressure is high, and coagulating bath nascent fibre breakage is more. The invention adopts the technical scheme that the fibre spinning method for the polyacrylonitrile solution comprises the following steps: for a polyacrylonitrile / dimethyl sulfoxide solution with the molecular weight of 80 thousands to 200 thousands and viscosity of 60Pa.s to 120Pa.s, adopting an embedded fibre spinning assembly, filtering by a multi-layer combined filter net, distributing by a distributing plate, extruding by a spinneret plate, entering a coagulating bath, and coagulating to form coagulated filaments. The problems are better solved, and the fibre spinning method can be used in industrial production of polyacrylonitrile-based carbon fiber protofilaments.

Description

technical field [0001] The invention belongs to a method for preparing polyacrylonitrile precursors for carbon fibers, in particular to a method for spinning polyacrylonitrile / dimethyl sulfoxide solution. Background technique [0002] Since the 1950s, developed countries have urgently needed new structural materials and corrosion-resistant materials in order to develop large-scale rockets and artificial satellites and comprehensively improve aircraft performance, so that carbon fibers reappeared on the stage of new materials, and gradually formed PAN-based carbon fibers. The three major raw material systems of viscose-based carbon fiber and pitch-based carbon fiber. Because the production process of PAN-based carbon fiber is simpler than other methods, and the mechanical properties of the product are good, it has been developed rapidly and has become the mainstream of the current production of carbon fiber. [0003] PAN-based carbon fiber has excellent properties such as hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D5/06D01D1/02D01D1/09D01F6/38
Inventor 王贺团沈志刚屠晓萍肖士洁
Owner CHINA PETROLEUM & CHEM CORP
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