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Spinning method of high molecular weight and high viscosity spinning solution

A spinning solution, high molecular weight technology, applied in wet spinning, stretch spinning, single-component synthetic polymer rayon, etc., can solve the problems of high fiber breakage rate and poor fiber formation, and achieve uniform color , low CV value and stable performance

Active Publication Date: 2018-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the high molecular weight and high viscosity spinning solution in the prior art has poor fiber-forming properties and high fiber breakage rate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of spinning 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 the unreacted monomer and the bubbles generated by the reaction to obtain the spinning dope, the initiator is azobisisoheptanonitrile, the mass ratio of acrylonitrile and comonomer is 98.5:1.5, and the initiator accounts for the mass of the total monomer The percentage is 0.08%, and the total monomer concentration is 15%. After filtration, the high-performance polyacrylonitrile copolymer spinning stock solution is obtained. The spinning stock solution has a subweight of 110,000, a molecular weight distribution of 2.0, and a viscosity of 90Pa at 60°C. S, the temperature of the spinning dope is 60°C.

[0027](2) Coagulation forming: the present invention adopts the method of wet spinning to prepare, and the spinning dope is metered by a me...

Embodiment 2

[0033] (1) Preparation of spinning 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 Remove the unreacted monomer and the bubbles generated by the reaction to obtain the spinning dope, the initiator is azobisisobutyronitrile, the mass ratio of acrylonitrile and comonomer is 90:10, and the initiator accounts for the mass percentage of the total monomer is 0.25%, and the total monomer concentration is 25%. After filtration, a high-performance polyacrylonitrile copolymer spinning stock solution is obtained. The spinning stock solution has a seed weight of 290,000, a molecular weight distribution of 1.8, and a viscosity of 270Pa·S at 60°C. , The spinning dope temperature is 60°C.

[0034] (2) Coagulation forming: the present invention adopts the method of wet spinning to prepare, and the spinning dope is metered by a meterin...

Embodiment 3

[0040] (1) Preparation of spinning stock solution: 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 mono body and the bubbles generated by the reaction to obtain the spinning dope, the initiator is azobisisobutyronitrile, the mass ratio of acrylonitrile and comonomer is 95:5, and the mass percentage of the initiator in the total monomer is 0.2%, and the total The concentration of the monomer is 20%, and the high-performance polyacrylonitrile copolymer spinning stock solution is obtained through filtration. The spinning stock solution has a subweight of 150,000, a molecular weight distribution of 15, a viscosity of 146Pa·S at 60°C, and a spinning stock solution temperature of is 60°C.

[0041] (2) Coagulation forming: the present invention adopts the method of wet spinning to prepare, and the spinning dope is metered by a metering pump, and after fi...

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Abstract

The invention relates to a spinning method of a high-molecular-weight and high-viscosity spinning solution, which mainly solves the technical problems of poor fluidity, poor spinnability, high spinning pressure and high filtration pressure of the high-molecular-weight and high-viscosity spinning solution in the prior art. By adopting a spinning method of high-molecular weight and high-viscosity spinning solution, comprising the following steps: a polyacrylonitrile / dimethyl sulfoxide solution with a molecular weight of 100,000 to 300,000 and a viscosity of 80 Pa·s to 300 Pa·s, through Wet spinning to obtain a polyacrylonitrile precursor, which is characterized as follows: the breaking strength is 5cN / dtex to 8cN / dtex, the CV value of the breaking strength is 4% to 20%; the elongation at break is 8% to 16 %, the CV value of elongation at break is 4% to 20%, which solves this problem well and can be used in the industrial production of polyacrylonitrile-based carbon fiber precursors.

Description

technical field [0001] The invention belongs to a method for preparing polyacrylonitrile precursors for carbon fibers, and in particular relates to a method for wet spinning a spinning solution of high molecular weight and high viscosity polyacrylonitrile / dimethyl sulfoxide. 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 fibe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F11/06D01D5/06D01D5/14C08F220/44
Inventor 王贺团沈志刚肖士洁李磊
Owner CHINA PETROLEUM & CHEM CORP
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