Low viscosity and high performance carbon fiber spinning stock solution preparation method

A spinning dope, low viscosity technology, used in spinning solution preparation, fiber chemical characteristics, textiles and papermaking, etc., can solve problems such as excessive viscosity, widened molecular weight distribution, poor spinnability, etc., and achieve good technical effects, The effect of improved spinnability

Active Publication Date: 2013-12-04
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 that the polyacrylonitrile spinning dope produced by one-step method in the prior art has too large molecular weight, too high viscosity and poor spinnability when no chain transfer agent is used. After adjusting the method, the molecular weight of the polyacrylonitrile spinning stock solution decreases and the molecular weight distribution becomes wider. It provides a new low-viscosity, high-performance carbon fiber spinning stock solution preparation method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 97g of distilled acrylonitrile (AN), 2g of itaconic acid (IA), 1g of acrylic acid, 0.6g of azobisisobutyronitrile (AIBN), 380g of dimethylsulfoxide (DMSO) and 20g of N,N-dimethyl Dimethyl formamide (DMF) is added in the reactor, magnetic sub-stirring makes the mixing uniform, and seals the reactor. Under nitrogen protection, react at a constant temperature of 60° C. for 20 hours to obtain a binary acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. After testing, the molecular weight is 95078, the molecular weight distribution is 2.74, and the viscosity is 34 Pa·S at 60°C.

[0016]

Embodiment 2

[0018] 121g of distilled acrylonitrile (AN), 3g of itaconic acid (IA), 0.75g of acrylic acid, 0.75g of azobisisobutyronitrile (AIBN), 357g of dimethylsulfoxide (DMSO) and 19g of N,N- Add dimethylformamide (DMF) into the reactor, stir with a magnet to make the mixture even, and seal the reactor. Under nitrogen protection, react at a constant temperature of 60° C. for 24 hours to obtain a binary acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. After testing, the molecular weight is 138067, the molecular weight distribution is 2.63, and the viscosity is 68 Pa·S at 60°C.

[0019]

Embodiment 3

[0021] 146g of distilled acrylonitrile (AN), 3g of itaconic acid (IA), 2g of methyl acrylate, 0.9g of azobisisobutyronitrile (AIBN), 332g of dimethylsulfoxide (DMSO) and 18g of N,N - Add dimethylformamide (DMF) into the reactor, stir with a magnet to make the mixture even, and seal the reactor. Under nitrogen protection, react at a constant temperature of 60° C. for 26 hours to obtain a binary acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. After testing, the molecular weight is 147560, the molecular weight distribution is 2.93, and the viscosity is 77 Pa·S at 60°C.

[0022]

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PUM

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Abstract

The present invention relates to a low viscosity and high performance carbon fiber spinning stock solution preparation method, wherein problems of high molecule weight, narrow molecule weight distribution, high viscosity and poor spinnability of the polyacrylonitrile spinning stock solution prepared through the one-step method in the prior art are mainly solved with the present invention. The technical scheme comprises that the low viscosity and high performance carbon fiber spinning stock solution preparation method comprises the following steps: adopting acrylonitrile, a copolymerization monomer 1 and a copolymerization monomer 2 as copolymerization components, mixing the copolymerization components, a solvent dimethyl sulfoxide, an initiator azobisisobutyronitrile and an adjustment agent, adding the obtained material to a reactor, carrying out a reaction for 20-40 h at a temperature of 50-70 DEG C under protection of gas presenting inertia for the reaction substances, and carrying out monomer removing and deaeration to obtain the polyacrylonitrile spinning stock solution with a molecule weight of 90000-150000, molecule weight distribution of less than 3 and a viscosity of 30-90 Pa.S at a temperature of 60 DEG C. With the technical scheme, the problems in the prior art are well solved, and the preparation method can be used for industrial production of carbon fiber precursors.

Description

technical field [0001] The invention relates to a method for preparing a low-viscosity, high-performance carbon fiber spinning dope. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] The initial copolymer structure and properties determine the final carbon fiber structure and properties. Therefore, starting from the synthesis of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38D01D1/02D01F9/22C08F220/46C08F220/48
Inventor 屠晓萍沈志刚王贺团崔晶史纪友
Owner CHINA PETROLEUM & CHEM CORP
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