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Method for preparing viscosity-controllable polyacrylonitrile carbon fiber spinning solution

A technology for polyacrylonitrile carbon fiber and spinning dope, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of molecular weight drop, poor spinnability, and excessive molecular weight of spinning solution.

Inactive Publication Date: 2015-04-29
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 when azobisisoheptanonitrile is used as an initiator in the polyacrylonitrile spinning stock solution prepared by the one-step method in the prior art, the molecular weight of the spinning solution is too large, the viscosity is too large, and the spinnability is poor. After the chain transfer agent, the molecular weight of polyacrylonitrile spinning dope decreases and the molecular weight distribution becomes wider. A kind of polyacrylonitrile carbon fiber spinning dope with controllable viscosity is provided.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 97 g of distilled acrylonitrile (AN), 2 g of itaconic acid (IA), 0.1 g of sodium propylene sulfonate, 0.6 g of azobisisoheptanonitrile (ABVN) and 400 g of dimethylsulfoxide (DMSO) were added to the reaction In the reactor, the magnetic sub-stirring makes the mixing uniform, and the reactor is sealed. Under nitrogen protection, react at a constant temperature of 38° C. for 20 hours to obtain a polyacrylonitrile 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 89084, the molecular weight distribution is 3.34, and the viscosity is 57 Pa·S at 60°C.

[0016]

Embodiment 2

[0018] 121 g of distilled acrylonitrile (AN), 2.75 g of methyl acrylate, 0.2 g of sodium propylene sulfonate, 0.75 g of azobisisoheptanonitrile (ABVN), and 376 g of dimethyl sulfoxide (DMSO) were added to the reactor , Magnetic stirring to make the mixing even, seal the reactor. Under the protection of helium, react at a constant temperature of 38° C. for 24 hours to obtain a polyacrylonitrile 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 105447, the molecular weight distribution is 3.23, and the viscosity is 86 Pa·S at 60°C.

[0019]

Embodiment 3

[0021] 146 g of distilled acrylonitrile (AN), 3 g of methyl methacrylate, 1.5 g of sodium methacrylate, 0.9 g of azobisisoheptanonitrile (ABVN) and 350 g of dimethylsulfoxide (DMSO) were added to In the reactor, the magnetic sub-stirring makes the mixing uniform, and the reactor is sealed. Under the protection of argon, react at a constant temperature of 38° C. for 26 hours to obtain a polyacrylonitrile 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 117856, the molecular weight distribution is 3.46, and the viscosity is 109 Pa·S at 60°C.

[0022]

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PUM

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Abstract

The invention relates to a method for preparing a viscosity-controllable polyacrylonitrile carbon fiber spinning solution and mainly solves the problems in the prior art that when the dimethylsulfoxide (DMSO) one-step method is adopted for preparing the polyacrylonitrile spinning solution and ABVN is used for low-temperature initiation, extremely high molecular weight, overlarge viscosity and poor spinnability are caused. The method provided by the invention comprises the steps of taking acrylonitrile, a comonomer 1 and a comonomer 2 as copolymerization components, adding a solvent (DMSO) and an initiator (ABVN) into a reactor, enabling reaction for 20-40h at the temperature of 30-55 DEG C under the protection of an inert gas to a reactive material, controlling the molecular weight and the viscosity of the spinning solution through adjusting components of the comonomer 2, obtaining the spinning solution with the molecular weight of 80,000-120,000 after demonomerisation and deaeration, enabling the molecular weight to be distributed in 1-4, and controlling the viscosity of the solution at 20-120Pa.S at the temperature of 60 DEG C to obtain the polyacrylonitrile copolymer spinning solution. By adopting the technical scheme, the problems are better solved, and the viscosity-controllable polyacrylonitrile carbon fiber spinning solution can be used in industrial production of carbon fiber precursors.

Description

technical field [0001] The invention relates to a method for preparing polyacrylonitrile carbon fiber spinning dope with controllable viscosity. 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 sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/46C08F222/02C08F220/14C08F220/56C08F228/02D01F9/22
Inventor 屠晓萍沈志刚李磊赵微微
Owner CHINA PETROLEUM & CHEM CORP
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