Method for preparing high-performance polyacrylonitrile solution for carbon fibers

A technology of polyacrylonitrile and acrylonitrile is applied in the field of preparing high-performance polyacrylonitrile stock solution for carbon fiber, which can solve the problems of wide molecular weight distribution and difficult process control, and achieve the effect of good technical effect.

Active Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is that there is a problem in the prior art that a single initiator is used to prepare acrylonitrile stock solution, the stock solution or molecular weight distribution is wide or a large amount of gel is produced, making the process difficult to control. The method for preparing polyacrylonitrile stock solution with initiator

Method used

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  • Method for preparing high-performance polyacrylonitrile solution for carbon fibers

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Experimental program
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Effect test

Embodiment 1

[0017] Weigh dimethyl sulfoxide, acrylonitrile, itaconic acid, β-butyl itaconate, and initiator at a weight ratio of 800:196:1.5:2.5:1, wherein azobisisoheptanonitrile accounts for 20 parts of the total weight of the initiator, 80 parts of azobisisobutyronitrile, polymerized at 35°C for 5 hours, raised the temperature to 60°C, and reacted for 19 hours. After the reaction, the residual monomers and bubbles were removed in vacuum to obtain The polyacrylonitrile stock solution obtained by GPC test has a weight-average molecular weight of 208,000, a molecular weight distribution index of 1.72, and a maximum apparent viscosity of 283 Pa·s during the preparation process. The obtained polyacrylonitrile stock solution was transparent and homogeneous, and no gel was produced through the filtration test.

Embodiment 2

[0019] Weigh dimethyl sulfoxide, acrylonitrile, itaconic acid, methyl acrylate, initiator at a weight ratio of 800:180:15:5:1, wherein azobisisoheptanonitrile in the initiator accounts for the total weight of the initiator The number of parts is 30 parts, and azobisisobutyronitrile is 70 parts. Polymerize at 40°C for 4 hours, heat up to 63°C, and react for 28 hours. After the reaction, the residual monomers and bubbles are removed in vacuum to obtain polyacrylonitrile stock solution According to the GPC test, the weight-average molecular weight of the copolymer is 203,000, the molecular weight distribution index is 2.21, and the highest apparent viscosity during the preparation process is 236Pa·s. The obtained polyacrylonitrile stock solution was transparent and homogeneous, and no gel was produced through the filtration test.

Embodiment 3

[0021] Weigh dimethyl sulfoxide, acrylonitrile, itaconic acid, acrylamide, initiator in a weight ratio of 800:190:5:5:0.5, wherein azobisisoheptanonitrile in the initiator accounts for the total weight part of the initiator 10 parts of azobisisobutyronitrile, 90 parts of azobisisobutyronitrile, polymerized at 30°C for 5 hours, raised the temperature to 63°C, and reacted for 30 hours. After the reaction, the residual monomers and bubbles were removed in a vacuum to obtain a polyacrylonitrile stock solution. According to GPC test, the weight average molecular weight of the copolymer is 156,000, the molecular weight distribution index is 1.87, and the highest apparent viscosity during the preparation process is 206Pa·s. The obtained polyacrylonitrile stock solution was transparent and homogeneous, and no gel was produced through the filtration test.

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Abstract

The invention relates to a method for preparing a high-performance polyacrylonitrile solution for carbon fibers, and especially relates to a method for preparing the polyacrylonitrile solution through adopting a new initiator to mainly solve a problem of difficult process control caused by wide molecular weight distribution or abundant gel generation of solutions prepared through a single initiator used for preparing an acrylonitrile solution in the prior art. According to the invention, the initiator comprises 70-100 parts by weight of azodiisobutyronitrile and 1-30 parts by weight of azobisisoheptonitrile. The method well solves the problem through above technical scheme, and can be used for the industrial production of the acrylonitrile solution polymerization

Description

technical field [0001] The invention relates to a method for preparing a high-performance polyacrylonitrile stock solution for carbon fibers. Background technique [0002] Carbon fiber has excellent mechanical properties and chemical stability. It is the fiber with the highest specific strength and the highest specific modulus among the high-performance fibers that have been mass-produced. Especially in high-temperature inert environments above 2000 ° C, carbon materials are The only substance whose strength does not decrease is unmatched by other main structural materials (metals and their alloys). High-performance carbon fiber, as one of the key materials to realize the "miniaturization" and "lightweight" of weapons and equipment, has a pivotal impact on the defense industry. It is also widely used for civilian purposes such as entertainment, and the consumption is considerable. In recent years, due to the technological development in the field of carbon fiber applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F4/04D01F6/38D01F9/22D01D1/02
Inventor 崔晶屠晓萍沈志刚王贺团
Owner CHINA PETROLEUM & CHEM CORP
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