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Polyacrylonitrile suspension with high solid content and low viscosity, preparation method and application thereof, and preparation method of polyacrylonitrile-based carbon fiber

A technology of polyacrylonitrile and high solid content, which is applied in the field of carbon fiber and can solve problems such as poor process continuity, high viscosity of the polymerization system, and difficulty in mass and heat transfer.

Active Publication Date: 2021-07-06
吉林碳谷碳纤维股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process of preparing polyacrylonitrile-based carbon fibers from polyacrylonitrile prepared by homogeneous solution polymerization method has long polymerization cycle, high viscosity of polymerization system, and difficulty in mass and heat transfer in the later stage of polymerization, resulting in poor process continuity in the preparation process. sex

Method used

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  • Polyacrylonitrile suspension with high solid content and low viscosity, preparation method and application thereof, and preparation method of polyacrylonitrile-based carbon fiber
  • Polyacrylonitrile suspension with high solid content and low viscosity, preparation method and application thereof, and preparation method of polyacrylonitrile-based carbon fiber
  • Polyacrylonitrile suspension with high solid content and low viscosity, preparation method and application thereof, and preparation method of polyacrylonitrile-based carbon fiber

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preparation example Construction

[0056] The present invention also provides a preparation method for the polyacrylonitrile suspension described in the above technical scheme, comprising the following steps:

[0057] mixing the preparation raw materials to obtain the mixed raw materials;

[0058] performing a polymerization reaction on the mixed raw materials to obtain the polyacrylonitrile suspension with high solid content and low viscosity;

[0059] The temperature of the polymerization reaction is 30-100° C., and the time is 0.5-24 hours; after the polymerization reaction, the total conversion rate of acrylonitrile, the first auxiliary monomer and the second auxiliary monomer is 15-90%.

[0060] The invention mixes the preparation raw materials to obtain the mixed raw materials. In the present invention, the mixing preferably includes the following steps:

[0061] mixing the initiator and part of the polymerization medium to obtain an initiator solution;

[0062] Mixing the preparation raw materials excep...

Embodiment 1

[0103] 38.8 parts of acrylonitrile, 0.4 part of itaconic acid, 0.8 part of methyl acrylate and 55 parts of N,N-dimethylacetamide were stirred for 5 minutes under nitrogen protection and a rotating speed of 150r / min to obtain primary mixed raw materials; 0.04 parts of azobisisobutyronitrile and 4.98 parts of N,N-dimethylacetamide were mixed to obtain an initiator solution; Stir for 2min to obtain mixed raw materials;

[0104] The mixed raw material is under the protection of nitrogen, the rotating speed is 150r / min, the temperature is 65°C, and the relative pressure is 0MPa, and the polymerization reaction is carried out for 4h (the total mass conversion rate of the polymerized monomer is 70%), and the solid content is obtained. 31.8%, a polyacrylonitrile suspension with a viscosity of 30 Pa s (the number average molecular weight of polyacrylonitrile is 13 × 10 4 g / mol).

Embodiment 2

[0106] The polyacrylonitrile suspension was prepared according to the method of Example 1 (solid content was 25%, the total mass conversion rate of polymerized monomers was 50%, the viscosity was 26 Pa s, and the number average molecular weight of polyacrylonitrile was 17 × 10 4 g / mol), the difference is that the initiator is adjusted to azobisisoheptanonitrile, and the polymerization temperature is limited to 55°C.

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Abstract

The invention belongs to the technical field of carbon fibers, and particularly relates to a polyacrylonitrile suspension with high solid content and low viscosity, a preparation method and application thereof, and a preparation method of a polyacrylonitrile-based carbon fiber. The polyacrylonitrile suspension with high solid content and low viscosity provided by the invention has the advantages of high monomer concentration and low viscosity of a polymerization system, and is beneficial to the rate of uniform dispersion of supplemented polymerization monomers during continuous polymerization and the transfer of polymerization reaction heat; and the formed small particles are beneficial to long-time survival of active free radical chains, rapid polymerization and preparation of polyacrylonitrile with high molecular weight can be realized, and a homogeneous polyacrylonitrile spinning solution with low viscosity and high mass concentration can be further formed through subsequent demonomerisation and defoaming. The polyacrylonitrile fiber and the polyacrylonitrile-based carbon fiber which are prepared by spinning with the high-mass-concentration homogeneous polyacrylonitrile spinning solution provided by the invention have relatively high monofilament tensile strength.

Description

technical field [0001] The invention belongs to the technical field of carbon fibers, and in particular relates to a high-solid-content, low-viscosity polyacrylonitrile suspension, a preparation method and application thereof, and a preparation method of polyacrylonitrile-based carbon fibers. Background technique [0002] Due to its simple production process, low production cost and excellent mechanical properties, polyacrylonitrile-based carbon fiber has become a carbon fiber with the fastest development, the highest output, the most varieties and the most widely used. It has been widely used in aerospace, national defense technology, construction, sporting goods and medical equipment and other fields. [0003] The main preparation methods of polyacrylonitrile carbon fiber in industry are divided into homogeneous solution polymerization and aqueous phase suspension polymerization. Chinese patents CN200910234654.X, CN200910234653.5, CN201210058764.7, CN201510434049.2, CN201...

Claims

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Application Information

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IPC IPC(8): C08F220/46C08F222/02C08F220/14C08F220/56D01F6/38D01F9/22
CPCC08F220/46D01F6/38D01F9/22C08F222/02C08F220/14C08F220/56
Inventor 付中禹张会轩闫慧洁徐哲
Owner 吉林碳谷碳纤维股份有限公司
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