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Spinning solution containing silicon acrylonitrile copolymer and preparation method thereof

A technology for spinning dope and acrylonitrile is applied in the field of polyacrylonitrile-based high-performance carbon fiber spinning dope and its preparation to achieve the effect of improving compact structure and large bond energy

Active Publication Date: 2013-04-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of silicon-based compounds with active sites into the acrylonitrile copolymer system for carbon fibers has not been reported in the literature

Method used

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  • Spinning solution containing silicon acrylonitrile copolymer and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Using dimethyl sulfoxide as a solvent, azobisisobutyronitrile as an initiator, acrylonitrile as the main monomer, methacrylic acid as comonomer 1, and vinyltrimethoxysilane as comonomer 2 to carry out acrylonitrile solution copolymerization Polymerization. Solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer 1 methacrylic acid, comonomer 2 vinyltrimethoxysilane and azobisisobutyronitrile are added respectively in the polymerization kettle. The weight ratio of added raw material is acrylonitrile: methacrylic acid: vinyltrimethoxysilane=98: 1: 1, and the consumption of azobisisobutyronitrile accounts for 0.8% of total monomer weight, controls monomer to account for total solution. 20% by weight. The mixture was stirred uniformly at room temperature, then bubbled with nitrogen for 20 minutes, and reacted at 63° C. for 25 hours. At a reaction temperature of 65°C and a vacuum of 0.090 MPa, the singlets are removed by a wiper-type singlet removal device, and af...

Embodiment 2

[0027] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer 1 acrylic acid, the comonomer 2 vinyltriacetylsilane and the initiator azobisisobutyronitrile are sequentially added to the polymerization kettle, and the added raw materials The weight ratio is acrylonitrile:acrylic acid:vinyltriacetylsilane=97:2:1, the amount of azobisisobutyronitrile accounts for 1.2% of the total weight of the monomers, and the monomers account for 22% of the total weight of the solution. The mixture was stirred uniformly at room temperature, then bubbled with nitrogen gas for 20 minutes, and reacted at 60° C. for 25 hours. At a reaction temperature of 60°C and a vacuum of 0.098 MPa, the singlets are removed by a wiper-type singlet removal device, and after static defoaming at 40°C, a silicon-containing acrylonitrile copolymer spinning stock solution is obtained. The molecular weight of the copolymer measured by gel permeation chromatography (GPC) is 206,000, and the molec...

Embodiment 3

[0029]The solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer 1 itaconic acid, comonomer 2 vinyltrichlorosilane and azobisisobutyronitrile are sequentially added to the polymerization kettle, and the weight ratio of the raw materials added is It is: acrylonitrile: itaconic acid: vinyltrichlorosilane = 90:5:5, the amount of azobisisobutyronitrile accounts for 2.0% of the total weight of the monomer, and the control monomer accounts for 25% of the total weight of the solution. The mixture was stirred and mixed at room temperature, followed by bubbling nitrogen gas for 20 minutes, and reacted at a temperature of 50° C. for 30 hours. At a reaction temperature of 68°C and a vacuum of 0.085 MPa, the singlets are removed by a wiper-type singlet removal device, and after static defoaming at 48°C, a silicon-containing acrylonitrile copolymer spinning stock solution is obtained. The molecular weight of the copolymer measured by gel permeation chromatography (GPC) is 112,00...

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Abstract

The invention relates to a spinning solution containing silicon acrylonitrile copolymer, which comprises a main monomer acrylonitrile, a comonomer 1, a comonomer 2, an initiator azodiisobutyronitrile, and an organic solvent, wherein the weight proportion of main monomer to comonomer 1 to comonomer 2 is (90.0-99.5):(0.25-5.0):(0.25-5.0); the usage of the initiator azodiisobutyronitrile is 0.3-2.0%of the total weight of the monomer; and the total monomer is 15-25% of the weight of the solution. The spinning solution provided by the invention has the advantages of capabilities of improving the compact structure of precursor yarn, forming a molecular oxygen diffusion channel, and being used for preparing uniform oxidative stabilization fibers and high-property carbon fibers.

Description

technical field [0001] The invention belongs to an acrylonitrile copolymer spinning stock solution and a preparation method thereof, in particular to a polyacrylonitrile-based high-performance carbon fiber spinning stock solution containing vinyl silane structural units and a preparation method thereof. technical background [0002] The advent of high-performance carbon fiber marks another breakthrough in the history of material development. It has excellent properties such as high specific strength, high specific modulus, ablation resistance, wear resistance, and fatigue resistance. As the most important reinforcing material in the field of advanced composite materials, it is widely used in various fields such as military and civilian industries. Compared with viscose-based and pitch-based carbon fibers, polyacrylonitrile-based carbon fibers have been vigorously developed due to their simple production process and good product mechanical properties, and have become the main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F9/22D01D1/02C08F220/44C08F230/08
Inventor 吕春祥李永红王鹏卢慧斌段晋星安锋袁淑霞
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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