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Method for preparing polyacrylonitrile spinning solution for high-performance carbon fiber in ionic liquid

A polyacrylonitrile spinning, ionic liquid technology, applied in the chemical characteristics of fibers, textiles and papermaking, bulk chemical production, etc. Wide range of speed, melting point, and the effect of improving production efficiency

Active Publication Date: 2010-06-30
ZHONGFU SHENYING CARBON FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The prepared polyacrylonitrile precursor contains metal sodium ions, which greatly reduces the performance of its carbon fiber
[0006] Chinese patent CN 1401675A discloses the use of organic solvent and water as the polymerization medium, which solves the problems of inhomogeneous polymerization system and slow polymerization speed, but the molecular weight and molecular weight distribution of polyacrylonitrile do not change significantly
[0007] Japanese patent JK. Zhao 63-35819 discloses a polyacrylonitrile using DMF and water as a polymerization medium to obtain a polyacrylonitrile with a weight average molecular weight of 800,000, and a molecular weight distribution of 3.4. Although the molecular weight is relatively large, the molecular weight distribution is still wide

Method used

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  • Method for preparing polyacrylonitrile spinning solution for high-performance carbon fiber in ionic liquid
  • Method for preparing polyacrylonitrile spinning solution for high-performance carbon fiber in ionic liquid
  • Method for preparing polyacrylonitrile spinning solution for high-performance carbon fiber in ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] At room temperature, acrylonitrile monomer, itaconic acid monomer and ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate were stirred to make them fully Mix and dissolve, then add a small amount of initiator AIBN, and pass nitrogen protection into the polymerization kettle. The temperature was raised to 58° C. for 4 hours, and the reaction conversion rate of the polymer was measured to be 65%.

[0041] Coagulate the polymer with normal temperature water whose volume is 5 times the volume of the reaction solution, wash 4 times with water at a temperature of 70°C and 3 times the mass of the solid matter, and vacuum dry at 65°C to constant weight. The viscosity-average molecular weight of the prepared polyacrylonitrile measured is 8.0×10 4 , the molecular weight distribution is 1.4.

[0042] Then use dimethyl sulfoxide as a solvent, the dissolution temperature is 65°C, the concentration of sulfoxide is 75%, the concentration of polyacrylonitrile powder is 25%, th...

Embodiment 2

[0044] At room temperature, stir the acrylonitrile monomer, itaconic acid monomer and ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate according to the mass fraction ratio of 20%, 1% and 79% respectively, and stir them to make them fully mixed Dissolve, then add a small amount of initiator AIBN, and pass nitrogen protection into the polymerization kettle. The temperature was raised to 55° C. for 4 hours and the reaction conversion rate of the polymer was measured to be 58%.

[0045] Coagulate the polymer with normal temperature water whose volume is 5 times the volume of the reaction solution, wash 4 times with water at a temperature of 70°C and 3 times the mass of the solid matter, and vacuum dry at 65°C to constant weight. The viscosity-average molecular weight of the prepared polyacrylonitrile measured is 9.6×10 4 , the molecular weight distribution is 1.6.

[0046] Then use dimethyl sulfoxide as a solvent, the dissolution temperature is 65°C, the concentratio...

Embodiment 3

[0048] At room temperature, stir the acrylonitrile monomer, itaconic acid monomer and ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate according to the mass fraction ratio of 20.5%, 0.5% and 79% respectively, and stir them to make them fully mixed Dissolve, then add a small amount of initiator AIBN, and pass nitrogen protection into the polymerization kettle. The temperature was raised to 58° C. for 4 hours, and the reaction conversion rate of the polymer was measured to be 69%.

[0049] Coagulate the polymer with normal temperature water whose volume is 5 times the volume of the reaction solution, wash 4 times with water at a temperature of 70°C and 3 times the mass of the solid matter, and vacuum dry at 65°C to constant weight. The viscosity-average molecular weight of the prepared polyacrylonitrile measured is 12.5×10 5 , the molecular weight distribution is 1.5.

[0050] Then use dimethyl sulfoxide as a solvent, the dissolution temperature is 65°C, the concen...

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Abstract

The invention relates to a method for a preparing polyacrylonitrile spinning solution for a high-performance carbon fiber in an ionic liquid. The method comprises the following steps: sequentially adding a monomer in an acrylonitrile binary copolymerization system or a monomer in an acrylonitrile ternary polymerization system into the ionic liquid, dissolving at the room temperature, adding an evocating agent, and charging inactive gas for free radical polyreaction, stopping the polyreaction with ice-bath after reaction, solidifying the polymerisate with water and obtaining the polyacrylonitrile material after repeated water rinsing, oven drying and purification, and mixing to dissolve the obtained polyacrylonitrile powder material with dimethyl sulfoxide as the solution, thereby obtaining the polyacrylonitrile spinning solution with high-performance carbon fiber. In the method, the ionic liquid is used as the reaction solvent, with a wide melting point range, thereby facilitating the control of the polymerization temperature, and greatly speeding up the polymerization; and the obtained polyacrylonitrile has high molecular weight and narrow molecular weight distribution, thereby facilitating the preparation of the polyacrylonitrile precursor with stable performance for carbon fiber, improving the productivity and reducing the cost.

Description

technical field [0001] The invention belongs to a method for preparing a high-performance fiber spinning stock solution, in particular to a method for preparing a high-performance carbon fiber polyacrylonitrile spinning stock solution in an ionic liquid. Background of the invention [0002] Carbon fiber has excellent characteristics such as high specific modulus, high specific strength, high temperature resistance, and corrosion resistance, and has been widely used in various fields. Polyacrylonitrile-based carbon fiber is a polymer with acrylonitrile as the main molecular chain structure unit, which is spun and then carbonized at high temperature. [0003] The high polymer polyacrylonitrile used to prepare polyacrylonitrile-based carbon fiber spinning dope can be divided into free radical polymerization, anionic polymerization, coordination polymerization, etc. according to its reaction mechanism. At present, free radical polymerization is the most widely used, and its imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F2/06D01F9/22
CPCY02P20/54
Inventor 张国良李怀京刘宣东金亮梁燕
Owner ZHONGFU SHENYING CARBON FIBER
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