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Multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof

A binary ammoniated polyacrylonitrile-based carbon fiber and spinning solution technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, and can solve the conditions of low-cost, high-efficiency large-scale industrial preparation and polymerization reaction process control that are not applicable Harsh requirements, complex comonomers in the preparation process, etc., to achieve the effect of improving structural compactness, improving hydrophilicity, and improving hydrophilicity

Active Publication Date: 2012-10-17
XIAN KANGBEN MATERIAL
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Problems solved by technology

Methyl acrylate can reduce the cohesive energy between polyacrylonitrile macromolecules, improve the spinnability of spinning solution, and at the same time, due to the volume effect of ester group, it can enhance the oxygen permeability during the pre-oxidation process, slow down or eliminate the skin-core structure formation; itaconic acid can reduce the activation energy of the reaction, promote cyclization and crosslinking, ease the pre-oxidation exothermic reaction, and prepare homogeneous pre-oxidized silk, but the hydrophilicity of itaconic acid is not very good. Therefore, in order to To improve the hydrophilicity of spinning solution, itaconic acid needs to be modified
[0004] In the patents No. 200510016572.X and CN200710056082.1, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences proposed two high-hydrophilic spinning solutions and preparation methods for high-performance polyacrylonitrile-based carbon fibers. In the polymerization process, itaconic acid and β-itaconic acid amide were used as comonomers or vinylimidazolium salts, itaconic acid, acrylic acid and methacrylic acid were used as comonomers. Polymerize monomers, introduce hydrophilic groups such as amide groups into the polymerization system, prepare highly hydrophilic carbon fiber spinning solution, and finally prepare precursors and carbon fibers with regular circular cross-sections and high strength, but the two methods The preparation process of the comonomers used is complicated or there are many types of comonomers required, which is not suitable for low-cost, high-efficiency large-scale industrial preparation
In the patents CN200510012581.1 and CN201010598880.9, the Shanxi Institute of Coal Chemistry, Chinese Academy of Sciences proposed a method for preparing a ternary copolymerization highly hydrophilic polyacrylonitrile spinning stock solution. Add acrylamide solution at a continuous speed to increase the hydrophilicity of the spinning solution, improve the polymer spinnability and the oxidizability of the precursor, but the polymerization operation of this method is cumbersome, and acrylamide is used as the polymerization monomer. Gel is easy to form during the process, and the control conditions of the polymerization reaction process are demanding

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  • Multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof
  • Multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof
  • Multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof

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Embodiment 1

[0028] This embodiment is a binary ammoniated polyacrylonitrile-based carbon fiber spinning solution and its preparation method.

[0029] In this embodiment, dimethyl sulfoxide is used as a solvent, azobisisobutyronitrile is used as an initiator, acrylonitrile and itaconic acid are used as polymer monomers, and the percentage of the monomers in the total weight of the solution is 20-22%. Acrylonitrile: the weight percent of itaconic acid is 97~98.0:3.0~2.0, and the consumption of azobisisobutyronitrile is 0.75~0.9% by weight of the total amount of monomers. Both the itaconic acid and azobisisobutyronitrile are solid. In this embodiment, the monomer accounts for 20% of the total weight of the solution, the weight percentage of acrylonitrile:itaconic acid is 98.0:2.0, and the amount of azobisisobutyronitrile is 0.75% by weight of the total monomer.

[0030] During preparation, proceed as follows:

[0031] Step 1, weighing materials. The dimethyl sulfoxide solvent accounting f...

Embodiment 2

[0038] This embodiment is a binary ammoniated polyacrylonitrile-based carbon fiber spinning solution and its preparation method.

[0039] In this example, dimethyl sulfoxide is used as a solvent, azobisisobutyronitrile is used as an initiator, acrylonitrile and itaconic acid are used as polymer monomers, and the weight percentage of the monomers in the total weight of the solution is 20-22%. , acrylonitrile: the weight percent of itaconic acid is 97~98.0:3.0~2.0, and the consumption of azobisisobutyronitrile is 0.75~0.9% by weight of the total amount of monomers. Both the itaconic acid and azobisisobutyronitrile are solid. In the present embodiment, the weight percentage of monomers accounting for the total weight of the solution is 21%, the weight percentage of acrylonitrile:itaconic acid is 97.5:2.5, and the consumption of azobisisobutyronitrile is 0.85% by weight of the total amount of monomers .

[0040] During preparation, proceed as follows:

[0041] Step 1, weighing ...

Embodiment 3

[0048] This embodiment is a ternary ammoniated polyacrylonitrile-based carbon fiber spinning solution and its preparation method.

[0049] In this embodiment, dimethyl sulfoxide is used as a solvent, azobisisobutyronitrile is used as an initiator, and acrylonitrile, itaconic acid, and 2-acrylamide-2-methylpropanesulfonic acid are used as polymer monomers. The percentage by weight of the monomer accounting for the total weight of the solution is 20-22%, and the percentage by weight of acrylonitrile: itaconic acid: 2-acrylamide-2-methylpropanesulfonic acid is 97.5-98.0:1.5-2.0:0.5, and the polymerized monomer The total amount is 100%, and the amount of azobisisobutyronitrile is 0.75-0.9% by weight of the total amount of monomers. The itaconic acid, azobisisobutyronitrile and 2-acrylamide-2-methylpropanesulfonic acid are all solid. In the present embodiment, the weight percentage of the monomer accounting for the total weight of the solution is 21%, the weight percentage of acry...

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Abstract

The invention discloses a multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and a preparation method of the multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution. The preparation method comprises the steps of combining acrylonitrile, methyl acrylate, 2-acrylamide-2-methylpro panesulfonic acid and itaconic acid to be a polymer monomer, respectively and sufficiently dissolving the weighed solid monomer (itaconic acid) and an initiator (azodiisobutyronitrile) into a dimethyl sulfoxide solution; conducting ammoniation on the dimethyl sulfoxide solution of the itaconic acid by ammonia water; and sequentially adding all the materials into a polymerizing pot, adding the initiator (azodiisobutyronitrile) to conduct batch polymerization reaction, gathering, defoaming and filtering to obtain the multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution. According to the multiple-ammoniation polyacrylonitrile-based carbon fiber spinning solution and the preparation method, the comonomer structure of a multiple-copolymerization system is changed by the ammonia water, and dimethyl sulfoxide is taken as a solvent for homogeneous solution polymerization to prepare the polyacrylonitrile-based carbon fiber spinning solution, so that the hydrophily of the spinning solution is improved, and further, the high-performance fiber with high structure compacting degree, good mechanical property and high bonding strength is obtained.

Description

technical field [0001] The invention relates to a preparation method of a polyacrylonitrile-based carbon fiber spinning solution, in particular to a polyacrylonitrile-based carbon fiber spinning solution and a preparation method thereof. Background technique [0002] Carbon fiber is a high-strength special fiber with a carbon content greater than 90%. Due to its high strength, high modulus, high temperature resistance, fatigue resistance, electrical conductivity, and thermal conductivity, it is widely used in cutting-edge fields such as aerospace, national defense, and national economy. Many fields of construction. The main raw material of high-performance carbon fiber is polyacrylonitrile-based precursors. Polymerization is the first step in the preparation of precursors. High-quality polymer solution is the prerequisite for the preparation of high-performance precursors. Adjust the characteristics of polymerized comonomers to improve the spinning solution. The hydrophilic...

Claims

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Application Information

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IPC IPC(8): D01F9/22C08F220/46C08F220/48
Inventor 韩笑王增加王华沈涛张文发彭卫东
Owner XIAN KANGBEN MATERIAL
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