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Preparing method of polyacrylonitrile (PAN) used for carbon fiber

A polymer, carbon fiber technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the adverse effects of PAN polymer thermal stability spinnable fibers physical properties, affect the spinnability and the improvement of pre-oxidation controllability effect, uneven distribution and other problems, to achieve the effect of shortening the polymerization reaction time, low cost and reducing production cost

Active Publication Date: 2014-12-24
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the ternary copolymerization system, due to the difference in reactivity between acrylonitrile and the second and third comonomers, it often leads to uneven distribution of comonomers on the PAN molecular chain, which affects its spinnability and prepolymerization. Improvement effect of oxidation controllability
[0006] In addition, inorganic initiators are often used as polymerization initiators in aqueous phase polymerization, but there are two problems with the commonly used inorganic initiators at present (1) high cost; (2) other metal elements are contained in the initiator, and these metal elements are The elements exist in the PAN polymer in the form of ions, which will have adverse effects on the thermal stability of the PAN polymer, the spinnability during spinning and fiber production, and the physical properties of the fiber.

Method used

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  • Preparing method of polyacrylonitrile (PAN) used for carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Deionized water, acrylonitrile, monomethyl itaconate, ammonium persulfate, sodium bisulfite, and ferrous sulfate were weighed and then added to a polymerization kettle with a stirrer and a jacketed constant temperature water system. Taking the quality of water as a benchmark, the mass percentage of acrylonitrile relative to water is 20%, the relative mass percentage of itaconate monomethyl ester to acrylonitrile is 8%, the relative mass percentage of ammonium persulfate to acrylonitrile is 0.6%, hydrogen sulfite The mass percentage of sodium relative to acrylonitrile is 0.8%, and the mass ratio of ferrous sulfate to acrylonitrile is 1 ppm. Sulfuric acid was used to adjust the pH value to 2.5, and the reaction was carried out for 50 min at a temperature of 58° C. and a stirring speed of 60 rpm. After the reaction, the pH value of the polymerization system was adjusted to 8.5 with ammonia water. Then filter, wash and dry to obtain PAN polymer powder.

[0029] After test...

Embodiment 2

[0032] Deionized water, acrylonitrile, monoethyl itaconate, ammonium persulfate, sodium bisulfite, and ferrous sulfate were weighed and then added to a polymerization kettle with a stirrer and a jacketed constant temperature water system. Taking the quality of water as a benchmark, the relative mass percentage of acrylonitrile to water is 22%, the relative mass percentage of itaconate monoethyl ester to acrylonitrile is 4%, the relative mass percentage of ammonium persulfate to acrylonitrile is 0.7%, hydrogen sulfite The mass percentage of sodium relative to acrylonitrile is 1.2%, and the mass ratio of ferrous sulfate to acrylonitrile is 3ppm. Sulfuric acid was used to adjust the pH value to 3.5, and the reaction was carried out for 70 min at a temperature of 60° C. and a stirring speed of 80 rpm. After the reaction, the pH value of the polymerization system was adjusted to 9 with ammonia water. Then filter, wash and dry to obtain PAN polymer powder.

[0033] After testing, ...

Embodiment 3

[0036] Add deionized water, acrylonitrile, mono-n-propyl itaconate, ammonium persulfate, sodium bisulfite, ferrous sulfate, and weigh them in sequence to a polymerization kettle with a stirrer and a jacketed constant temperature water system. Taking the quality of water as a benchmark, the relative mass percentage of acrylonitrile to water is 24%, the relative mass percentage of itaconate mono-n-propyl ester to acrylonitrile is 2%, the relative mass percentage of ammonium persulfate to acrylonitrile is 1.6%, sulfurous acid The mass percentage of sodium hydrogen relative to acrylonitrile is 1.8%, and the mass ratio of ferrous sulfate to acrylonitrile is 5ppm. Sulfuric acid was used to adjust the pH value to 2.5, and the reaction was carried out for 50 min at a temperature of 62° C. and a stirring speed of 100 rpm. After the reaction, the pH value of the polymerization system was adjusted to 10 with ammonia water. Then filter, wash and dry to obtain PAN polymer powder.

[0037...

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Abstract

A preparing method of polyacrylonitrile (PAN) used for carbon fiber is provided. The preparing method adopts a water-phase precipitation polymerization reaction, adopts water-soluble ammonium sulfate-sodium bisulfite-ferrous sulfate as an oxidation-reduction initiation system, adopts a monoester of itaconic acid as a bifunctional copolymerization monomer, and adopts sulfuric acid as a pH conditioner. The bifunctional copolymerization monomer and acrylonitrile are subjected to a precipitation polymerization reaction in a water phase, then the reaction system is alkalified by aqueous ammonia, and after separation, washing and drying, PAN powder is obtained. The preparing method is low in cost, short in polymerization time, and high in production efficiency, and the prepared polyacrylonitrile is high in purity and good in spinnability and preoxidation controllability, so that the preparing method is suitable for large-scale production of carbon fiber precursor and facilitates reduction of the production cost of carbon fiber.

Description

technical field [0001] The invention relates to the technical field of carbon fiber preparation, in particular to a preparation method of polyacrylonitrile (PAN) polymer for carbon fiber. Background technique [0002] Carbon fiber is a well-known high-tech fiber material with a series of excellent properties such as high specific strength, high specific modulus, high temperature resistance, corrosion resistance, good electrical and thermal conductivity, and small thermal expansion coefficient. Advanced composite materials reinforced with carbon fiber have played an irreplaceable role in key components of military and civil aircraft, as well as strategic missiles and launch vehicles. In recent years, with the increasingly prominent problems of energy shortage and environmental pollution, the lightweight automobile technology using carbon fiber composite materials has attracted more and more attention. Using carbon fiber reinforced resin-based composite materials instead of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/46C08F222/16C08F4/40D01F9/22
Inventor 欧阳琴陈友汜皇静黄显雯莫高明杨建行
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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