Method for preparing carbon fiber precursor by polymerization from mixed solvent

A technology of carbon fiber precursors and mixed solvents, which is applied in the direction of wet spinning, etc., can solve the problems that the spinnability of carbon fiber precursors cannot be improved, it is not conducive to the preparation of high-performance carbon fiber precursors, and it cannot meet the requirements of T700 carbon fibers. Conducive to environmental protection, small fineness, and the effect of improving structural regularity

Inactive Publication Date: 2015-06-10
JIANGNAN UNIV
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Problems solved by technology

Chinese patents CN 102477121A and CN 102586921A disclose a method for preparing carbon fiber precursor spinning dope by solution polymerization using itaconic acid or acrylic acid as a comonomer; Chinese patent CN 101724922B discloses a method using itaconic acid as a Comonomer, dimethyl sulfoxide as a solvent solution polymerization method for preparing carbon fiber precursor; Chinese patent CN 103103631A discloses a method of preparing carbon fiber precursor by using ammonium itaconate as a comonomer, solution polymerization dry spray wet method method; in the above method, an acidic monomer is added as the second comonomer, which promotes the pre-oxidation reaction of the carbon fiber precursor, but without adding the lubricating ester monomer, the spinnability of the carbon fiber precursor cannot be obtained. Improvement, which is not conducive to the preparation of high-performance carbon fiber precursors
The viscosity-average molecular weight of the polymer obtained by solution polymerization in the above-mentioned published patents is less than 3.0 × 10 5 g / mol, which cannot meet the requirements of T700 carbon fiber; while the molecular weight of the polymer obtained by aqueous phase suspension polymerization is 8.0×10 5 ~1.2×10 6 g / mol, gels are prone to occur in the spinning process, and it is not easy to prepare high-performance carbon fiber precursors; for the above problems, Chinese patent CN 102517671A discloses a method for preparing high-performance carbon fiber precursors by a two-step method of aqueous phase suspension, but there are Complicated and complicated process defects

Method used

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  • Method for preparing carbon fiber precursor by polymerization from mixed solvent

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Experimental program
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Effect test

Embodiment 1

[0029] (1) Acrylonitrile, 3-carboxy-3-butenamide, and dimethyl itaconate are mixed evenly at a mass ratio of 98.2:1.5:0.3 and then added to the reactor (total concentration of mixed monomers is 16%), and then methyl Sulfoxide / deionized water (60 / 40wt / wt), finally add azobisisobutyronitrile (accounting for 0.7wt% of the total mass of mixed monomers), react at 60°C for 8 hours, and the prepared polyacrylonitrile molecular weight is 4.8×10 5 g / mol, the molecular weight distribution is 2.23. The above-mentioned polymer was dissolved, defoamed, and filtered (0.8 μm filter material) to obtain a spinning dope.

[0030] (2) step (1) is obtained spinning dope through dry jet wet spinning, the distance of air section is 10cm, and the temperature of air section is 10 ℃, and relative humidity is 65%, the dimethyl sulfoxide in coagulation bath The content is 60wt%, the temperature of the coagulation bath is 0 °C, and the coagulation time is 1 min; the first-level hot water (75 °C) draws ...

Embodiment 2

[0033] (1) Acrylonitrile, 3-carboxy-3-butenamide, and dimethyl itaconate are mixed evenly at a mass ratio of 98.2:1.5:0.3 and then added to the reactor (total concentration of mixed monomers is 16%), and then methyl Sulfoxide / deionized water (60 / 40wt / wt), finally add azobisisobutyronitrile (accounting for 0.6wt% of the total mass of mixed monomers), react at 60°C for 8 hours, and the prepared polyacrylonitrile molecular weight is 5.6×10 5 g / mol, the molecular weight distribution is 2.30. The above-mentioned polymer was dissolved, defoamed, and filtered (0.8 μm filter material) to obtain a spinning dope.

[0034] (2) Step (1) is obtained spinning dope through dry-spray wet spinning, and the distance of air section is 10cm, and the temperature of air section is 10 ℃, and relative humidity is 65%, and the dimethyl sulfoxide in coagulation bath The content is 60wt%, the temperature of the coagulation bath is 0 °C, and the coagulation time is 1 min; the first-level hot water (75 ...

Embodiment 3

[0036] (1) Acrylonitrile, 3-carboxy-3-butenamide, and dimethyl itaconate are mixed uniformly at a mass ratio of 98.7:1.0:0.3 and then added to the reactor (the total concentration of mixed monomers is 16%), and then methyl Sulfoxide / deionized water (60 / 40wt / wt), finally add azobisisobutyronitrile (accounting for 0.7wt% of the total mass of mixed monomers), react at 60°C for 8 hours, and the prepared polyacrylonitrile molecular weight is 5.2×10 5 g / mol, the molecular weight distribution is 2.24. The above-mentioned polymer was dissolved, defoamed, and filtered (0.8 μm filter material) to obtain a spinning dope.

[0037] (2) step (1) is obtained spinning dope through dry jet wet spinning, the distance of air section is 10cm, and the temperature of air section is 10 ℃, and relative humidity is 65%, the dimethyl sulfoxide in coagulation bath The content is 60wt%, the temperature of the coagulation bath is 0 °C, and the coagulation time is 1 min; the first-level hot water (75 °C)...

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Abstract

The invention relates to a method for preparing a carbon fiber precursor by polymerization from a mixed solvent. The method for preparing the carbon fiber precursor by polymerization from the mixed solvent comprises the following steps: (1) initiating copolymerization on acrylonitrile, 3-carboxyl-3 butylene amide and itaconic acid diester at the temperature of 50-80 DEG C while dimethyl sulfoxide/deionized water or N,N-dimethyl formamide/deionized water is taken as the solvent and azodiisobutyronitrile is taken as an initiating agent; and (2) dissolving an acrylonitrile polymer obtained in the step (1), defoaming, filtering, carrying out dry jet wet spinning, drawing, oiling, compacting by drying, drawing in superheated steam, and carrying out heat setting, so that the carbon fiber precursor is obtained. The method for preparing the carbon fiber precursor by the polymerization from the mixed solvent has the advantages that the characteristic that the chain transfer constant of the deionized water is zero is utilized, the molecular weight of the polymer is regulated and controlled by regulating the ratio of the deionized water to the organic solvent, the molecular weight of the prepared polymer is more than 1.5 times of the molecular weight of the polymer obtained by the polymerization from the traditional solvent, and the prepared carbon fiber precursor is uniform in structure, low in fineness and high in strength; meanwhile, water is adopted for substituting part of the organic solvent, the environment protection can be facilitated, and the production cost is effectively reduced.

Description

technical field [0001] The invention belongs to the field of carbon fiber precursor preparation, in particular to a method for preparing carbon fiber precursor by mixed solvent polymerization. technical background [0002] Carbon fiber has a series of superior physical, chemical and mechanical properties such as high specific strength, high specific modulus, heat resistance and low temperature resistance, chemical corrosion resistance, friction resistance, thermal conductivity, radiation resistance and good damping and shock absorption. An impressive new generation of reinforcements. At present, carbon fiber has been widely used in civilian industries such as construction, transportation, energy, advanced sporting goods, and medical equipment, as well as cutting-edge fields such as aerospace and national defense. [0003] Due to its excellent comprehensive performance and relatively simple production process, polyacrylonitrile-based carbon fiber has become a carbon fiber wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38D01D5/06D01F9/22C08F220/48C08F220/58C08F222/14C08F2/10C08F2/06
Inventor 巨安奇王舒琳汪月夏朝斌葛明桥
Owner JIANGNAN UNIV
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