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Preparation method of narrow-distribution polyacrylonitrile-based carbon fiber spinning solution

A polyacrylonitrile-based carbon fiber and spinning dope technology, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of wide molecular weight distribution of polyacrylonitrile, long reaction time, high residual monomer content, and achieve polymerization reaction time. The effect of shortening, reducing residues, reducing half-life

Active Publication Date: 2020-01-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the problems of wide polyacrylonitrile molecular weight distribution, high residual monomer content and long reaction time in the prior art. It provides a preparation of spinning dope for narrow distribution polyacrylonitrile-based carbon fiber The method has the advantages of narrow molecular weight distribution of polyacrylonitrile, low residual monomer content of spinning dope and short polymerization reaction time, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 990 g of distilled acrylonitrile (AN), 5 g of itaconic acid (IA), 2.5 g of sodium methacrylate, 5 g of azobisisobutyronitrile (AIBN) and 3900 g of dimethylsulfoxide (DMSO) were added to Stir the reactor evenly, close the reactor, and start the constant temperature reaction under the protection of nitrogen under a slight positive pressure, and control the reaction temperature to 60°C. When the conversion rate reaches 70%, raise the temperature by 5°C to 65°C, and continue the reaction; when the conversion rate reaches 90%, raise the temperature by 5°C to 70°C, and continue the reaction; when the conversion rate reaches 95%, stop the polymerization, The total polymerization time was 22 hours. Start stripping for 8 hours, control the temperature at 70°C, and the pressure at 200Pa; let stand for defoaming for 12 hours, control the temperature at 75°C, and the pressure at 150Pa.

[0032] The molecular weight of the spinning stock solution is 70,000, the molecular weight dis...

Embodiment 2

[0034] 1210 g of distilled acrylonitrile (AN), 27.5 g of methyl methacrylate, 2 g of sodium propylene sulfonate, 7.5 g of azobisisobutyronitrile (AIBN) and 3760 g of dimethylsulfoxide (DMSO) were charged to the reactor , stir evenly, close the reactor, and start the constant temperature reaction under the protection of helium under a slight positive pressure, and control the reaction temperature to 65°C. When the conversion rate reaches 65%, raise the temperature by 5°C to 70°C, and continue the reaction; when the conversion rate reaches 85%, raise the temperature by 10°C to 80°C, and continue the reaction; when the conversion rate reaches 90%, stop the polymerization, The total polymerization time was 20 hours. Start stripping for 8 hours, control the temperature at 75°C, and the pressure at 300Pa; let stand for defoaming for 12 hours, control the temperature at 75°C, and the pressure at 200Pa.

[0035] The molecular weight of the spinning stock solution is 60,000, the molec...

Embodiment 3

[0037]Add 1460g of distilled acrylonitrile (AN), 30g of acrylamide, 15g of sodium methacrylate, 9g of azobisisobutyronitrile (AIBN) and 3500g of dimethyl sulfoxide (DMSO) into the reactor and stir evenly , close the reactor, start the constant temperature reaction under the protection of argon under a slight positive pressure, and control the reaction temperature to 62°C. When the conversion rate reaches 60%, raise the temperature by 10°C to 72°C, and continue the reaction; when the conversion rate reaches 80%, raise the temperature by 5°C to 77°C, and continue the reaction; when the conversion rate reaches 95%, stop the polymerization, The total polymerization time was 22 hours. Start stripping for 8 hours, control the temperature at 70°C, and the pressure at 100Pa; let stand for defoaming for 12 hours, control the temperature at 75°C, and the pressure at 100Pa.

[0038] The molecular weight of the spinning stock solution is 80,000, the molecular weight distribution is 3.7, ...

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Abstract

The invention relates to a preparation method of a narrow-distribution polyacrylonitrile-based carbon fiber spinning solution. The preparation method of the narrow-distribution polyacrylonitrile-basedcarbon fiber spinning solution mainly solves the problems of wide molecular weight distribution of polyacrylonitrile, high residual monomer content and long polymerization reaction time in the priorart. The preparation method of the narrow-distribution polyacrylonitrile-based carbon fiber spinning solution includes the following steps that (1) polymerization raw material acrylonitrile, a comonomer 1 and / or a comonomer 2, a solvent and an initiator are added into a reactor, a thermostatic reaction is started under the protection of inert gas to the reaction materials, and a reaction temperature is controlled to 60-65 DEG C; (2) when the conversion rate exceeds T1, the temperature is increased by 5-10 DEG C; (3) when the conversion rate exceeds T2, the temperature is increased by 5-10 DEGC; and (4) when the conversion rate reaches T3, the reaction is finished, and preparation of the spinning solution is completed. According to the technical scheme, the problems of wide molecular weight distribution of polyacrylonitrile, high residual monomer content and long polymerization reaction time are well solved, and the preparation method can be used in the industrial production of the polyacrylonitrile-based carbon fiber spinning solution.

Description

technical field [0001] The invention belongs to a preparation method of narrow distribution polyacrylonitrile-based carbon fiber spinning stock solution. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] The premise of producing high-performance carbon fiber is to use high-quality polyacrylonitrile precursor, and the prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F220/14C08F220/56C08F222/02C08F228/02C08F220/42D01F9/22
CPCC08F220/44D01F9/22C08F220/14C08F228/02C08F220/56C08F222/02C08F220/42
Inventor 沈志刚王贺团李磊缪金根
Owner CHINA PETROLEUM & CHEM CORP
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