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Spinning method of spinning solution with narrow molecular-weight distribution

A technology of narrow molecular weight distribution and spinning dope, which is applied in spinning solution preparation, stretch spinning, textiles and papermaking, etc., can solve problems such as broken filaments and multi-fiber CV value, reduce residue, improve mass transfer and transfer Effects of thermal efficiency and half-life reduction

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

[0006] The technical problem to be solved by the present invention is the problem of many broken filaments in the coagulation bath and large fiber CV value in the prior art, and a spinning method of spinning dope with narrow molecular weight distribution is provided, which has polyacrylonitrile precursor The dispersion coefficient of mechanical properties is low and the mass of broken wires in the coagulation bath is small, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037](1) Preparation of spinning stock solution: Distilled 99kg acrylonitrile (AN), 0.5kg itaconic acid (IA), 0.25kg sodium methacrylate, 0.5kg azobisisobutyronitrile (AIBN) and 390kg Add dimethyl sulfoxide (DMSO) into the reactor, stir evenly, close the reactor, 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.

[0038] The molecular weight of the spinning stock solution is 70,000, ...

Embodiment 2

[0045] (1) 121kg of distilled acrylonitrile (AN), 2.75kg of methyl methacrylate, 0.2kg of sodium propylene sulfonate, 0.75kg of azobisisobutyronitrile (AIBN) and 376kg of dimethyl sulfoxide (DMSO) Add it into 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.

[0046] The molecular weight of the spinning stock solution is 60,000, the mole...

Embodiment 3

[0053] (1) Preparation of spinning stock solution: 146kg of distilled acrylonitrile (AN), 3kg of acrylamide, 1.5kg of sodium methacrylate, 0.9kg of azobisisobutyronitrile (AIBN) and 350kg of dimethyl sulfoxide (DMSO) was added to the reactor, stirred evenly, the reactor was closed, and the constant temperature reaction was started under the protection of argon under a slight positive pressure, and the reaction temperature was controlled at 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.

[0054] The molecular weight of the sp...

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Abstract

The invention relates to a spinning method of spinning solution with narrow molecular-weight distribution, primarily solving the problem of great yarn break and high CV-value of fiber in coagulating bath of the prior art. The technical scheme refers that the spinning method includes the steps of introducing polymerization raw material acrylonitrile, comonomer 1 and / or comonomer 2, solvents and initiators into a reactor, performing thermostatic reaction with reactive material in protection of inert gas, while controlling the reaction temperature within 60-65 DEG C; rising temperature by 5-10 DEG C when the conversion rate is higher than T1, and continuing to perform reaction; rising temperature by 5-10 DEG C when the conversion rate is higher than T2, and continuing to perform reaction; finishing the polymerization reaction when the conversion rate reaches T3, performing demonomer and deaeration to obtain the spinning solution; coagulating and shaping, drafting, washing, oil applying, drying and compacting, drafting in steam, heat setting with steam, and rolling up to obtain a polyacrylonitrile precursor. The spinning method solves the above problem effectively and can be applied toindustrial production of the polyacrylonitrile-based carbon fiber precursor.

Description

technical field [0001] The invention belongs to a method for preparing polyacrylonitrile raw silk for carbon fiber, in particular to a method for spinning a spinning dope with narrow molecular weight distribution. Background technique [0002] Since the 1950s, developed countries have urgently needed new structural materials and corrosion-resistant materials in order to develop large-scale rockets and artificial satellites and comprehensively improve aircraft performance, so that carbon fibers reappeared on the stage of new materials, and gradually formed PAN-based carbon fibers. The three major raw material systems of viscose-based carbon fiber and pitch-based carbon fiber. Because the production process of PAN-based carbon fiber is simpler than other methods, and the mechanical properties of the product are good, it has been developed rapidly and has become the mainstream of the current production of carbon fiber. [0003] PAN-based carbon fiber has excellent properties s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D13/00D01D1/02D01D5/14D01D10/02D01F9/22
CPCD01D1/02D01D5/14D01D10/02D01D13/00D01F9/22
Inventor 王贺团沈志刚陈辉赵微微
Owner CHINA PETROLEUM & CHEM CORP