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A method for determining the content of residual acrylonitrile monomer in spinning dope during carbon fiber production

A technology for spinning stock solution and production process, which is applied in the field of determining the content of residual acrylonitrile monomer in spinning stock solution, and achieves the effects of simple method, easy judgment and convenient operation

Active Publication Date: 2019-04-16
ZHONGJIAN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And if it is a difficult problem to determine the content of residual acrylonitrile monomer in the spinning dope, there is no literature report at home and abroad how to determine the content of residual acrylonitrile in the spinning dope of polyacrylonitrile carbon fiber

Method used

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  • A method for determining the content of residual acrylonitrile monomer in spinning dope during carbon fiber production
  • A method for determining the content of residual acrylonitrile monomer in spinning dope during carbon fiber production
  • A method for determining the content of residual acrylonitrile monomer in spinning dope during carbon fiber production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A method for determining the content of residual acrylonitrile monomers in spinning dope during carbon fiber production, comprising the following steps:

[0040] (1) Weigh m on a ten-thousandth analytical balance 1 0.7037g polyacrylonitrile spinning dope is placed in a 250mL conical flask;

[0041] (2) Add 20mL dimethyl sulfoxide in the Erlenmeyer flask described in step (1);

[0042] (3) Add a magnetic stirrer to the Erlenmeyer flask, cover with a stopper, and place on an electromagnetic stirrer to stir and mix evenly;

[0043] (4) After the polyacrylonitrile spinning stock solution is completely dissolved, open the bottle stopper, add 50 mL of deionized water along the bottle wall of the Erlenmeyer flask, and stir evenly;

[0044] (5) After the solution in the Erlenmeyer flask is cooled, add 20mL of 0.5mol / L sodium sulfite solution into the Erlenmeyer flask and shake well; let stand for 10min;

[0045] (6) Add 6 drops of mixed indicator in the conical flask again, ...

Embodiment 2

[0069] A method for determining the content of residual acrylonitrile monomers in spinning dope during carbon fiber production, comprising the following steps:

[0070] (1) Weigh m on a ten-thousandth analytical balance 1 1.0325g polyacrylonitrile spinning dope is placed in a 250mL conical flask;

[0071] (2) Add 20mL dimethyl sulfoxide in the Erlenmeyer flask described in step (1);

[0072] (3) Add a magnetic stirrer to the Erlenmeyer flask, cover with a stopper, and place on an electromagnetic stirrer to stir and mix evenly;

[0073] (4) After the polyacrylonitrile spinning stock solution is completely dissolved, open the bottle stopper, add 50 mL of deionized water along the bottle wall of the Erlenmeyer flask, and stir evenly;

[0074] (5) After the solution in the Erlenmeyer flask is cooled, add 20mL of 0.5mol / L sodium sulfite solution into the Erlenmeyer flask and shake well; let stand for 10min;

[0075] (6) Add 6 drops of mixed indicator in the conical flask again, ...

Embodiment 3

[0099] A method for determining the content of residual acrylonitrile monomers in spinning dope during carbon fiber production, comprising the following steps:

[0100] (1) Weigh m on a ten-thousandth analytical balance 1 1.3984g polyacrylonitrile spinning dope is placed in a 250mL conical flask;

[0101] (2) Add 20mL dimethyl sulfoxide in the Erlenmeyer flask described in step (1);

[0102] (3) Add a magnetic stirrer to the Erlenmeyer flask, cover with a stopper, and place on an electromagnetic stirrer to stir and mix evenly;

[0103] (4) After the polyacrylonitrile spinning stock solution is completely dissolved, open the bottle stopper, add 50 mL of deionized water along the bottle wall of the Erlenmeyer flask, and stir evenly;

[0104] (5) After the solution in the Erlenmeyer flask is cooled, add 20mL of 0.5mol / L sodium sulfite solution into the Erlenmeyer flask and shake well; let stand for 10min;

[0105] (6) Add 6 drops of mixed indicator in the conical flask again, ...

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Abstract

The invention especially relates to a determination method for the content of residual acrylonitrile monomer in the spinning solution of carbon fiber production, belonging to the field of testing methods for chemicals. The determination method comprises the following steps: dividing a to-be-determined sample into a first to-be-determined sample and a second to-be-determined sample; adding sodium sulfite into the first to-be-determined sample, allowing acrylonitrile monomer in the first to-be-determined sample to react with sodium sulfite so as to produce alkali and titrating the first to-be-determined sample by using a standard sulfuric acid solution; titrating the second to-be-determined sample by using a sodium hydroxide aqueous alkali; and calculating the mass percentage content of the residual acrylonitrile monomer in the to-be-determined sample according to a formula; wherein the to-be-determined sample is the spinning solution of carbon fiber production. The method is simple and convenient to operate; a titration end point is easy to determine; and testing results are more accurate.

Description

technical field [0001] The invention relates to the field of chemical testing methods, in particular to a method for determining the content of residual acrylonitrile monomers in spinning dope during carbon fiber production. 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. [0003] Due to the process of producing carbon fiber, the spinning dope contains acrylonitrile monomer. If the content of residual acrylonitrile in the spinning stock solution is greater than 0.01%, the prepared polyacrylonitrile carb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 杨永岗
Owner ZHONGJIAN TECH CO LTD