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Method for measuring acrylonitrile monomer content in polyacrylonitrile polymer fluid

A technology for polyacrylonitrile and monomer content, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problems of large subjective randomness and large errors, and achieve the effect of convenient and easy determination of the method.

Inactive Publication Date: 2010-10-20
XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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Problems solved by technology

[0003] The purpose of the present invention is to provide a quick and accurate measurement method for measuring residual acrylonitrile monomer content in polyacrylonitrile polymerization liquid, which solves the relatively subjective arbitrariness of the existing measurement method for monomer content in polyacrylonitrile polymerization liquid. Large technical problems resulting in large errors,

Method used

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Embodiment

[0031] Pipette 6 samples of the same polyacrylonitrile polymer solution of 15ml and place them in six 25ml headspace bottles, tighten the bottle caps with polytetrafluoroethylene, shake well; place them in a constant temperature water bath at 80°C, and heat for 30 Minutes, during which the headspace bottle was shaken 3 times, and 3ml of headspace was extracted rapidly with a 3ml syringe and injected into a gas chromatograph for experimentation; ℃, sampling temperature: 170 ℃, hydrogen flow rate 30ml / min, air flow rate 400ml / min, high-purity nitrogen (99.999%) flow rate 30ml / min, detector: hydrogen flame ionization detector, 180 ℃, gas sample volume 3ml) to measure the peak area of ​​acrylonitrile; calculate the concentration of acrylonitrile in the polyacrylonitrile polymerization liquid to be measured by external standard method and be respectively: 14.5mg / L, 14.3mg / L, 13.9mg / L, 14.8mg / L, 13.7mg / L, 14.2mg / L, the average value was 14.23mg / L, and the standard deviation (SD) of ...

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Abstract

The invention discloses a method for measuring the acrylonitrile monomer content in polyacrylonitrile polymer fluid, which comprises the following steps: 1) preparing polyacrylonitrile polymer fluid with standard acrylonitrile content; 2) preparing a standard acrylonitrile content curve; 3) obtaining a chromatogram map of residue acrylonitrile monomer in the polyacrylonitrile polymer fluid to be measured; and 4) measuring the residue acrylonitrile monomer in the polyacrylonitrile polymer fluid to be measured: adopting a static-state headspace method as an enrichment method of samples. The invention solves the technical problem that the existing method for measuring the acrylonitrile monomer content in polyacrylonitrile polymer fluid has larger error caused by large subjective arbitrariness, is convenient and feasible, and can quickly and accurately analyze the content of the residue acrylonitrile monomer in the polyacrylonitrile polymer fluid according to the requirements.

Description

technical field [0001] The invention belongs to the technical field of polymer testing methods, and in particular relates to a testing method for residual acrylonitrile monomer content in polyacrylonitrile polymerization liquid. Background technique [0002] Polyacrylonitrile (PAN) carbon fiber has been widely used in various fields due to a series of excellent properties. High-quality raw silk is the prerequisite for the production of high-performance carbon fibers. High-quality raw silk should have the characteristics of high purity, high strength, high degree of orientation, fine denier and no adhesion. The preparation of precursors includes two process steps of polymerization and spinning. Among them, polymerization is the source of carbon fiber production and one of the key steps to improve the quality of raw silk. Therefore, the performance of the polymerization solution directly affects the performance of the precursor. And the existence of polymerization monomer ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/60
Inventor 王浩静刘福杰范立东庞培东程璐王红飞李福平刘欢
Owner XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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