Method for determining content of dimethyl sulfoxide in sample in purification process

A technology of dimethyl sulfoxide and purification process is applied in the field of carbon fiber solvent recovery to achieve the effect of saving detection cost and shortening detection time

Pending Publication Date: 2020-08-18
山西钢科碳材料有限公司 +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the deficiencies in the prior art and solve the technical problems of the method for quickly and accurately measuring the content of dimethyl sulfoxide in the feed tank and the c

Method used

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  • Method for determining content of dimethyl sulfoxide in sample in purification process
  • Method for determining content of dimethyl sulfoxide in sample in purification process
  • Method for determining content of dimethyl sulfoxide in sample in purification process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for determining the content of dimethyl sulfoxide in a purification process sample, comprising the following steps:

[0024] (a) Select coagulation bath sample solutions with different concentrations at the positions of the first, second and third bath coagulation baths after 2 days of normal production in the polyacrylonitrile-based carbon fiber spinning process, and use the iodometric method to titrate the dimethyl methoxide in the sample solution respectively. The content of sulfone, obtain the sample solution of known dimethyl sulfoxide content;

[0025] (b) Use the sample solution with known dimethyl sulfoxide content in step (a) to prepare dimethyl sulfoxide solutions with different contents, and use a refractive index meter to measure the refractive index of the prepared dimethyl sulfoxide solutions with different contents , draw the corresponding curve of the refractive index and the content of dimethyl sulfoxide, as a standard curve;

[0026] (c) Take...

Embodiment 2

[0029] Using the same steps as in Example 1, test the crude product tower top sample in the purification process of dimethyl sulfoxide, and titrate the dimethyl sulfoxide content with iodometric method to be 75.88%, and record the refractive index of the sample at the same time as 1.44978, drawing The corresponding curve of refractive index and dimethyl sulfoxide content at the crude product tower top position is as follows figure 2 As shown, the dimethyl sulfoxide content was found to be 75.44% on the standard curve.

Embodiment

[0030] Example data comparison:

[0031]

[0032] Conclusion: As can be seen from the above table, the content of dimethyl sulfoxide in the samples taken from the feed tank and the top of the crude product tower during the purification process measured by this method is compared with the value obtained by iodometric titration analysis. In comparison, the relative error is in the range of 1 to 2%. The same sample takes about 2 hours to be titrated by the traditional iodometric method, but it only takes about 5 minutes to use this method; this method can quickly determine dimethyl methylene During the sulfone purification process, the content of dimethyl sulfoxide in the samples taken from the feed tank, the top of the crude product tower, etc., and the determination results are accurate.

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Abstract

The invention discloses a method for determining the content of dimethyl sulfoxide in a sample in a purification process, belongs to the technical field of carbon fiber solvent recovery, and solves the technical problem of dimethyl sulfoxide content detection in a sample in a purification process. The method comprises the following steps: firstly, performing sampling and respectively titrating thecontent of dimethyl sulfoxide in a sample solution by adopting an iodometry to obtain a sample solution with known dimethyl sulfoxide content; secondly, preparing dimethyl sulfoxide solutions with different contents by adopting a sample solution with known dimethyl sulfoxide contents, measuring the refractive indexes of the prepared dimethyl sulfoxide solutions with different contents by utilizing a refractive index instrument, and drawing a curve corresponding to the refractive indexes and the dimethyl sulfoxide contents; thirdly, placing the to-be-detected sample on the refractive index instrument, and reading the refractive index of the to-be-detected sample; finally, enabling the read refractive index of the sample to be detected to correspond to the standard curve, and finding the dimethyl sulfoxide content of the sample to be detected. The detection time is shortened, production can be rapidly guided, and the detection cost is saved.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber solvent recovery, and in particular relates to a method for determining the content of dimethyl sulfoxide in a sample in a purification process. Background technique [0002] At present, the production of polyacrylonitrile-based carbon fiber accounts for more than 90% of the world's total carbon fiber production. Carbon fiber has high axial strength and modulus, no creep, good fatigue resistance, small thermal expansion coefficient and good corrosion resistance. Polyacrylonitrile-based carbon fibers are mainly composed of acrylonitrile and other small amounts of second and third monomers in solvents (dimethyl sulfoxide, sodium thiocyanate, etc.) And unreacted acrylonitrile monomer process, or solvent dissolving resin process to form a spinning solution with suitable viscosity, spin through wet and dry methods, and then make polyacrylonitrile fibers through washing and drawing processes. A l...

Claims

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Application Information

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IPC IPC(8): G01N1/38G01N21/41
CPCG01N1/38G01N21/4133
Inventor 雷爱民刘纳新段瑞云李旭东严华
Owner 山西钢科碳材料有限公司
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