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Refining method for dimethyl sulfoxide solvent in carbon fiber precursor production process

A technology of carbon fiber precursors and dimethyl sulfoxide, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as not considering the influence of acrylonitrile polymers, and achieve the effect of improving the recovery rate

Active Publication Date: 2017-12-12
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can remove metal ions in dimethyl sulfoxide, it does not consider the influence of acrylonitrile polymer on the adsorption process

Method used

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  • Refining method for dimethyl sulfoxide solvent in carbon fiber precursor production process
  • Refining method for dimethyl sulfoxide solvent in carbon fiber precursor production process
  • Refining method for dimethyl sulfoxide solvent in carbon fiber precursor production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] according to figure 1 The specific operating parameters are: the evaporator 1 evaporates 1 / 3 of the material, the operating temperature of the evaporator 1 is 130°C, and the operating pressure is 0.015MPa; the operating temperature of the filter 2 is 70°C, and the operating pressure is normal The temperature at the top of the dehydration tower 3 is 31.9°C, the temperature of the bottom of the dehydration tower 3 is 107°C, and the pressure at the top of the dehydration tower 3 is 0.005MPa; the temperature at the top of the dehydration tower 4 is 86.5°C, The temperature of the bottom of the column 4 is 91.1° C., and the pressure at the top of the heavy removal column 4 is 0.001 MPa. See Table 1 for the raw materials used in this example and the weight percentage composition of each unit component, process parameters and dimethyl sulfoxide yield.

[0035] Table 1

[0036]

Embodiment 2

[0038] according to figure 1The specific operating parameters are: the evaporator 1 evaporates 1 / 2 of the material in it, the operating temperature of the evaporator 1 is 120°C, and the operating pressure is 0.010MPa; the operating temperature of the filter 2 is 70°C, and the operating pressure is normal The temperature at the top of the dehydration tower 3 is 45.5°C, the temperature of the bottom of the dehydration tower 3 is 123°C, and the pressure at the top of the dehydration tower 3 is 0.010MPa; the temperature at the top of the dehydration tower 4 is 100.2°C, The temperature of the bottom of the column 4 is 112.5° C., and the pressure at the top of the weight removal column 4 is 0.005 MPa. See Table 2 for the raw materials used in this example and the weight percent composition, process parameters and dimethyl sulfoxide yield of each unit component.

[0039] Table 2

[0040]

Embodiment 3

[0042] according to figure 2 The specific operating parameters are: the evaporator 1 is heated for 10 hours (only heating, no evaporation), the operating temperature of the evaporator 1 is 110°C, and the operating pressure is 0.10MPa; the operating temperature of the filter 2 is 70°C, and the operating pressure It is normal pressure; the tower top temperature of dehydration tower 3 is 59.9 ℃, and the tower still temperature of dehydration tower 3 is 141 ℃, and the tower top pressure of dehydration tower 3 is 0.020MPa; The temperature of the bottom of the heavy column 4 is 124.9° C., and the pressure at the top of the heavy column 4 is 0.010 MPa. See Table 3 for the raw materials used in this example and the weight percentage composition, process parameters and dimethyl sulfoxide yield of each unit component.

[0043] table 3

[0044]

[0045] The unanalyzed parameters in Tables 1-3 are because this parameter is not a control index.

[0046] The comparison between the an...

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Abstract

The invention relates to a refining method for a dimethyl sulfoxide solvent in a carbon fiber precursor production process. The refining method comprises the following steps: removing a polymer in a polymerization kettle cleaning solution produced in a carbon fiber precursor production process, then, mixing the polymerization kettle cleaning solution with crude dimethyl sulfoxide produced in the carbon fiber precursor production process, and then, dehydrating the mixture in a dehydrating tower to obtain a dehydrated product at the bottom of the tower; enabling the dehydrated product to enter a de-heavy tower to carry out de-heavy operation to obtain a refined product of dimethyl sulfoxide at the top of the tower and a liquid-phase material 2 at the bottom of the tower; and after circulating the obtained liquid-phase material and mixing the liquid-phase material with the polymerization kettle cleaning solution, removing the polymer. By using the method, the phenomenon that a polymer impurity enters a rectifying tower to block equipment can be effectively avoided, and a device can stably operate for a long period; and meanwhile, a bottom liquid of the de-heavy tower returns to an inlet of an evaporator, so that dimethyl sulfoxide in the bottom liquid is further recycled, and furthermore, the recovery rate of dimethyl sulfoxide is effectively increased.

Description

technical field [0001] The invention relates to a method for refining dimethyl sulfoxide (DMSO) solvent. Background technique [0002] The separation and refining process in the production process of dimethyl sulfoxide is: firstly conduct evaporation and desalination, and then obtain dimethyl sulfoxide product through the process of dehydration and refining in the rectification tower. [0003] In the production process of carbon fiber precursors, acrylonitrile monomers are polymerized with dimethyl sulfoxide as a solvent, and the obtained polymers are used to produce carbon fiber precursors after separation. The dimethyl sulfoxide solvent introduces impurities such as metal ions, acrylonitrile polymers, acrylonitrile monomers, and water during the polymerization process, which cannot be directly recycled. In order to reduce the production cost and enable the dimethyl sulfoxide solvent to be recycled, it must be refined to remove impurities. [0004] "Contemporary Chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/06C07C317/04
CPCC07C315/06C07C317/04
Inventor 程延华武冬冬王旭孟繁辉徐金峰韩小平姜晓东彭建林姚玉媛
Owner PETROCHINA CO LTD
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