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Preparation method and equipment for extracting waste dimethyl sulfoxide solvent

A technology of dimethyl sulfoxide and waste solvent, which is applied in the field of waste organic solvent recovery and purification, can solve the problems of high energy consumption, environmental pollution, difficult purification and the like, and achieves the advantages of reducing pollution degree, good recovery quality and simple production process. Effect

Inactive Publication Date: 2021-10-22
四川熔增环保科技有限公司
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Problems solved by technology

In the production of carbon fiber precursor acrylonitrile polymer, a large amount of dimethyl sulfoxide waste solvent containing impurities such as water, acrylonitrile monomer and acrylonitrile polymer is produced. Because it is not easy to purify, it is often discarded and no longer used, resulting in huge waste and emissions. It will also cause great pollution to the environment
The purpose of the present invention is to overcome the shortcomings of low purity of recovered products and huge energy consumption in the existing recovery technology, and to remove dimethyl methylene Water and other impurities in the sulfone solvent can improve the cycle performance characteristics of dimethyl sulfoxide and prolong the service life. In view of this, in-depth research on the above problems led to this case

Method used

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  • Preparation method and equipment for extracting waste dimethyl sulfoxide solvent
  • Preparation method and equipment for extracting waste dimethyl sulfoxide solvent
  • Preparation method and equipment for extracting waste dimethyl sulfoxide solvent

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preparation example Construction

[0030] A method for extracting and preparing waste dimethyl sulfoxide solvent, comprising the following steps: step S1, high boiling point removal of impurities; step S2, azeotropic separation; step S3, recovery of azeotropic agent;

[0031] The step S1: taking the waste solvent dimethyl sulfoxide and entering it into the rake dryer 2 to remove high-boiling impurities such as acrylonitrile polymers in the waste solvent;

[0032] The step S2: add the dimethyl sulfoxide obtained in the step S1 to the organic solvent that forms an azeotrope with water, drain the mixed solution into the pressure swing rectification tower 3, and the pressure swing rectification tower 3 top Remove low boilers and azeotropes with water, extract dimethyl sulfoxide from the 3 tanks of the pressure swing rectification tower, and obtain industrial grade dimethyl sulfoxide products with a purity of ≥99.9% (wt);

[0033] The step S3: the overhead azeotropic fraction obtained in step S2 is rectified, and th...

Embodiment 1

[0041] Embodiment 1: By draining the waste solvent in the waste solvent box 1 into the rake dryer 2, the ratio of the waste solvent of 60% dimethyl sulfoxide, 38% water and 2% other impurities is drained to the rake dryer In the device 2, set: the vacuum pressure is 40mmHg, the heating temperature is gradually raised to 102°C, most of the solvent is evaporated, and the high-boiling point polymer is discharged from the tailings, and the dimethylformamide obtained after the above-mentioned removal of acrylonitrile polymer is treated The base sulfoxide crude product is drained into the pressure swing rectification tower 3, and the liquid in the high-temperature box is pumped to a pair of high-temperature driven shunt pipes through the operation of a pair of high-temperature pumping pumps in the high-temperature component. The tube drains the high-temperature liquid into multiple high-temperature shunt tubes, and through the multiple high-temperature shunt tubes, drains some high-t...

Embodiment 2

[0042] Embodiment 2: Get the waste solvent containing 84% dimethyl sulfoxide, 11% acrylonitrile polymer, 5% water and other impurities, enter rake dryer 2, set: vacuum pressure 30mm, heating temperature rises gradually to At 95°C, most of the solvent was distilled off, and the high-boiling point polymer was discharged from the tailings. The crude dimethyl sulfoxide obtained after the above-mentioned removal of the acrylonitrile polymer was added to the crude dimethyl sulfoxide with 0.6 Double the volume of cyclohexane, carry out rectification at 100°C, the top water and cyclohexane form the lowest azeotrope and distill out together, then rectify under reduced pressure, extract dimethyl sulfoxide from the tower reactor, and extract After passing the liquid test, put it in a tank and store it with nitrogen gas to obtain industrial-grade dimethyl sulfoxide with a purity ≥ 99.9% (wt). After the cyclohexane obtained by the above-mentioned rectification is subjected to liquid separat...

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Abstract

The invention discloses a preparation method and equipment for extracting a waste dimethyl sulfoxide solvent. The preparation method and preparation equipment have the beneficial effects that a series of low-energy-consumption procedures for removing impurities in the waste dimethyl sulfoxide solvent through a rake dryer, an azeotropic separation dehydration method and a pressure-swing distillation purification method are adopted, the waste dimethyl sulfoxide solvent with a purity of only 25-92% (wt) is purified into industrial-grade dimethyl sulfoxide with a purity of larger than or equal to 99.9% (wt), recycling of the waste dimethyl sulfoxide solvent is achieved, the pollution degree of the waste dimethyl sulfoxide solvent to the environment is reduced, and production cost is saved. The purification method provided by the invention also has the advantages of high yield, low energy consumption, good recovery quality, recyclability, simple and convenient production process, stable operation, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to the technical field of recovery and purification of waste organic solvents, in particular to a preparation method and equipment for extraction and preparation of waste dimethyl sulfoxide solvents. Background technique [0002] With the wide application of high-tech fiber materials, the demand for carbon fiber in aerospace, engineering structure, mining, medical equipment and other industries is also increasing. In the production of carbon fiber precursor acrylonitrile polymer, a large amount of dimethyl sulfoxide waste solvent containing impurities such as water, acrylonitrile monomer and acrylonitrile polymer is produced. Because it is not easy to purify, it is often discarded and no longer used, resulting in huge waste and emissions. It will also cause great pollution to the environment. The purpose of the present invention is to overcome the shortcomings of low purity of recovered products and huge energy consumption in the...

Claims

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Application Information

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IPC IPC(8): C07C315/06C07C317/04B01D3/14B01D3/32B01D3/36B01D3/42
CPCC07C315/06B01D3/36B01D3/143B01D3/32B01D3/42C07C317/04Y02P70/10
Inventor 范文林纪王洋张怡黄啟虓
Owner 四川熔增环保科技有限公司
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