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Method for purifying dimethyl sulfoxide

A technology of dimethyl sulfoxide and purification method, which is applied in the field of purification of dimethyl sulfoxide, can solve the problems of high impurities in equipment requirements, reduce embedding, slow heating/cooling rate, and eliminate hidden dangers of decomposition and deterioration Effect

Active Publication Date: 2017-05-17
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the existing DMSO purification technology, which requires high equipment and easily introduces new impurities during the purification process, the present invention aims to provide a new purification method for dimethyl sulfoxide with good purification effect and high recovery rate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Purification of crude dimethyl sulfoxide.

[0031] Add 1 g of calcium oxide to 1000 g of crude dimethyl sulfoxide to be purified, then stir the above mixture at room temperature at 2000 rpm for 1 h by a mechanical stirring device, and filter out the solid matter after the stirring is completed to obtain deacidification and water removal. Dimethyl sulfoxide.

[0032] Put the above-mentioned dimethyl sulfoxide that has been deacidified and dewatered in a vacuum distillation device equipped with an oil pump, and carry out vacuum distillation under the condition of a pressure of 10mmHg, and collect fractions with a distillation range of 76-77°C to obtain Dimethyl sulfoxide that has been distilled under reduced pressure.

[0033] Using the above-mentioned dimethyl sulfoxide treated by vacuum distillation as the starting material, the starting material is placed in a melting crystallizer (cooled by ice-brine), and 18.5 ° C is used as the starting temperature of co...

Embodiment 2

[0035] Example 2: Purification of crude dimethyl sulfoxide.

[0036] Add 5 g of barium oxide to 1000 g of crude dimethyl sulfoxide to be purified, then stir the above mixture at room temperature at 1500 rpm for 0.5 h with a magnetic stirring device, filter out the solid matter after the stirring is completed, and obtain of dimethyl sulfoxide.

[0037]Place the above-mentioned dimethyl sulfoxide that has undergone deacidification and water removal treatment in a vacuum distillation device equipped with an oil pump, and carry out vacuum distillation under the condition of a pressure of 8mmHg, and collect fractions with a distillation range of 75-78°C to obtain Dimethyl sulfoxide that has been distilled under reduced pressure.

[0038] Using the above-mentioned dimethyl sulfoxide treated by vacuum distillation as the starting material, the starting material is placed in a melting crystallizer (cooled by ice-brine), and 18.5 ° C is used as the starting temperature of cooling crys...

Embodiment 3

[0040] Example 3: Purification of crude dimethyl sulfoxide.

[0041] Add 2 g of calcium oxide to 1000 g of crude dimethyl sulfoxide to be purified, then stir the above mixture at 2000 rpm for 1 h by means of a mechanical stirring device, and filter out the solid matter after the stirring is complete to obtain dimethyl sulfoxide treated with deacidification and water removal. base sulfoxide.

[0042] Put the above-mentioned dimethyl sulfoxide that has been deacidified and dewatered in a vacuum distillation device equipped with an oil pump, and carry out vacuum distillation under the condition of a pressure of 10mmHg, and collect fractions with a distillation range of 76-77°C to obtain Dimethyl sulfoxide that has been distilled under reduced pressure.

[0043] Using the above-mentioned dimethyl sulfoxide treated by vacuum distillation as the starting material, the starting material is placed in a melting crystallizer (cooled by ice-brine), and 18.5 ° C is used as the starting t...

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Abstract

The invention belongs to the technical field of chemical reagent purification, and relates to a method for purifying dimethyl sulfoxide. Specifically, the method comprises the following steps of: 1) performing deacidification and dehydration; 2) performing reduced pressure distillation; 3) performing primary melting crystallization; and 4) performing secondary melting crystallization. The method is low in requirement on production equipment and easy in industrialization; compared with a common method, the method provided by the invention is capable of preparing a purified dimethyl sulfoxide product with satisfactory purity (greater than or equal to 99.99%) and relatively high yield (about 85%).

Description

technical field [0001] The invention belongs to the technical field of chemical reagent purification, and relates to a method for purifying dimethyl sulfoxide. Background technique [0002] Dimethyl Sulfoxide (DMSO) is a sulfur compound with the molecular formula (CH 3 ) 2 SO, at room temperature, is a colorless, odorless transparent liquid with a melting point of 18.5°C and a boiling point of 189°C. It tastes slightly bitter, is easily soluble in water, alcohol, ether, and ester, and has strong hygroscopicity. It is stable below 140°C, and it will decompose a small amount of dimethyl sulfide (melting point is -138.5°C, boiling point is -24.9°C) and methyl mercaptan (melting point is -123.1°C, boiling point is 7.6°C) and dimethyl sulfone (melting point: 109°C, boiling point: 238°C) and other substances, the decomposition is accelerated under acidic conditions, and the decomposition can be inhibited under alkaline conditions. [0003] Dimethylsulfoxide (DMSO) is an aprotic...

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 郑琦顾金凤郭建国凌芳
Owner SINOPHARM CHEM REAGENT
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