CN1150164C - Process for preparing dimethyl sulfone - Google Patents
Process for preparing dimethyl sulfone Download PDFInfo
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- CN1150164C CN1150164C CNB011279354A CN01127935A CN1150164C CN 1150164 C CN1150164 C CN 1150164C CN B011279354 A CNB011279354 A CN B011279354A CN 01127935 A CN01127935 A CN 01127935A CN 1150164 C CN1150164 C CN 1150164C
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- dimethyl sulfoxide
- hydrogen peroxide
- reaction
- dimethyl
- dimethyl sulfone
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Abstract
The present invention discloses a process for preparing dimethyl sulfone, which relates to a preparation method of organic matters, particularly to a process for preparing dimethyl sulfone. The process solves the problems of complicated process of a nitric acid method, high cost and products with kakosmia. The dimethyl sulfone is prepared by oxidation reaction, cooling to separate, filtration, dehydration and drying. In the oxidation reaction, dimethyl sulfoxide reacts with hydrogen peroxide to generate the dimethyl sulfoxide. The weight ratio of the effective ingredients of the dimethyl sulfoxide and the hydrogen peroxide is from 1:0.44 to 0.65, the reaction temperature is from 80 to 150 DEG C and the reaction time is from 4 to 40 hours. Then, the dimethyl sulfoxide is cooled and crystals are separated out. A finished product is obtained by the filtration, the dehydration and the drying. The concentration of the dimethyl sulfoxide is from 10 to 100% and the concentration of the hydrogen peroxide is from 15 to 40%. Compared with the nitric acid method, the reaction temperature is moderate, harmful substances are not generated in the preparation process and side reaction products are not generated; the product does not need vacuum distillation without odor; the present invention has the advantages of easy operation, low cost, short periodicity and high efficiency; the yield of dimethyl sulfoxide produced by the method is from 65 to 94%.
Description
(1) technical field:
The present invention relates to organic preparation method, refer in particular to the preparation method of dimethyl sulfone.
(2) background technology:
At present, domesticly can get dimethyl sulfone with the nitric acid oxidation dimethyl sulfoxide (DMSO), have a lot of shortcomings with nitric acid oxidation: temperature of reaction is higher, and energy consumption is big, wastes energy; The side reaction product nitrogen oxide can't all absorb, contaminate environment; Need just can obtain finished product through underpressure distillation, complex process, product has cacosmia.
(3) summary of the invention:
It is complicated to the invention solves nitrate method technology, the cost height; Product has the problem of cacosmia.
Preparation method of the present invention is through oxidizing reaction, and cooling is separated out, and filters, dehydration, oven dry makes, and it is characterized in that: oxidizing reaction is that dimethyl sulfoxide (DMSO) and hydrogen peroxide reaction generate dimethyl sulfone, and the effective ingredient weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 1: 0.44～0.65, temperature of reaction is 80～150 ℃, in 4～40 hours reaction times, crystal is separated out in cooling then, filters, the dehydration, dry finished product.The concentration of dimethyl sulfoxide (DMSO): 10～100%, the concentration of hydrogen peroxide is 15～40%.
Reaction formula is:
The invention has the beneficial effects as follows: contrast nitrate method temperature of reaction is moderate, does not produce objectionable impurities in the preparation process, no side reaction product; Product does not need vacuum distilling, and does not have stink; Easy and simple to handle, cost is low, and is with short production cycle, the efficient height, and with the dimethyl sulfone that present method is produced, yield is 65～94%.
(4) embodiment:
Embodiment 1
The weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is: 1: 0.5, dimethyl sulfoxide (DMSO) 1150kg with 40% joins in 3 tons of reactors, the hydrogen peroxide 836kg of adding 27.5%, intensification makes it react 36 hours down at 90 ℃, lowers the temperature then and separates out crystal below 25 ℃, and common filter cloth filters, centrifuge dehydration, 40 ℃ of oven dry make moisture≤0.5% get finished product, and yield is 75%.
Embodiment 2
The weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is: 1: 0.6, dimethyl sulfoxide (DMSO) 260kg with 30% joins in 1 ton of reactor, the hydrogen peroxide 234kg of adding 20%, intensification makes it react 30 hours down at 90 ℃, lower the temperature then 20 ℃ and separate out crystal, filter centrifuge dehydration, 30 ℃ dry finished product, yield is 70.21%.
Embodiment 3
The weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is: 1: 0.44, dimethyl sulfoxide (DMSO) 1000kg with 40% joins in 3 tons of reactors, the hydrogen peroxide 586kg of adding 30%, intensification makes it react 35 hours down at 130 ℃, lower the temperature then and separate out crystal below 25 ℃, filtration, centrifuge dehydration, 35 ℃ dry finished product, yield is 69%.
Embodiment 4
The weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is: 1: 0.65, dimethyl sulfoxide (DMSO) 800kg with 40% joins in 3 tons of reactors, the hydrogen peroxide 693kg of adding 30%, intensification makes it react 36 hours down at 90 ℃, lower the temperature then and separate out crystal below 20 ℃, filter centrifuge dehydration, 35 ℃ dry finished product, yield is 66.06%.
Claims (4)
1, the preparation method of dimethyl sulfone, through oxidizing reaction, cooling is separated out, filter, dehydration, oven dry makes, it is characterized in that: oxidizing reaction is that dimethyl sulfoxide (DMSO) and hydrogen peroxide reaction generate dimethyl sulfone, the effective ingredient weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 1: 0.44～0.65, and temperature of reaction is 80～150 ℃, 4～40 hours reaction times.
2, the preparation method of dimethyl sulfone according to claim 1 is characterized in that: cool to below 25 ℃ and separate out crystal, filter cloth filters, centrifuge dehydration, 30～40 ℃ dry finished product.
3, the preparation method of dimethyl sulfone according to claim 1 is characterized in that: the concentration of dimethyl sulfoxide (DMSO) is 10～100%, and the concentration of hydrogen peroxide is 15～40%.
4, the preparation method of dimethyl sulfone according to claim 1 is characterized in that: the effective ingredient weight ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 1: 0.5～0.6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011279354A CN1150164C (en) | 2001-07-13 | 2001-07-13 | Process for preparing dimethyl sulfone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011279354A CN1150164C (en) | 2001-07-13 | 2001-07-13 | Process for preparing dimethyl sulfone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1397548A CN1397548A (en) | 2003-02-19 |
| CN1150164C true CN1150164C (en) | 2004-05-19 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011279354A Expired - Fee Related CN1150164C (en) | 2001-07-13 | 2001-07-13 | Process for preparing dimethyl sulfone |
Country Status (1)
| Country | Link |
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| CN (1) | CN1150164C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195595B (en) * | 2007-12-12 | 2012-02-01 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfone and sodium nitrate from dimethyl sulfoxide waste slag |
| CN102010354A (en) * | 2010-11-30 | 2011-04-13 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfoxide waste residue |
| CN104311460B (en) * | 2014-09-15 | 2016-06-15 | 夏瑜 | A kind of recovery and treatment method of dimethyl sulfoxide abraum salt |
| CN104592067B (en) * | 2015-01-30 | 2016-08-24 | 湖北大学 | A kind of method that multitple extraction dimethyl sulfoxide waste residue recycles |
| CN106083666B (en) * | 2016-06-14 | 2017-11-07 | 岳阳蓬诚科技发展有限公司 | A kind of production technology of dimethyl sulfone |
| CN105884662B (en) * | 2016-06-14 | 2017-07-21 | 岳阳蓬诚科技发展有限公司 | A kind of production technology of dimethyl sulfone |
| CN105837477B (en) * | 2016-06-14 | 2017-07-21 | 岳阳蓬诚科技发展有限公司 | A kind of preparation method of dimethyl sulfone |
| CN105859595B (en) * | 2016-06-14 | 2018-03-09 | 岳阳蓬诚科技发展有限公司 | A kind of production technology of dimethyl sulfone |
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2001
- 2001-07-13 CN CNB011279354A patent/CN1150164C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1397548A (en) | 2003-02-19 |
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Granted publication date: 20040519 Termination date: 20100713 |