CN1130339C - Process for preparing dimethylsulfone - Google Patents
Process for preparing dimethylsulfone Download PDFInfo
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- CN1130339C CN1130339C CN 01144216 CN01144216A CN1130339C CN 1130339 C CN1130339 C CN 1130339C CN 01144216 CN01144216 CN 01144216 CN 01144216 A CN01144216 A CN 01144216A CN 1130339 C CN1130339 C CN 1130339C
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Abstract
The present invention relates to a method for producing dimethyl sulfone, which belongs to the technical field of the preparation process of chemical substances. Dimethyl sulfoxide with purity larger than or equal to 99.8% and a solidifying point at 17.8DEG, and hydrogen peroxide with weight being 1.566 to 1.567 times of the weight of the dimethyl sulfoxide, concentration being 27.5% and acidity being at most 0.01% are conducted with oxidation reaction for 60 minutes at the temperature of 22(+/-)2DEG C in neutral water serving as a reaction medium of which the amount is equivalent to 1.266 to 1.267 times of the feed amount of dimethyl sulfoxide; white crystals of high quality dimethyl sulfone with purity larger than or equal to 99.9% are finally produced through the processing steps of dewatering, purifying, drying, sieving, etc. dimethyl sulfone crystal mixed liquid produced by the oxidation reaction. The total yield of the dimethyl sulfone reaches 85%.
Description
Technical Field
The invention relates to a method for producing dimethyl sulfone, belonging to a process for preparing chemical substances
The technical field is as follows.
Background
Dimethyl sulfone (Methyl sulfonyl methane) is used as a base material of beauty and health care medicines for promoting wound healing and repairing scars, enabling human skin to have luster and elasticity and treating arthritis diseases, and is widely applied to the fields of medicine health care, beauty treatment and the like. Although it has been produced abroad, it has not been possible to obtain high-purity dimethyl sulfone so far because of the limitations of production process means and levels, and it is known from the publicly known literature that only the purity index is set to 99.5% standard for a representative U.S.A.
Disclosure of Invention
Aiming at the defects of the prior production process technology which is difficult to prepare high-purity dimethyl sulfone, the invention innovatively designs a method for producing dimethyl sulfone, so that the purity of the product reaches more than or equal to 99.8 percent.
The invention is realized by adopting the following technical scheme.
The production process steps are carried out according to the following sequence:
selecting and matching materials
Firstly, dimethyl sulfoxide with purity more than or equal to 98.8 percent and freezing point of 17.8 ℃ is input into a reaction tank, then normal-temperature neutral purified tap water with weight 1.266-1.267 times of the dimethyl sulfoxide is injected for uniform dilution, and the PH value is adjusted within the range of 5-6; under the condition that the temperature in the tank is lower than 20 ℃, hydrogen peroxide with the concentration of 27.5 percent and the acidity of less than or equal to 0.01 percent which are 1.566-1.567 times of the weight of dimethyl sulfoxide is slowly injected at the flow rate of 2.8-3.0 liters/min, and the temperature in the tank is controlled at 15-20 ℃;
oxidation reaction
Under the conditions of normal pressure, sealing, keeping the temperature in the tank at 20 +/-2 ℃ and stirring, carrying out oxidation reaction on the mixed material liquid for 60 minutes;
concentrating
The material liquid generated by the reaction is moved to a concentration tank, stirred and heated to 60 ℃, and exhausted, and after three gradual heating stages of 60-70 ℃ in the first hour, 70-90 ℃ in the second hour and 90-103 ℃ in the third hour, a large amount of water after the reaction is evaporated;
spin-drying
Cooling the concentrated and crystallized mixed solution to 22 +/-2 ℃, performing centrifugal drying separation treatment, recovering the mother solution into a concentration tank, and transferring the dimethyl sulfone crystallized wet product to a refining tank;
refining
Fully dissolving the dimethyl sulfone wet product in the refining tank with distilled water which is 1.2 times of the weight of the dimethyl sulfone wet product at the temperature of 82 +/-2 ℃, filtering to remove impurities, stirring, cooling to separate out crystals, centrifugally drying at the temperature of 15-20 ℃, recovering the separated mother liquor, and sending the filtered refined dimethyl sulfone wet product to a drying box;
drying
Drying the refined dimethyl sulfone crystal wet product in a drying oven at a constant temperature of 81 +/-1 ℃ to prepare white crystals with the moisture content of less than or equal to 0.2%;
screen pack
Sieving to obtain dimethyl sulfone with fineness of 20-100 meshes, and quantitatively packaging.
The reagent used to adjust the pH of the aqueous dimethyl sulfoxide dilution solution in the selected batch was a 65% strength chemically pure nitric acid.
The invention has the advantages that:
the process flow is simple, the process parameters can be stably controlled, the total yield of the dimethyl sulfone product reaches 85 percent, and the purity of the dimethyl sulfone product is as high as 99.9 percent, so that the production cost is reduced while the product quality is improved, and the cosmetic and health care medicine prepared by using the dimethyl sulfone product as a base material through a known technology has remarkable application and commercial effects.
The specific implementation mode is as follows:
the process for producing dimethyl sulfone of the present invention will be described in detail by way of exemplary embodiments:
example 1
Firstly, 236.8kg of dimethyl sulfone with the purity of more than or equal to 99.8 percent and the freezing point of 17.8 ℃ is input into a reaction tank provided with a stirrer and a jacket from a high-level tank, then, the normal-temperature neutral purified tap water with the weight of 1.266 times that of the dimethyl sulfone, namely 299.4kg of the dimethyl sulfone is injected into the tank and stirred for uniform dilution, cooling water is introduced into the jacket of the reaction tank to ensure that the temperature in the tank is lower than 20 ℃, meanwhile, the pH value of the diluent is measured, and when the concentration exceeds 6.0, 65 percent of reagent pure-grade nitric acid is dripped to ensure that the pH value of the dimethyl sulfone aqueous solution is within the range of 5-6. Under the condition, hydrogen peroxide which is about 370.8kg and has the concentration of 27.5 percent and the acidity of less than or equal to 0.01 percent and is about 1.566 times of the weight of the dimethyl sulfoxide is slowly injected from the storage tank at the flow rate of 2.8-3.0 liters/minute for about 10 minutes, and the temperature in the storage tank is kept at 15-17 ℃.
After the dosing is finished, the oxidation reaction is carried out.
The reaction was carried out under normal pressure, sealed, with stirring and with the temperature in the tank kept at 18-20 ℃ for 60 minutes.
Transferring the material liquid generated by the reaction into a concentration tank with a jacket filled with steam, heating to 60 ℃ with stirring and exhausting, and gradually heating for three stages of 60-65 ℃ in the first hour, 65-85 ℃ in the second hour and 85-100 ℃ in the third hour to evaporate a large amount of water after the reaction.
Cooling the concentrated crystallization mixed liquor to 20 ℃, transferring the cooled crystallization mixed liquor into a centrifugal machine for spin-drying, recovering the mother liquor into a concentration tank, and conveying the dimethyl sulfone crystallization wet product to a refining tank.
Distilled water which is 1.2 times of the weight of a dimethyl sulfone crystal wet product is injected into a refining tank which is provided with astirrer, a jacket and a filtering device, the temperature is raised to 80-81 ℃ by stirring for fully dissolving, then mechanical impurities are filtered, and cooling water is stopped to be introduced into jacket steam. Cooling while stirring to separate out crystal, centrifugal drying at 15-18 deg.c, recovering separated mother liquid, and filtering to obtain wet product of dimethyl sulfone crystal.
Drying at constant temperature of 80 ℃ in a drying oven to obtain the dimethyl sulfone crystal.
After the whole production and preparation process is finished through screening and packaging, the product achieves the following quality indexes:
appearance: white crystal, good fluidity
Purity: not less than 99.9 percent
Melting point: 108 temperature 109 deg.C
Boiling point: 238 deg.C
Heavy metals: less than or equal to 10PPM
Moisture content: less than or equal to 0.5 percent
Fineness: 20-100 mesh
Example 2
Firstly, 236.8kg of dimethyl sulfone with the purity of more than or equal to 99.8 percent and the freezing point of 17.8 ℃ is input into a reaction tank provided with a stirrer and a jacket from a high-level tank, then normal-temperature neutral purified tap water which is equal to 1.266 times of the weight of the dimethyl sulfone, namely 300kg of the dimethyl sulfone is injected into the tank and is stirred with the tank to be uniformly diluted, cooling water is introduced into the jacket of the reaction tank to ensure that the temperature in the tank is lower than 20 ℃, the pH value of a diluent is measured, and when the concentration of the pure-grade nitric acid is higher than 6.0, 65 percent of reagent pure-gradenitric acid is dripped to ensure that the pH value of a dimethyl sulfone aqueous solution is within. Under the condition, about 371.1kg of hydrogen peroxide with the weight 1.567 times that of dimethyl sulfoxide, the concentration of 27.5 percent and the acidity of less than or equal to 0.01 percent is injected slowly from the storage tank at the flow rate of 2.8-3.0 liters/minute for about 10 minutes, and the temperature in the storage tank is kept at 16-17 ℃.
After the dosing is finished, the oxidation reaction is carried out.
The reaction is carried out under the conditions of normal pressure, sealing, stirring and temperature in the tank kept at 19-20 ℃, and takes 60 minutes.
Transferring the material liquid generated by the reaction into a concentration tank with a jacket filled with steam, heating to 60 ℃ with stirring and exhausting, and gradually heating for three stages of 65-70 ℃ for the first hour, 70-90 ℃ for the second hour and 90-103 ℃ for the third hour to evaporate a large amount of water after the reaction.
Cooling the concentrated crystallization mixed liquor to 22 ℃, transferring the concentrated crystallization mixed liquor into a centrifugal machine for spin-drying, recovering the mother liquor into a concentration tank, and conveying the dimethyl sulfone crystallization wet product to a refining tank.
Distilled water which is 1.2 times of the weight of a dimethyl sulfone crystal wet product is injected into a refining tank which is provided with a stirrer, a jacket and a filtering device, the temperature is raised to 81-82 ℃ for full dissolution by stirring, then mechanical impurities are filtered, and the jacket steam stops introducing cooling water. Cooling while stirring to separate out crystal, centrifugal drying at 17-20 deg.c, recovering separated mother liquid, and filtering to obtain wet product of dimethyl sulfone crystal.
The crystals were dried in a drying oven at a constant temperature of 82 ℃ to obtain the dimethylsulfone crystals having the same quality index as in example 1.
Claims (2)
1. A method for producing dimethyl sulfoxide comprises the following process steps in the following sequence:
(A) selecting and matching materials
Firstly, dimethyl sulfoxide with purity more than or equal to 98.8 percent and freezing point of 17.8 ℃ is input into a reaction tank, then normal-temperature neutral purified tap water with weight 1.266-1.267 times of the dimethyl sulfoxide is injected for uniform dilution, and the PH value is adjusted within the range of 5-6; under the condition that the temperature in the tank is lower than 20 ℃, hydrogen peroxide with the concentration of 27.5 percent and the acidity of less than or equal to 0.01 percent which are 1.566-1.567 times of the weight of dimethyl sulfoxide is slowly injected at the flow rate of 2.8-3.0 liters/min, and the temperature in the tank is controlled at 15-20 ℃;
(B) oxidation reaction
Under the conditions of normal pressure, sealing, keeping the temperature in the tank at 20 +/-2 ℃ and stirring, carrying out oxidation reaction on the mixed material liquid for 60 minutes;
(C) concentrating
The material liquid generated by the reaction is moved to a concentration tank, stirred and heated to 60 ℃, and exhausted, and after three gradual heating stages of 60-70 ℃ in the first hour, 70-90 ℃ in the second hour and 90-103 ℃ in the third hour, a large amount of water after the reaction is evaporated;
(D) spin-drying
Cooling the concentrated and crystallized mixed solution to 22 +/-2 ℃, performing centrifugal drying separation treatment, recovering the mother solution into a concentration tank, and transferring the dimethyl sulfone crystallized wet product to a refining tank;
(E) refining
Fully dissolving the dimethyl sulfone wet product in the refining tank with distilled water which is 1.2 times of the weight of the dimethyl sulfone wet product at the temperature of 82 +/-2 ℃, filtering to remove impurities, stirring, cooling to separate out crystals, centrifugally drying at the temperature of 15-20 ℃, recovering the separated mother liquor, and sending the filtered refined dimethyl sulfone wet product to a drying box;
(F) drying
Drying the refined dimethyl sulfone crystal wet product in a drying oven at a constant temperature of 81 +/-1 ℃ to prepare white crystals with the moisture content of less than or equal to 0.2%;
(G) screen pack
Sieving to obtain dimethyl sulfone with fineness of 20-100 meshes, and quantitatively packaging.
2. The process for the production of dimethyl sulfone as set forth in claim 1, characterized in that: the reagent for adjusting the pH value of the dimethyl sulfoxide diluted aqueous solution in the material selecting and preparing process is pure-grade nitric acid with the concentration of 65 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01144216 CN1130339C (en) | 2001-12-13 | 2001-12-13 | Process for preparing dimethylsulfone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01144216 CN1130339C (en) | 2001-12-13 | 2001-12-13 | Process for preparing dimethylsulfone |
Publications (2)
| Publication Number | Publication Date |
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| CN1356315A CN1356315A (en) | 2002-07-03 |
| CN1130339C true CN1130339C (en) | 2003-12-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 01144216 Expired - Fee Related CN1130339C (en) | 2001-12-13 | 2001-12-13 | Process for preparing dimethylsulfone |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| RU2490254C1 (en) * | 2012-06-18 | 2013-08-20 | Федеральное Государственное Бюджетное Учреждение Науки Институт Химии Коми Научного Центра Уральского Отделения Российской Академии Наук | Method of obtaining dimethyl sulphone |
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