CN114805145A - Device and method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide - Google Patents
Device and method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide Download PDFInfo
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- CN114805145A CN114805145A CN202210425397.3A CN202210425397A CN114805145A CN 114805145 A CN114805145 A CN 114805145A CN 202210425397 A CN202210425397 A CN 202210425397A CN 114805145 A CN114805145 A CN 114805145A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/02—Preparation of sulfones; Preparation of sulfoxides by formation of sulfone or sulfoxide groups by oxidation of sulfides, or by formation of sulfone groups by oxidation of sulfoxides
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Abstract
The invention relates to a device and a method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide. The method has the advantages of short production flow, few byproducts, easy product purification, convenient operation, mild conditions, no hazardous waste and high environmental friendliness.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a device and a method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide.
Background
Dimethyl sulfoxide (DMSO) is an aprotic polar solvent, and is called a "universal solvent" because it has a special solvent effect on chemical reactions and solubility characteristics for many substances. In addition, it has the curative effects of diminishing inflammation, relieving pain, promoting urination, tranquilizing and promoting wound healing, and has strong penetrating capacity to body and the carrying and synergistic effect to other medicine. Therefore, DMSO is widely applied in the industries of petroleum, chemical industry, medicine, electronics, synthetic fiber, plastics, printing and dyeing and the like.
The production process of the dimethyl sulfoxide product is mature, and the nitrogen dioxide method production process is generally adopted at home and abroad at present, namely, the dimethyl sulfide is dissolved in the dimethyl sulfoxide, and N0 is introduced 2 And 0 2 The emulsion oxidation reaction is carried out, but the safety of the process operation control of the method is relatively low, and meanwhile, the oxidation process can generate nitrogen oxide tail gas and solid waste nitrate, which can cause pollution to the environment.
Disclosure of Invention
The invention provides a device and a method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, which are convenient to operate, do not generate hazardous waste and are safer and more environment-friendly.
The technical scheme adopted by the invention is as follows: the utility model provides an adopt hydrogen peroxide solution oxidation dimethyl sulfide to prepare device of dimethyl sulfoxide, including the dimethyl sulfide storage tank, the hydrogen peroxide solution storage tank, tubular reactor group, the crude product jar, the dimethyl sulfide measuring pump, the hydrogen peroxide solution measuring pump, the crude product discharge pump, the blender, above equipment all is provided with exit, dimethyl sulfide storage tank export and dimethyl sulfide measuring pump access connection, hydrogen peroxide solution storage tank export and hydrogen peroxide solution measuring pump access connection, the export of dimethyl sulfide measuring pump and hydrogen peroxide solution measuring pump and blender access connection, the blender, tubular reactor group, crude product jar and crude product discharge pump connect gradually.
Preferably, the device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide comprises a tubular reactor group which comprises a first-stage tubular reactor, a second-stage tubular reactor, a third-stage tubular reactor, a fourth-stage tubular reactor, a fifth-stage tubular reactor and a sixth-stage tubular reactor which are connected in series.
Preferably, the device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide is provided with thermometers at the outlets of the first-stage to sixth-stage tubular reactors.
Preferably, in the device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, a dimethyl sulfide filter is arranged at an outlet of a dimethyl sulfide storage tank, and a hydrogen peroxide filter is arranged at an outlet of the hydrogen peroxide storage tank.
Preferably, in the device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, a dimethyl sulfide three-way valve is arranged between a dimethyl sulfide metering pump and a mixer, and a hydrogen peroxide three-way valve is arranged between the hydrogen peroxide metering pump and the mixer.
Preferably, in the device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, the jacket is arranged outside the first-stage to sixth-stage tubular reactors, and the jacket of the first-stage tubular reactor is provided with a hot water pipeline and a low-temperature water pipeline; the jackets of the second-level to sixth-level tubular reactors are all provided with low-temperature water pipelines.
The invention also provides a method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, which comprises the following steps:
step 1: after being filtered by a dimethyl sulfide filter, the dimethyl sulfide in the dimethyl sulfide storage tank is conveyed into a mixer by a dimethyl sulfide metering pump;
step 2: hydrogen peroxide in the hydrogen peroxide storage tank is filtered by a hydrogen peroxide filter, and then is conveyed by a hydrogen peroxide metering pump to enter a mixer;
and step 3: the dimethyl sulfide and hydrogen peroxide are mixed in a mixer and then sequentially enter a first-stage to sixth-stage tubular reactor for reaction, the first-stage tubular reactor is preheated by hot water in the initial stage of the reaction, the temperature is reduced by low-temperature water after the heat release is large, and the second-stage to sixth-stage tubular reactor is cooled by low-temperature water;
and 4, step 4: dimethyl sulfoxide generated by the reaction enters a crude product tank, and is discharged out of the crude product tank through a crude product discharge pump for storage.
Preferably, in the method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, the concentration of hydrogen peroxide is 24-28%, and the feed mass ratio of dimethyl sulfide to hydrogen peroxide is 1: 2.0-1: 2.2.
Preferably, in the method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, the outlet temperature of the first-stage tubular reactor is controlled to be 30-35 ℃, the outlet temperature of the second-stage tubular reactor is controlled to be 40-50 ℃, the outlet temperature of the third-stage tubular reactor is controlled to be 50-70 ℃, the outlet temperatures of the fourth-stage tubular reactor and the fifth-stage tubular reactor are controlled to be less than 70 ℃, and the outlet temperature of the sixth-stage tubular reactor is controlled to be less than 20 ℃.
Compared with the prior art, the invention has the beneficial effects that: dimethyl sulfide and hydrogen peroxide are conveyed into a mixer through a metering pump, the two materials are uniformly mixed and then sequentially enter a first-stage tubular reactor, a second-stage tubular reactor, a third-stage tubular reactor, a fourth-stage tubular reactor, a fifth-stage tubular reactor and a sixth-stage tubular reactor, a hot water pipeline is arranged in a jacket of the first-stage tubular reactor, pre-reaction is carried out by controlling the temperature, the unreacted dimethyl sulfide and the hydrogen peroxide are sequentially and completely reacted in the second-stage tubular reactor, the third-stage tubular reactor, the fourth-stage tubular reactor, the fifth-stage tubular reactor and the sixth-stage tubular reactor, reaction products mainly comprise dimethyl sulfoxide and water and are stored in a crude product tank, and the crude product tank is discharged and stored after reaching a certain liquid level. The method has the advantages that the required oxidant is hydrogen peroxide, the method is high in environmental friendliness, few in product purification procedures and convenient to operate, the hydrogen peroxide is convenient to transport, the byproduct is only water, the water can be removed by adopting a rectification mode, no other waste residues and waste gases are generated, and the production is safer and more environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
In the figure: 1. a dimethyl sulfide storage tank; 2. a hydrogen peroxide storage tank; 3. a first-stage tubular reactor; 4. a two-stage tubular reactor; 5. a three-stage tubular reactor; 6. a four-stage tubular reactor; 7. a five-stage tubular reactor; 8. a six-stage tubular reactor; 9. a coarse product tank; 10. a dimethyl sulfide metering pump; 11. a hydrogen peroxide metering pump; 12. a crude product discharge pump; 13. a mixer; 14. a dimethyl sulfide filter; 15. a hydrogen peroxide filter; 16. dimethyl sulfide three-way valves; 17. a hydrogen peroxide three-way valve.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1:
this embodiment provides an adopt hydrogen peroxide solution oxidation dimethyl sulfide to prepare device of dimethyl sulfoxide, as shown in fig. 1, including dimethyl sulfide storage tank 1, hydrogen peroxide solution storage tank 2, tubular reactor group, coarse product jar 9, dimethyl sulfide measuring pump 10, hydrogen peroxide solution measuring pump 11, coarse product ejection of compact pump 12, blender 13, above equipment all is provided with the exit, 1 export of dimethyl sulfide storage tank and 10 access connection of dimethyl sulfide measuring pump, 2 exports of hydrogen peroxide solution storage tank and 11 access connection of hydrogen peroxide solution measuring pump, 10 exports of dimethyl sulfide measuring pump and 11 exports of hydrogen peroxide solution measuring pump and 13 access connection of blender, blender 13, tubular reactor group, coarse product jar 9 and coarse product ejection of compact pump 12 connect gradually. The tubular reactor group comprises a first-stage tubular reactor 3, a second-stage tubular reactor 4, a third-stage tubular reactor 5, a fourth-stage tubular reactor 6, a fifth-stage tubular reactor 7 and a sixth-stage tubular reactor 8 which are connected in series, the tubular reactor group is formed by connecting the first-stage tubular reactors 3-8 to the sixth-stage tubular reactors in series, the reaction conversion rate is high, and the equipment investment is small. The outlet of the first-stage to sixth-stage tubular reactors 3-8 is provided with a thermometer, so that the reaction condition can be monitored at any time. The outlet of the dimethyl sulfide storage tank 1 is provided with a dimethyl sulfide filter 14 which can filter impurities in the dimethyl sulfide, and the outlet of the hydrogen peroxide storage tank 2 is provided with a hydrogen peroxide filter 15 which can filter impurities in the hydrogen peroxide. A dimethyl sulfide three-way valve 16 is arranged between the dimethyl sulfide metering pump 10 and the mixer 13 to control the feeding or the backflow of the dimethyl sulfide, and a hydrogen peroxide three-way valve 17 is arranged between the hydrogen peroxide metering pump 11 and the mixer 13 to control the feeding or the backflow of the hydrogen peroxide. A jacket is arranged outside the first-stage to sixth-stage tubular reactors 3-8, wherein the jacket of the first-stage tubular reactor 3 is provided with a hot water pipeline and a low-temperature water pipeline, so that the pre-reaction temperature can be controlled conveniently; the jackets of the second-level to sixth-level tubular reactors 4-8 are all provided with low-temperature water pipelines, so that the reaction heat can be removed in time, and the risk of the reaction process is controllable.
Example 2:
the embodiment provides a method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide, which comprises the following steps:
step 1: after being filtered by a dimethyl sulfide filter 14, dimethyl sulfide in a dimethyl sulfide storage tank 1 is conveyed into a mixer 13 by a dimethyl sulfide metering pump 11;
step 2: the hydrogen peroxide in the hydrogen peroxide storage tank 2 is filtered by a hydrogen peroxide filter 15, and then is conveyed by a hydrogen peroxide metering pump 10 and enters a mixer 13;
and step 3: the concentration of hydrogen peroxide is 24-28%, and the mass ratio of dimethyl sulfide to hydrogen peroxide is 1: 2.0-1: 2.2, mixing dimethyl sulfide and hydrogen peroxide in a mixer 13, and then sequentially entering a first-stage to sixth-stage tubular reactor 3-8 for reaction, preheating the first-stage tubular reactor 3 by hot water in the initial stage of reaction, cooling by low-temperature water after the heat release is large, cooling by low-temperature water in a second-stage to sixth-stage tubular reactor 4-8, controlling the outlet temperature of the first-stage tubular reactor 3 at 30-35 ℃, controlling the outlet temperature of the second-stage tubular reactor 4 at 40-50 ℃, controlling the outlet temperature of the third-stage tubular reactor 5 at 50-70 ℃, controlling the outlet temperatures of a fourth-stage tubular reactor 6 and a fifth-stage tubular reactor 7 at less than 70 ℃ and controlling the outlet temperature of the sixth-stage tubular reactor 8 at less than 20 ℃;
and 4, step 4: dimethyl sulfoxide generated by the reaction enters a crude product tank 9, and is discharged and stored through a crude product discharge pump 12.
It is to be understood that the above-described embodiments are only a few, and not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. A device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide is characterized in that
Including dimethyl sulfide storage tank (1), hydrogen peroxide solution storage tank (2), tubular reactor group, coarse product jar (9), dimethyl sulfide measuring pump (10), hydrogen peroxide solution measuring pump (11), coarse product ejection of compact pump (12), blender (13), above equipment all is provided with imports and exports, dimethyl sulfide storage tank (1) export and dimethyl sulfide measuring pump (10) access connection, hydrogen peroxide solution storage tank (2) export and hydrogen peroxide solution measuring pump (11) access connection, dimethyl sulfide measuring pump (10) export and hydrogen peroxide solution measuring pump (11) export and blender (13) access connection, blender (13), tubular reactor group, coarse product jar (9) and coarse product ejection of compact pump (12) connect gradually.
2. The device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 1, wherein the tubular reactor group comprises a first-stage tubular reactor (3), a second-stage tubular reactor (4), a third-stage tubular reactor (5), a fourth-stage tubular reactor (6), a fifth-stage tubular reactor (7) and a sixth-stage tubular reactor (8) which are connected in series.
3. The device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 2, wherein thermometers are arranged at outlets of the first-stage to sixth-stage tubular reactors (3-8).
4. The device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 3, wherein a dimethyl sulfide filter (14) is arranged at an outlet of the dimethyl sulfide storage tank (1), and a hydrogen peroxide filter (15) is arranged at an outlet of the hydrogen peroxide storage tank (2).
5. The device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 1, wherein a dimethyl sulfide three-way valve (16) is arranged between the dimethyl sulfide metering pump (10) and the mixer (13), and a hydrogen peroxide three-way valve (17) is arranged between the hydrogen peroxide metering pump (11) and the mixer (13).
6. The device for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 2, wherein a jacket is arranged outside the first-stage to sixth-stage tubular reactors (3-8), wherein the jacket of the first-stage tubular reactor (3) is provided with a hot water pipeline and a low-temperature water pipeline; the jackets of the second-level to sixth-level tubular reactors (4-8) are all provided with low-temperature water pipelines.
7. A method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide is characterized by comprising the following steps:
step 1: dimethyl sulfide in the dimethyl sulfide storage tank (1) passes through a dimethyl sulfide filter (14)
After filtration, the mixture is conveyed into a mixer (13) by a dimethyl sulfide metering pump (11);
step 2: after the hydrogen peroxide in the hydrogen peroxide storage tank (2) is filtered by the hydrogen peroxide filter (15),
the hydrogen peroxide is conveyed by a hydrogen peroxide metering pump (10) and then enters a mixer (13);
and step 3: the dimethyl sulfide and hydrogen peroxide are mixed in a mixer (13) and then enter a first-stage to sixth-stage tubular reactors (3-8) in sequence for reaction, the first-stage tubular reactor (3) is preheated by hot water at the initial stage of the reaction, low-temperature water is used for cooling after the heat release is large, and the second-stage to sixth-stage tubular reactors (4-8) are cooled by the low-temperature water;
and 4, step 4: dimethyl sulfoxide generated by the reaction enters a crude product tank (9) and is discharged out for storage through a crude product discharge pump (12).
8. The method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 7, wherein the concentration of hydrogen peroxide is 24% -28%, and the mass ratio of dimethyl sulfide to hydrogen peroxide is 1: 2.0-1: 2.2.
9. The method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide according to claim 7, wherein the outlet temperature of the first-stage tubular reactor (3) is controlled to be 30-35 ℃, the outlet temperature of the second-stage tubular reactor (4) is controlled to be 40-50 ℃, the outlet temperature of the third-stage tubular reactor (5) is controlled to be 50-70 ℃, the outlet temperatures of the fourth-stage tubular reactor (6) and the fifth-stage tubular reactor (7) are controlled to be less than 70 ℃, and the outlet temperature of the sixth-stage tubular reactor (8) is controlled to be less than 20 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210425397.3A CN114805145A (en) | 2022-04-22 | 2022-04-22 | Device and method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210425397.3A CN114805145A (en) | 2022-04-22 | 2022-04-22 | Device and method for preparing dimethyl sulfoxide by oxidizing dimethyl sulfide with hydrogen peroxide |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104058911A (en) * | 2014-07-10 | 2014-09-24 | 联化科技股份有限公司 | Method for preparing sulfoxide or sulfone by using micro-channel reactor |
| CN104557628A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Method for oxidizing dimethyl sulfide |
| CN105439921A (en) * | 2014-08-26 | 2016-03-30 | 中国石油化工股份有限公司 | A method of producing dimethyl sulfoxide |
| CN107698472A (en) * | 2017-10-18 | 2018-02-16 | 辽宁省轻工设计院有限公司 | A kind of method that dimethyl sulfide prepares dimethyl sulfoxide (DMSO) |
| CN108840809A (en) * | 2018-07-17 | 2018-11-20 | 常州大学 | A kind of method of continuous synthesis dimethyl sulfone |
| CN112300033A (en) * | 2020-11-03 | 2021-02-02 | 刘继明 | Device and method for fully and continuously synthesizing 2-nitro-4-methylsulfonylbenzoic acid from 4-methylsulfonyltoluene |
| CN113072598A (en) * | 2021-04-02 | 2021-07-06 | 青岛凯源祥化工有限公司 | Method for continuously preparing emamectin benzoate and intermediate thereof |
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2022
- 2022-04-22 CN CN202210425397.3A patent/CN114805145A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557628A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Method for oxidizing dimethyl sulfide |
| CN104058911A (en) * | 2014-07-10 | 2014-09-24 | 联化科技股份有限公司 | Method for preparing sulfoxide or sulfone by using micro-channel reactor |
| CN105439921A (en) * | 2014-08-26 | 2016-03-30 | 中国石油化工股份有限公司 | A method of producing dimethyl sulfoxide |
| CN107698472A (en) * | 2017-10-18 | 2018-02-16 | 辽宁省轻工设计院有限公司 | A kind of method that dimethyl sulfide prepares dimethyl sulfoxide (DMSO) |
| CN108840809A (en) * | 2018-07-17 | 2018-11-20 | 常州大学 | A kind of method of continuous synthesis dimethyl sulfone |
| CN112300033A (en) * | 2020-11-03 | 2021-02-02 | 刘继明 | Device and method for fully and continuously synthesizing 2-nitro-4-methylsulfonylbenzoic acid from 4-methylsulfonyltoluene |
| CN113072598A (en) * | 2021-04-02 | 2021-07-06 | 青岛凯源祥化工有限公司 | Method for continuously preparing emamectin benzoate and intermediate thereof |
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