CN114105840A - Method for preparing dimethyl sulfoxide from dimethyl sulfide - Google Patents
Method for preparing dimethyl sulfoxide from dimethyl sulfide Download PDFInfo
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- CN114105840A CN114105840A CN202111385969.1A CN202111385969A CN114105840A CN 114105840 A CN114105840 A CN 114105840A CN 202111385969 A CN202111385969 A CN 202111385969A CN 114105840 A CN114105840 A CN 114105840A
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- dimethyl sulfide
- hydrogen peroxide
- dimethyl sulfoxide
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- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 title claims abstract description 186
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 93
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 37
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 4
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 239000010457 zeolite Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 25
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract 1
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 description 13
- 239000012071 phase Substances 0.000 description 13
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 4
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- XOCUXOWLYLLJLV-UHFFFAOYSA-N [O].[S] Chemical group [O].[S] XOCUXOWLYLLJLV-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- GRKWHXNAHIMNJD-UHFFFAOYSA-N methoxysulfanyloxymethane Chemical compound COSOC GRKWHXNAHIMNJD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- -1 organic synthesis Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of dimethyl sulfoxide preparation, belongs to a method for preparing dimethyl sulfoxide from dimethyl sulfide, and relates to a method for preparing dimethyl sulfoxide. The method is characterized in that under the conditions of pressure: 0.0 MPa.G-0.3 MPa.G, temperature: and (3) carrying out oxidation reaction at the temperature of-10-70 ℃. Mixing dimethyl sulfide, water and dimethyl sulfoxide according to a molar ratio of the solution (1-5:0.5-1: 1). Under the conditions of specific temperature, pressure, liquid level and active oxidation carrier, introducing hydrogen peroxide (27.5% -70%) and dimethyl sulfide into the two-phase mixed solution. Hydrogen peroxide is used as an oxidant, continuous oxidation reaction is carried out in a tower reactor with large length-diameter ratio, and the oxidized dimethyl sulfide is converted into dimethyl sulfoxide in the process. The continuous production process of continuous feeding and discharging is realized by controlling the temperature, the pressure, the liquid level and the active oxidation carrier of the reaction system. By the embodiment, the reaction conversion rate (hydrogen peroxide) is 95-98%, the yield (dimethyl sulfoxide) is 93-98%, and the method for preparing the dimethyl sulfoxide by oxidizing the dimethyl sulfide is efficient, safe, environment-friendly and high in selectivity.
Description
Technical Field
The invention belongs to the field of dimethyl sulfoxide preparation, and particularly relates to a method for preparing dimethyl sulfoxide from dimethyl sulfide.
Background
Dimethyl sulfoxide is a typical fine chemical product. Is an important intermediate in the fields of electronics, carbon fiber, medicine, pesticide, organic synthesis and the like, and has wide application. Dimethyl sulfoxide is a high-efficiency organic solvent and a new extracting agent developed in the 60 th of the 20 th century, and the molecule of the dimethyl sulfoxide contains a semipolar sulfur-oxygen group which can effectively generate a coordination complex or a solvate with metal ions. Therefore, the dimethyl sulfoxide can extract noble metals such as gold, silver, platinum and the like in hydrochloric acid and sulfuric acid media, and can also extract rare earth elements such as uranium, thorium and the like. More expensive, it is a polar organic solvent, and has the characteristics of good solubility and strong permeability for organic matters and inorganic matters. Therefore, the method has wide application in the fields of electronics, carbon fiber, medicine, pesticide, organic synthesis, precious metal extraction and the like.
The oxidation of dimethyl sulfide and hydrogen peroxide is the most direct method for preparing dimethyl sulfoxide, and researchers also explore a variety of different oxidation systems to realize the conversion. The preparation of dimethyl sulfoxide is generally carried out by dimethyl sulfide under the action of an oxidizing agent, and due to different types of the oxidizing agent, the oxidation reaction inevitably brings influence on safety and environment. The traditional dimethyl sulfoxide preparation method is a preparation method which adopts nitrogen dioxide as an oxidant and pure oxygen and dimethyl sulfide as raw materials. According to the method, dimethyl sulfide is oxidized into heterogeneous gas phase oxidation reaction, so that the potential safety hazard is large; in the reaction process, a large amount of nitrogen oxides are discharged from a gas phase, and in order to eliminate nitrogen dioxide, alkali needs to be added into a liquid phase for neutralization, and sodium nitrate waste salt is generated. Dimethyl sulfide has a low boiling point (36.5 ℃), and the steam and oxygen are easy to form explosive mixtures, so that safety accidents caused by the oxidation reaction in the industrial production process are more. Therefore, the development of a new method which is safe and efficient and has no three-waste discharge has important significance in the aspects of safety and environmental influence.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing dimethyl sulfoxide from dimethyl sulfide, which solves the problems of poor safety, environmental pollution and the like
The present invention is achieved in such a way that,
a method for preparing dimethyl sulfoxide from dimethyl sulfide, which comprises the following steps:
dimethyl sulfide, water and dimethyl sulfoxide are mixed into a two-phase mixed solution according to the molar ratio of the solution to 1-5:0.5-1: 1;
putting an active oxidation carrier into the two-phase mixed solution;
introducing hydrogen peroxide and dimethyl sulfide into the two-phase mixed solution, and carrying out continuous oxidation reaction in a tower reactor with a large length-diameter ratio, wherein the molar ratio of the hydrogen peroxide to the dimethyl sulfide is 1: 1.
Further, the oxidation reaction conditions are as follows: pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -10 to 70 ℃.
Further, the active oxidation carrier is zeolite, active carbon, silica gel, alkali metal oxide or oxidized ceramic balls, and the weight ratio of the active oxidation carrier to the mixed solution is 1: 0.1-1: 100.
furthermore, the mass percentage concentration of the hydrogen peroxide is 27.5-70%, and the mass percentage concentration of the dimethyl sulfide is more than 90%.
Furthermore, the flow rate of the hydrogen peroxide is 0.001-10.0 t/h, and the flow rate of the dimethyl sulfide is 0.001-20.0 t/h.
Further, the reactor adopts a fixed bed reactor, and the length-diameter ratio range of the reactor is 1: 1-20: 1, wherein the position where the dimethyl sulfide and the hydrogen peroxide are introduced is below the liquid level of the two-phase mixed solution.
Further, the oxidation reaction time is 0.01s to 100 s.
Compared with the prior art, the invention has the beneficial effects that:
1. the reaction product of the invention is dimethyl sulfoxide and water, and the reaction product of the traditional method is dimethyl sulfoxide and nitrogen dioxide. Compared with the prior art, the method of the invention can not generate a large amount of nitrogen oxide tail gas; a large amount of waste salt containing organic matters generated in the separation process of dimethyl sulfoxide and nitrogen dioxide is avoided; and the potential safety hazard generated by separating waste salt.
2. The temperature, pressure, liquid level and the adding amount of the active oxidation carrier of the reaction system are controlled. So that the activity of hydrogen peroxide oxidation is always kept when dimethyl sulfide is oxidized to dimethyl sulfoxide. And dimethyl sulfoxide is used as an oxidation product and a solvent and does not participate in the oxidation reaction any more.
3. Dimethyl sulfide and hydrogen peroxide are continuously reacted in the reactor, and reaction heat is timely removed through a heat exchange facility in the reactor, so that potential safety hazards are reduced, and side reactions are reduced.
4. The reactor of the invention is a reactor with large length-diameter ratio, and the position for introducing the dimethyl sulfide and the hydrogen peroxide is positioned below the liquid level of the mixed solution. The dimethyl sulfide and the hydrogen peroxide continuously enter the mixed solution, so that the hydrogen peroxide is fully contacted with the dimethyl sulfide, the continuous oxidation reaction can be favorably carried out, and the large-scale continuous industrial production is favorably realized.
Drawings
FIG. 1 is a schematic diagram of a reactor provided in an embodiment of the present invention for carrying out a reaction.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for preparing dimethyl sulfoxide from dimethyl sulfide, which comprises the following steps:
dimethyl sulfide, water and dimethyl sulfoxide are mixed into a two-phase mixed solution according to the molar ratio of the solution to 1-5:0.5-1: 1;
putting an active oxidation carrier into the two-phase mixed solution;
introducing hydrogen peroxide and dimethyl sulfide into the two-phase mixed solution, and carrying out continuous oxidation reaction in a tower reactor with a large length-diameter ratio, wherein the molar ratio of the hydrogen peroxide to the dimethyl sulfide is 1: 1.
The oxidation reaction conditions are as follows: pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -10 to 70 ℃.
The active oxidation carrier is selected from zeolite, activated carbon, silica gel, alkali metal oxide or oxidized ceramic balls, and the weight ratio of the active oxidation carrier to the mixed solution is 1: 0.1-1: 100.
the mass percentage concentration of the hydrogen peroxide is 27.5-70%, and the mass percentage concentration of the dimethyl sulfide is more than 90%. The flow rate of the hydrogen peroxide is 0.001-10.0 t/h, and the flow rate of the dimethyl sulfide is 0.001-20.0 t/h. Referring to fig. 1, the reactor is a fixed bed reactor, and the length-diameter ratio of the reactor is 1: 1-20: 1, wherein the reactor is provided with heat exchange tubes, jacket heat-taking facilities, temperature measuring, pressure measuring, liquid level and other facilities, and the position where the dimethyl sulfide and the hydrogen peroxide are introduced is positioned below the liquid level of the two-phase mixed solution.
The oxidation reaction time is 0.01 s-100 s.
(1) The reaction mechanism of the present invention:
main reaction (formation of dimethyl sulfoxide): c2H6S+H2O2→C2H6OS+H2O
Side reaction (formation of dimethyl sulfone): c2H6S+2H2O2→C2H6O2S+2H2O
(2) The conversion and yield of the present invention are defined as follows:
conversion (hydrogen peroxide) ═ mass [ (mass of added hydrogen peroxide-mass of unreacted hydrogen peroxide)/mass of added hydrogen peroxide ] + 100%,
yield (dimethyl sulfide) — (mass of dimethyl sulfoxide actually newly produced/theoretical consumption of dimethyl sulfide all converted to mass of dimethyl sulfoxide) × 100%.
(3) By combining the method and the attached drawing, a two-phase mixed solution with the mass concentration of 10-80% of dimethyl sulfide is prepared in a reactor by taking dimethyl sulfoxide, water and dimethyl sulfide as media. The mass percentage concentration of dimethyl sulfide is more preferably 10-50%.
(4) The reaction pressure of the invention is as follows: 0.0 MPa.G-0.3 MPa.G, temperature: -10 to 70 ℃; the temperature of the reaction system is more preferably 0-40 ℃.
(5) Dimethyl sulfide and hydrogen peroxide continuously enter the mixed solution and diffuse from the bottom of the reactor to the upper part of the liquid level. In order to increase the retention time of the hydrogen peroxide in the mixed solution, the adjustment is carried out according to the liquid level height of the solution. Adjusting the flow rates of the hydrogen peroxide and the dimethyl sulfide and the concentration of the hydrogen peroxide. Selecting the optimal solution of the solution level height.
(6) Controlling the temperature, pressure, liquid level of the reaction system and the adding amount of the active oxidation carrier. So that the activity of hydrogen peroxide oxidation is always kept when dimethyl sulfide is oxidized to dimethyl sulfoxide. And dimethyl sulfoxide is used as an oxidation product and a solvent and does not participate in the oxidation reaction any more. The weight ratio of the carrier added into the reactor to the mixed solution is 0.1-100.0: 1, and more preferably 0.5-10.0: 1.
(7) Under the action of oxidants of hydrogen peroxide with different concentrations (27.5%, 35%, 50% and 70%) and active oxidation carriers, the dimethyl sulfide is consumed by the hydrogen peroxide, and the reaction is rapidly carried out. Wherein the reaction time for oxidizing the dimethyl sulfide into the dimethyl sulfoxide is 0.01 s-100 s.
Examples
Example 1, the reagent in this example was prepared to prepare a two-phase mixed solution of dimethyl sulfide, water and dimethyl sulfoxide: the weight ratio of the carrier to the two-phase mixed solution is 1:2, and the carrier is selected from zeolite. The concentration of the hydrogen peroxide is selected to be 27.5 percent at the flow rate of 50mL/min and the flow rate of 30 mL/min. The reaction temperature is kept at 25 ℃, the pressure is kept at 0.01MPa.G, and the reaction is continued for 30 min. Detection and calculation: the conversion rate of hydrogen peroxide is 96.5%, and the yield of dimethyl sulfide is 95.1%.
Example 2, the reagent prepared in this example, the mixed reagent of dimethyl sulfide, water and dimethyl sulfoxide: the weight ratio of the carrier to the reagent is 1:2, and the carrier is activated carbon. The concentration of the hydrogen peroxide is selected to be 27.5 percent at the flow rate of 50mL/min and the flow rate of 30 mL/min. Keeping the reaction temperature at 15 ℃ and the pressure at 0.01MPa.G, and continuously reacting for 30 min. Detection and calculation: the conversion rate of hydrogen peroxide is 95.4%, and the yield of dimethyl sulfide is 96.2%.
Example 3, reagents were prepared in this example, and a mixed reagent of dimethyl sulfide, water and dimethyl sulfoxide was prepared: the weight ratio of the carrier to the reagent is 1:2, and the carrier is silica gel. The concentration of the hydrogen peroxide is selected to be 27.5 percent at the flow rate of 50mL/min and the flow rate of 30 mL/min. Keeping the reaction temperature at 5 ℃ and the pressure at 0.01MPa.G, and continuously reacting for 30 min. Detection and calculation: the conversion rate of hydrogen peroxide is 95.1%, and the yield of dimethyl sulfide is 97.5%.
Example 4, reagents were prepared in this example, a mixed reagent of dimethyl sulfide, water and dimethyl sulfoxide was prepared: the weight ratio of the carrier to the reagent is 1: 20. Hydrogen peroxide with the flow rate of 50mL/min and dimethyl sulfide with the flow rate of 30mL/min, wherein the concentration of the hydrogen peroxide is selected to be 35%. Keeping the reaction temperature at 5 ℃ and the pressure at 0.01MPa.G, and continuously reacting for 30 min. Detection and calculation: the conversion rate of hydrogen peroxide is 97.5%, and the yield of dimethyl sulfide is 96.1%.
Example 5, reagents were prepared in this example, and a mixed reagent of dimethyl sulfide, water and dimethyl sulfoxide was prepared: the weight ratio of the carrier to the reagent is 1:8, and the carrier is alkali metal oxide. Hydrogen peroxide with the flow rate of 50mL/min and dimethyl sulfide with the flow rate of 30mL/min, wherein the concentration of the hydrogen peroxide is selected to be 35%. Keeping the reaction temperature at 15 ℃ and the pressure at 0.01MPa.G, and continuously reacting for 30 min. Detection and calculation: the conversion rate of hydrogen peroxide is 97.6%, and the yield of dimethyl sulfide is 95.2%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A method for preparing dimethyl sulfoxide from dimethyl sulfide is characterized by comprising the following steps:
dimethyl sulfide, water and dimethyl sulfoxide are mixed into a two-phase mixed solution according to the molar ratio of the solution to 1-5:0.5-1: 1;
putting an active oxidation carrier into the two-phase mixed solution;
introducing hydrogen peroxide and dimethyl sulfide into the two-phase mixed solution, and carrying out continuous oxidation reaction in a tower reactor with a large length-diameter ratio, wherein the molar ratio of the hydrogen peroxide to the dimethyl sulfide is 1: 1.
2. The method of claim 1, wherein the oxidation reaction conditions are: pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -10 to 70 ℃.
3. The method according to claim 1, wherein the active oxidation carrier is selected from zeolite, activated carbon, silica gel, alkali metal oxide or oxidized ceramic balls, and the weight ratio of the active oxidation carrier to the mixed solution is 1: 0.1-1: 100.
4. the method according to claim 1, wherein the concentration of hydrogen peroxide is 27.5-70% by mass, and the concentration of dimethyl sulfide is more than 90% by mass.
5. The method according to claim 1 or 4, wherein the flow rate of the hydrogen peroxide is 0.001-10.0 t/h, and the flow rate of the dimethyl sulfide is 0.001-20.0 t/h.
6. The method of claim 1, wherein the reactor is a fixed bed reactor, and the length-diameter ratio of the reactor is in a range of 1: 1-20: 1, wherein the position where the dimethyl sulfide and the hydrogen peroxide are introduced is positioned on the liquid level of the two-phase mixed solution.
7. The process according to any one of claims 1 to 6, wherein the oxidation reaction time is from 0.01s to 100 s.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787932A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of dimethyl sulfoxide |
| CN103787931A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Production method of dimethyl sulfoxide |
| CN104549549A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Method for molding tin-silicon molecular sieve, molded tin-silicon molecular sieve prepared by method and method for preparing 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) |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787932A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of dimethyl sulfoxide |
| CN103787931A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Production method of dimethyl sulfoxide |
| CN104549549A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Method for molding tin-silicon molecular sieve, molded tin-silicon molecular sieve prepared by method and method for preparing 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) |
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