CN114105840B - Method for preparing dimethyl sulfoxide from dimethyl sulfide - Google Patents
Method for preparing dimethyl sulfoxide from dimethyl sulfide Download PDFInfo
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- CN114105840B CN114105840B CN202111385969.1A CN202111385969A CN114105840B CN 114105840 B CN114105840 B CN 114105840B CN 202111385969 A CN202111385969 A CN 202111385969A CN 114105840 B CN114105840 B CN 114105840B
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- dimethyl sulfide
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- dimethyl
- dimethyl sulfoxide
- sulfide
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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 84
- 238000000034 method Methods 0.000 title claims abstract description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 35
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 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
- 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
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 31
- 230000001590 oxidative effect Effects 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract 1
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 35
- 239000012071 phase Substances 0.000 description 13
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 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
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 3
- 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
- 230000010718 Oxidation Activity Effects 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
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000003960 organic solvent Substances 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
- 229910052573 porcelain Inorganic materials 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
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 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
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 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
- 230000001105 regulatory effect Effects 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
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, and relates to a method for preparing dimethyl sulfoxide by using dimethyl sulfide. The method is that under pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -oxidation reaction at 10-70 ℃. And mixing dimethyl sulfide, water and dimethyl sulfoxide according to the molar ratio of the solution (1-5:0.5-1:1). Under the conditions of specific temperature, pressure, liquid level and active oxidation carrier, hydrogen peroxide (27.5% -70%) and dimethyl sulfide are introduced into the two-phase mixed solution. And (3) taking hydrogen peroxide as an oxidant, and carrying out continuous oxidation reaction in a tower reactor with a large length-diameter ratio, wherein 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, pressure, liquid level and active oxidation carrier of the reaction system. By the embodiment, the method has the advantages of 95-98% of reaction conversion rate (hydrogen peroxide) and 93-98% of yield (dimethyl sulfoxide), and realizes the efficient, safe, environment-friendly and high-selectivity method for preparing the dimethyl sulfoxide by oxidizing the dimethyl sulfide.
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 an emerging extractant developed in the 60 th century, and the dimethyl sulfoxide molecule contains semi-polar sulfur-oxygen groups which can effectively form coordination complexes or solvates 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. The organic solvent is a polar organic solvent, and has the characteristics of good solubility and strong permeability for organic matters and inorganic matters. Therefore, the method is widely applied to the fields of electronics, carbon fibers, medicines, pesticides, organic synthesis, precious metal extraction and the like.
Dimethyl sulfide and hydrogen peroxide oxidation are the most direct method for preparing dimethyl sulfoxide, and researchers also explore a plurality of different oxidation systems to realize the conversion. The dimethyl sulfoxide is generally prepared by dimethyl sulfide under the action of an oxidant, and the oxidation reaction inevitably affects the safety and the environment due to different oxidant types. The traditional dimethyl sulfoxide preparation method adopts nitrogen dioxide as an oxidant and pure oxygen and dimethyl sulfide as raw materials. In the method, dimethyl sulfide is oxidized into heterogeneous gas phase oxidation reaction, so that potential safety hazard is high; in the reaction process, a large amount of nitrogen oxides are discharged from a gas phase, and in order to eliminate nitrogen dioxide, alkali is added into a liquid phase for neutralization, and sodium nitrate waste salt is generated. Dimethyl sulfide has a low boiling point (36.5 ℃) and steam and oxygen are easy to form explosive mixtures, and safety accidents caused by the oxidation reaction in the industrial production process are numerous. Therefore, the development of a novel method which is safe and efficient and has no three-waste emission has important significance in both safety and environmental impact.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing dimethyl sulfoxide by dimethyl sulfide, which solves the problems of poor safety, environmental pollution and the like
The present invention has been achieved in such a way that,
a method for preparing dimethyl sulfoxide from dimethyl sulfide, the method comprising:
dimethyl sulfide, water and dimethyl sulfoxide are mixed according to the molar ratio of 1-5:0.5-1:1 to form a two-phase mixed solution;
placing an active oxidation carrier in the two-phase mixed solution;
and (3) introducing hydrogen peroxide and dimethyl sulfide into the two-phase mixed solution, and performing 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: pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -10-70 ℃.
Further, the active oxidation carrier is zeolite, active carbon, silica gel, alkali metal oxide or oxidized porcelain ball, and the weight ratio of the active oxidation carrier to the mixed solution is 1:0.1-1: 100.
further, 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%.
Further, 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, a fixed bed reactor is adopted as the reactor, and the length-diameter ratio of the reactor is in the range of 1: and the position of introducing dimethyl sulfide and hydrogen peroxide is positioned below the liquid level of the two-phase mixed solution in a ratio of 1-20:1.
Further, the oxidation reaction time is 0.01s to 100s.
Compared with the prior art, the invention has the beneficial effects that:
1. the reaction products of the invention are dimethyl sulfoxide and water, and the reaction products of the traditional method are dimethyl sulfoxide and nitrogen dioxide. Compared with the method, the method does not generate a large amount of nitrogen oxide tail gas; a large amount of waste salts containing organic matters generated in the separation process of dimethyl sulfoxide and nitrogen dioxide are avoided; and the potential safety hazard generated by separating the waste salt.
2. By controlling the temperature, pressure, liquid level and the addition amount of the active oxidation carrier of the reaction system. So that the dimethyl sulfide is oxidized to the dimethyl sulfoxide stage, and the hydrogen peroxide oxidation activity is always kept. And dimethyl sulfoxide is used as an oxidation product and a solvent, and does not participate in oxidation reaction.
3. Dimethyl sulfide and hydrogen peroxide are subjected to continuous reaction in a 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 is a reactor with large length-diameter ratio, and the position for introducing dimethyl sulfide and 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 and the dimethyl sulfide are fully contacted, the continuous oxidation reaction can be realized, and the large-scale continuous industrial production is facilitated.
Drawings
FIG. 1 is a schematic illustration of a reaction performed in a reactor according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
A method for preparing dimethyl sulfoxide from dimethyl sulfide, the method comprising:
dimethyl sulfide, water and dimethyl sulfoxide are mixed according to the molar ratio of 1-5:0.5-1:1 to form a two-phase mixed solution;
placing an active oxidation carrier in the two-phase mixed solution;
and (3) introducing hydrogen peroxide and dimethyl sulfide into the two-phase mixed solution, and performing 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: -10-70 ℃.
The active oxidation carrier is selected from zeolite, active carbon, silica gel, alkali metal oxide or oxidized porcelain ball, 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, a fixed bed reactor is used as the reactor, and the aspect ratio of the reactor ranges from 1: 1-20:1, a heat exchange tube and a jacket heat-taking facility are arranged in the reactor, and facilities such as temperature measurement, pressure measurement and liquid level are arranged, and the position of introducing dimethyl sulfide and hydrogen peroxide 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 invention:
main reaction (dimethyl sulfoxide formation): c (C) 2 H 6 S+H 2 O 2 →C 2 H 6 OS+H 2 O
Side reaction (formation of dimethyl sulfone): c (C) 2 H 6 S+2H 2 O 2 →C 2 H 6 O 2 S+2H 2 O
(2) Conversion and yield definitions of the invention:
conversion (hydrogen peroxide) = [ (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 formed/mass of dimethyl sulfoxide theoretically consumed all conversion of dimethyl sulfide to 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 concentration of dimethyl sulfide by mass percent is more preferably 10 to 50%.
(4) The reaction pressure of the invention: 0.0 MPa.G-0.3 MPa.G, temperature: -10-70 ℃; the reaction system temperature is more preferably 0 to 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 surface. In order to increase the residence time of the hydrogen peroxide in the mixed dissolution, the solution is adjusted according to the liquid level of the solution. And regulating the flow and the concentration of the hydrogen peroxide and the dimethyl sulfide. And selecting the optimal solution level.
(6) Controlling the temperature, pressure, liquid level and the adding amount of the active oxidation carrier of the reaction system. So that the dimethyl sulfide is oxidized to the dimethyl sulfoxide stage, and the hydrogen peroxide oxidation activity is always kept. And dimethyl sulfoxide is used as an oxidation product and a solvent, and does not participate in oxidation reaction. The weight ratio of the carrier to the mixed solution added to the reactor is 0.1-100.0:1, more preferably 0.5-10.0:1.
(7) Under the action of oxydol (27.5%, 35%, 50%, 70%) oxidants and active oxidation carriers with different concentrations, dimethyl sulfide is consumed by the oxydol, and the reaction is fast carried out. Wherein the reaction time for oxidizing dimethyl sulfide to generate dimethyl sulfoxide is 0.01 s-100 s.
Examples
Example 1 the reagents were formulated in this example 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 zeolite. The concentration of hydrogen peroxide is selected to be 27.5% at the flow rate of 50mL/min and the flow rate of 30 mL/min. The reaction temperature was kept at 25℃and the pressure at 0.01MPa.G, and the reaction was continued for 30 minutes. Detecting and calculating: the conversion rate of hydrogen peroxide is 96.5%, and the yield of dimethyl sulfide is 95.1%.
Example 2 the reagents of this example were formulated as a mixture 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 hydrogen peroxide is selected to be 27.5% at the flow rate of 50mL/min and the flow rate of 30 mL/min. The reaction temperature was kept at 15℃and the pressure at 0.01MPa.G, and the reaction was continued for 30 minutes. Detecting and calculating: the conversion rate of hydrogen peroxide is 95.4%, and the yield of dimethyl sulfide is 96.2%.
Example 3 the reagents of this example were formulated as a mixture of dimethyl sulfide, water and dimethyl sulfoxide: the weight ratio of the carrier to the reagent is 1:2, and the carrier is silica gel. The concentration of hydrogen peroxide is selected to be 27.5% at the flow rate of 50mL/min and the flow rate of 30 mL/min. The reaction temperature was kept at 5℃and the pressure at 0.01MPa.G, and the reaction was continued for 30 minutes. Detecting and calculating: the conversion rate of hydrogen peroxide is 95.1%, and the yield of dimethyl sulfide is 97.5%.
Example 4 the reagents of this example were formulated as a mixture of dimethyl sulfide, water and dimethyl sulfoxide: the weight ratio of the carrier to the reagent is 1:20. The concentration of hydrogen peroxide is selected to be 35% at the flow rate of 50mL/min and the flow rate of 30mL/min of dimethyl sulfide. The reaction temperature was kept at 5℃and the pressure at 0.01MPa.G, and the reaction was continued for 30 minutes. Detecting and calculating: the conversion rate of hydrogen peroxide is 97.5%, and the yield of dimethyl sulfide is 96.1%.
Example 5 the reagents of this example were formulated as a mixture of dimethyl sulfide, water and dimethyl sulfoxide: the weight ratio of the carrier to the reagent is 1:8, and the carrier is alkali metal oxide. The concentration of hydrogen peroxide is selected to be 35% at the flow rate of 50mL/min and the flow rate of 30mL/min of dimethyl sulfide. The reaction temperature was kept at 15℃and the pressure at 0.01MPa.G, and the reaction was continued for 30 minutes. Detecting and calculating: the conversion rate of hydrogen peroxide is 97.6%, and the yield of dimethyl sulfide is 95.2%.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (5)
1. A method for preparing dimethyl sulfoxide from dimethyl sulfide, which is characterized by comprising the following steps:
dimethyl sulfide, water and dimethyl sulfoxide are mixed according to the molar ratio of 1-5:0.5-1:1 to form a two-phase mixed solution;
placing an active oxidation carrier in the two-phase mixed solution;
hydrogen peroxide and dimethyl sulfide are introduced into the two-phase mixed solution, and continuous oxidation reaction is carried out 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 active oxidation carrier is selected from zeolite, active carbon or silica gel, and the weight ratio of the active oxidation carrier to the mixed solution is 1:0.1-1: 100;
the reactor adopts a fixed bed reactor, and the length-diameter ratio range of the reactor is 1: 1-20:1, the position of introducing dimethyl sulfide and hydrogen peroxide is positioned below the liquid surface of the two-phase mixed solution.
2. The method according to claim 1, wherein the oxidation reaction conditions are: pressure: 0.0 MPa.G-0.3 MPa.G, temperature: -10-70 ℃.
3. The method of claim 1, wherein the hydrogen peroxide is 27.5-70% by mass and the dimethyl sulfide is > 90% by mass.
4. The method according to claim 3, wherein the flow rate of hydrogen peroxide is 0.001-10.0 t/h and the flow rate of dimethyl sulfide is 0.001-20.0 t/h.
5. The method according to any one of claims 1 to 4, wherein the oxidation reaction time is 0.01s to 100s.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
|---|---|---|---|---|
| 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 |
| 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 |
| 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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