CN104058911A - Method for preparing sulfoxide or sulfone by using micro-channel reactor - Google Patents

Abstract

The invention discloses a method for preparing sulfoxide and sulfone by utilizing a microchannel reactor. The invention provides a method for preparing sulfoxide or sulfone, which comprises the following steps: the homogeneous solution formed by thioether 1 and a solvent, and the oxidizing agent are injected into a microchannel reactor through a metering pump respectively, contacted in the microchannel and Carry out the oxidation reaction to obtain sulfoxide or sulfone, and the time of the oxidation reaction is 1 second to 300 seconds; the preparation method of the present invention has extremely short reaction time, precise control of reaction conditions, high safety, and is suitable for kilogram-level products Rapid preparation, continuous production, high selectivity of sulfoxide and sulfone, high product yield, good purity, suitable for large-scale industrial production.

Description

A kind of method utilizing microchannel reactor to prepare sulfoxide or sulfone

technical field

The invention relates to a method for preparing sulfoxide or sulfone using a microchannel reactor.

Background technique

Sulfoxide and sulfone are important chemical raw materials and intermediates for the synthesis of other pharmaceuticals and pesticides. They are mainly used in fine chemicals, pharmaceuticals, pesticides, synthetic fibers, plastics, printing and dyeing, rare metal extractants, and organic synthesis. Sulfoxides and sulfones are mainly used as raw materials for pharmaceuticals and other organic synthesis, and are also used in antacid and anti-ulcer drugs, ophthalmic medicines, anti-leprosy drugs, antibiotics, stimulant drugs such as armodafinil, herbicides and insecticides , Electrolyte functional additive, can also be used as raw material for engineering plastics and membrane materials.

At present, sulfoxide and sulfone are prepared by the oxidation method of sulfide and nitric acid and nitrate, the synthesis method of sulfide and halogen compound, the catalytic method of metal oxide, the peroxide reaction method such as hydrogen peroxide, and the oxygen oxidation method commonly used in industry. However, the existing preparation method has disadvantages such as expensive catalyst, difficult to remove, cumbersome operation, need to drop oxidant in batches, long reaction time, it takes more than ten hours to complete the reaction, potential safety hazard, violent reaction exotherm, easy flushing or even explosion and other defects.

Finding a short reaction time, precise control of reaction conditions, high safety, suitable for kilogram-scale products, and an environmentally friendly preparation method for the industrial production of sulfoxide or sulfone is a technical problem that needs to be solved urgently.

Contents of the invention

The technical problem to be solved by the present invention is to overcome the long reaction time and high risk of reaction in the preparation method of sulfoxide or sulfone in the prior art, which is not suitable for the preparation of kilogram-level products, cannot be continuously produced, and has poor selectivity between sulfoxide and sulfone , low product yield, poor purity, unsuitable for large-scale industrial production, and provides a method for preparing sulfoxide or sulfone using a microchannel reactor. The preparation method of the present invention has extremely short reaction time, precise control of reaction conditions, high safety, is suitable for rapid preparation of kilogram-level products, can be continuously produced, has high selectivity for sulfoxide or sulfone, high product yield, good purity, and is suitable for in large-scale industrial production.

The invention provides a method for preparing sulfoxide or sulfone, which comprises the following steps:

The homogeneous solution formed by thioether 1 and the solvent, and the oxidizing agent are pumped into the microchannel reactor through the metering pump, contact and carry out the oxidation reaction in the microchannel to obtain sulfoxide or sulfone, and the time for the oxidation reaction is 1 second to 300 seconds;

Wherein, R ₁ and R ₂ are each independently substituted or unsubstituted C ₁ -C ₆ alkyl (the "substituted or unsubstituted C ₁ -C ₆ alkyl" is preferably substituted or unsubstituted C ₁ -C 6 alkyl C ₄ Alkyl, such as substituted or unsubstituted methyl, substituted or unsubstituted ethyl, substituted or unsubstituted propyl, substituted or unsubstituted isopropyl, substituted or unsubstituted n-butyl, substituted or Unsubstituted isobutyl, or substituted or unsubstituted tert-butyl; the "substituted methyl" can be trifluoromethyl), substituted or unsubstituted C ₅ -C ₁₀ aryl (the described "Substituted or unsubstituted C ₅ -C ₁₀ aryl" is preferably substituted or unsubstituted C ₅ -C ₆ aryl, and the substituted or unsubstituted C ₅ -C ₆ aryl is preferably substituted or unsubstituted benzene Base; The substituted phenyl is preferably 2-nitrophenyl, 3-nitrophenyl, 4-nitrophenyl or ) or a substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl group (preferably "a substituted or unsubstituted C ₄ -C ₇ heterocyclic aryl group whose heteroatom is nitrogen or oxygen atom, and the number of heteroatoms is 1-3 ", the "heteroatom is nitrogen or oxygen atom, substituted C ₄ ~ C ₇ heterocyclic aryl group with 1-3 heteroatoms" is preferably "substituted or unsubstituted benzimidazolyl" or "substituted Or unsubstituted pyridyl"; the substituted benzimidazolyl is preferably or The substituted pyridyl is preferably or ), the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted heterocyclic aryl""Substituted" is C ₁ -C ₆ alkyl (preferably C ₁ -C ₄ alkyl, such as methyl, ethyl, propyl, isopropyl, n-butyl, isobutyl or tert-butyl), C ₁ -C ₆ alkoxy (preferably methoxy), nitro, halogen (such as F, Cl, Br or I, preferably Br or Cl), and "halogen substituted C ₁ -C ₆ alkyl" (preferably "halogen substituted C ₁ -C ₄ alkyl", the "halogen" can be fluorine, chlorine or bromine; for example, halogen substituted methyl, halogen One or more of substituted ethyl, halogen-substituted propyl, halogen-substituted isopropyl or halogen-substituted tert-butyl; the halogen-substituted methyl is preferably difluoromethyl or trifluoromethyl) Substituted, when there are multiple substituents, the substituents may be the same or different.

In the method for preparing sulfoxide or sulfone, the microchannel reactor can be of commercial type. The size of the microchannel is between 10um and 1000um. Further preference is given to Corning microchannel reactors.

In the method for preparing sulfoxide, the solvent can be a conventional solvent for this type of reaction in the art, and alcohol solvents, nitrile solvents, carboxylic acid solvents, halogenated hydrocarbon solvents and water are particularly preferred in the present invention. one or more. The alcohol solvent is preferably C ₁ ~C ₄ alcohol solvent, and the C ₁ ~C ₄ alcohol solvent is preferably methanol and/or ethanol; the nitrile solvent is preferably acetonitrile; the carboxylic acid The solvent is preferably acetic acid; the halogenated hydrocarbon solvent is preferably a chlorinated hydrocarbon solvent, and the chlorinated hydrocarbon solvent is preferably dichloromethane. The solvent is further preferably methanol, acetonitrile, methylene chloride, acetic acid or water, and further preferably acetic acid.

In the method for preparing sulfone, the solvent may be a conventional solvent for this type of reaction in the art, and one or more of carboxylic acid solvents, halogenated hydrocarbon solvents and water are particularly preferred in the present invention. The carboxylic acid solvent is preferably acetic acid; the halogenated hydrocarbon solvent is preferably a chlorinated hydrocarbon solvent, and the chlorinated hydrocarbon solvent is preferably methylene chloride. The solvent is further preferably methanol, acetonitrile, methylene chloride, acetic acid or water, and further preferably acetic acid.

In the method for preparing sulfoxide or sulfone, the mass ratio of the solvent to thioether 1 is preferably 1:1-15:1, more preferably 3:1-10:1.

In the method for preparing sulfoxide or sulfone, the oxidizing agent may be a conventional oxidizing agent for this type of oxidation reaction in the art, preferably hydrogen peroxide.

In the method for preparing sulfoxide or sulfone, when hydrogen peroxide is used as the oxidizing agent, the mass percentage of hydrogen peroxide is preferably 27% to 50%, and the mass percentage refers to the mass percentage of hydrogen peroxide in the total mass of hydrogen peroxide. percentage.

In the method for preparing sulfoxide or sulfone, the molar ratio of the oxidizing agent to the thioether 1 is preferably 1:1-8:1, more preferably 1.5:1-8:1. In the reaction to prepare sulfoxide, the molar ratio of the hydrogen peroxide to the thioether 1 is further preferably 1.5:1 to 3:1; in the reaction to prepare sulfone, the molar ratio of the hydrogen peroxide to the thioether 1 The molar ratio is still more preferably 3:1 to 7:1.

The method for preparing sulfoxide or sulfone is preferably carried out in the presence of a catalyst, which is a conventional catalyst for this type of reaction in the art, preferably tetraisopropyl titanate, titanium tartrate, sodium tungstate, phosphomolybdic acid , iron acetylacetonate, hydrochloric acid or sulfuric acid, more preferably sulfuric acid; Described hydrochloric acid can be conventional commercially available hydrochloric acid reagent in the art, and the mass percentage concentration of described hydrochloric acid is preferably 5%～37%, and described mass percentage Concentration refers to the percentage of the mass of hydrogen chloride in the total mass of hydrochloric acid aqueous solution.

In the method for preparing sulfoxide or sulfone, when the reaction is carried out in the presence of a catalyst, the mass ratio of the catalyst to the sulfide 1 is preferably 0 to 0.3 (but not including 0), more preferably 0 to 0.2 (but not including 0). In the reaction for preparing sulfoxide, when the reaction is carried out in the presence of a catalyst, the mass ratio of the catalyst to the thioether 1 is preferably 0.01-0.1, more preferably 0.01-0.05. In the reaction for preparing sulfone, when the reaction is carried out in the presence of a catalyst, the mass ratio of the catalyst to the thioether 1 is preferably 0.1-0.2.

In the method for preparing sulfoxide or sulfone, the oxidizing agent is preferably divided into 1 to 3 feeds; the homogeneous solution is preferably a single feed. In the method for preparing sulfone, it is further preferred that the oxidizing agent is preferably divided into 2-3 feeds; the homogeneous solution is preferably 1 feed alone.

The temperature of the oxidation reaction is preferably from 40°C to 150°C, more preferably from 50°C to 130°C, and still more preferably from 75°C to 120°C. When preparing sulfoxide, the temperature of the oxidation reaction is preferably 70°C-100°C, and when preparing sulfone, the temperature of the oxidation reaction is preferably 100°C-130°C.

In the method for preparing sulfoxide or sulfone, the oxidation reaction time is preferably 1 second to 50 seconds, more preferably 4 seconds to 15 seconds.

In the present invention, when not specified, the "alkyl" refers to a branched or straight-chain saturated aliphatic hydrocarbon group with a specified number of carbon atoms; as defined in "C ₁ ~ C ₂₀ alkyl" as Including 1, 2, 3, 4, 5, 6, 7, 8, 9, 11, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20 in a linear or branched structure group of carbon atoms. For example, "C ₁ -C ₁₀ alkyl" specifically includes methyl, ethyl, n-propyl, isopropyl, n-butyl, tert-butyl, isobutyl, pentyl, hexyl, heptyl, octyl, Nonyl and decyl and so on.

In the present invention, when not specified, the "aryl" refers to any stable monocyclic or bicyclic carbocycle with up to 7 atoms in each ring, wherein at least one ring is an aromatic ring; the above-mentioned aryl Examples of units include phenyl, naphthyl, tetrahydronaphthyl, indanyl, biphenyl, phenanthrenyl, anthracenyl or acenaphthyl. It is understood that where the aryl substituent is a bicyclic substituent and one of the rings is non-aromatic, the attachment is through the aromatic ring.

In the present invention, when not specified, the "heterocyclic aryl" means a stable monocyclic or bicyclic ring with up to 7 atoms in each ring, wherein at least one ring is an aromatic ring and contains 1-4 optional Heteroatoms from O, N, and S; heterocyclic aryl groups within the scope of this definition include, but are not limited to: acridinyl, carbazolyl, cinnolinyl, quinoxalinyl, pyrazolyl, indolyl, Benzotriazolyl, furyl, thienyl, benzothienyl, benzofuryl, quinolinyl, isoquinolyl, oxazolyl, isoxazolyl, indolyl, pyrazinyl, pyridazine Base, pyridyl, pyrimidinyl, pyrrolyl, tetrahydroquinoline. "Heteroaryl" should also be understood to include the N-oxide derivative of any nitrogen-containing heteroaryl. In cases where the heteroaryl substituent is a bicyclic substituent and one ring is non-aromatic or contains no heteroatoms, it is understood that attachment is through the aromatic ring or through the ring-containing heteroatom, respectively.

In the present invention, when not specified, the "halogen" means fluorine, chlorine, bromine, iodine or astatine.

In the present invention, the substituents of "C _x1 ~C _y1 " whose carbon number range is determined (x1 and y1 are integers), such as the alkyl group of "C _x1 ~C _y1 ", "C _x1 ~C _y1 " The aryl group in or the heterocyclic aryl group of "C _x1 ~ C _y1 " all represent the carbon number without substituents, for example, C ₁ ~C ₆ alkyl represents C ₁ ~C ₆ alkyl without substituents.

On the basis of not violating common knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily to obtain preferred examples of the present invention.

The reagents and raw materials used in the present invention are all commercially available.

In the present invention, the room temperature refers to ambient temperature, which is 10°C to 35°C.

The positive progress effect of the present invention is:

1. The present invention adopts a continuous-flow microchannel reactor, the reaction process is safe and stable, and there is no temperature and pressure runaway phenomenon, which solves the safety hazard of this type of reaction.

2. The reaction time is shortened from the traditional hours to tens of seconds, which significantly improves the reaction efficiency.

3. Raw materials, catalysts and accelerators are well mixed in the microchannel, the temperature is precisely controlled, and there is no back-mixing in the reaction.

4. The present invention adopts cheap and easy-to-get hydrogen peroxide as an oxidizing agent, avoids the use of more expensive peroxides such as m-chloroperoxybenzoic acid, potassium persulfate, etc., and improves the selectivity of the reaction in the microchannel reactor, and Reduced environmental pollution.

Description of drawings

Fig. 1 is the flow chart of reaction process for preparing sulfoxide and sulfone by sulfide oxidation of the present invention;

Fig. 2 is the Corning microchannel reactor flow diagram used in the present invention, 1,2-raw material tank, 3,4-material pump, 5,6-stop valve, 7-Corning microchannel, 8-raw material collection tank.

Fig. 3 is the Corning microchannel reactor multi-feed flow schematic diagram that the present invention uses, 1,2-raw material tank, 3,4,10-material pump, 5,6,11-stop valve, 7-Corning microchannel , 8-raw material collection tank.

Detailed ways

The present invention is further illustrated below by means of examples, but the present invention is not limited to the scope of the examples. For the experimental methods that do not specify specific conditions in the following examples, select according to conventional methods and conditions, or according to the product instructions.

Example 1

1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 300.0 grams of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 126.4 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize device Fig. 2 of the present invention, according to following steps: (1) the acetic acid solution that contains 2-(isopropylsulfide base) nitrobenzene enters microchannel reactor 7 by pump 3 in raw material tank 1, raw material tank 2 The oxidizing agent 30% hydrogen peroxide enters microchannel reactor 7 through pump 4; Ratio (that is the solution of 2-(isopropyl sulfide group) nitrobenzene+300.0 gram acetic acid of 100.0 grams: this ratio feeding of 126.4 grams of 30% hydrogen peroxide), is squeezed into microchannel reactor 7 through metering pump, in setting The fixed temperature is a mixed reaction at 95°C; (3) the residence time of the reaction material is controlled to be 5 seconds by adjusting the flow rate of the pump, and the two stocks of materials are mixed and reacted in the reaction module; (4) the reaction channel passes through the shut-off valve 5 and 6 to prevent the backflow of the material; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. In the reaction product, 0.32% of the raw material 2-(isopropylsulfide)nitrobenzene remains, the purity of sulfoxide is 97.6%, and the purity of sulfone is 0.2% (LC analysis results). Yield 95%.

Example 2

1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 300.0 grams of acetic acid, then add 1.0 grams of concentrated sulfuric acid dropwise to the container at room temperature, and stir Mix well and seal. Then weigh 126.4 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize device Fig. 2 of the present invention, according to following steps: (1) the acetic acid solution that contains 2-(isopropyl sulfide group) nitrobenzene, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3, The oxidizing agent mass percentage in raw material tank 2 is 30% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) enters microchannel reactor 7 by pump 4; (2) adopts in the reaction process Continuous flow microchannel reactor, the acetic acid solution of raw material 2-(isopropylsulfide group) nitrobenzene, concentrated sulfuric acid and oxidant according to the above ratio (i.e. 100.0 grams of 2-(isopropylsulfide group) nitrobenzene+300.0 The solution of gram acetic acid: 126.4 grams of 30% hydrogen peroxide (this ratio feeding), squeezes into microchannel reactor 7 through metering pump, is mixed reaction under 85 ℃ at the set temperature; (3) controls by the flow rate of regulating pump The residence time of the reaction material is 4 seconds, and the two stocks of materials are mixed and reacted in the reaction module; (4) the backflow of the material is prevented by stop valves 5 and 6 on the reaction channel; (5) after the mixed reaction through the microchannel 7, the oxidation The product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. The raw material 2-(isopropylsulfide)nitrobenzene has no residue in the reaction product, the purity of sulfoxide is 96.5%, and the purity of sulfone is 1.2% (LC analysis results). Yield 95%.

Example 3

1. Raw material preparation: Weigh 100.0 g of dimethyl sulfide, place it in a container and seal it, pour it into a container containing 300.0 g of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 401.4 grams of 30% hydrogen peroxide, place it in another container, and seal it.

2, utilize Fig. 2 device figure of the present invention, according to subordinate steps: (1) dimethyl sulfide enters microchannel reaction 7 by pump 3 in raw material tank 1, and the oxidant mass percentage in raw material tank 2 is the hydrogen peroxide of 30% ( Described mass percent refers to that the quality of hydrogen peroxide accounts for the percentage of hydrogen peroxide gross mass) enters microchannel reactor 7 by pump 4; (2) adopts continuous flow microchannel reactor in the reaction process, raw material dimethyl sulfide and The oxidizing agent is mixed according to the above ratio (that is, 100.0 grams of 2-methyl sulfide: 401.4 grams of 30% hydrogen peroxide feed), at a set temperature of 50 ° C; (3) controlled by adjusting the flow rate of the pump The residence time of the reaction material is 10 seconds, and the two stocks of materials are mixed and reacted in the reaction module; (4) on the reaction channel, stop valves 5 and 6 are used to prevent the backflow of the material; (5) after the mixed reaction of the microchannel 7, the oxidation The product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. The raw material dimethyl sulfide has no residue in the reaction product, the purity of sulfoxide is 99.0%, and the purity of sulfone is 0.1% (GC analysis result). Yield 98%.

Example 4

1. Raw material preparation: Weigh 100.0 g of diphenyl sulfide, pour it into a container containing 300.0 g of acetic acid, then add 5.0 g of concentrated sulfuric acid dropwise into the container at room temperature, stir to mix evenly, and then seal it. Then weigh 133.9 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 2 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains diphenyl sulfide, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3, and the oxygenant 30 in the raw material tank 2 % hydrogen peroxide enters microchannel reactor 7 by pump 4; solution+1.0 gram of concentrated sulfuric acid: 133.9 grams of 30% hydrogen peroxide (feeding ratio), mixed reaction at a set temperature of 100°C; (3) controlling the residence time of the reaction material by adjusting the flow rate of the pump to be 5 seconds , the two streams of materials are mixed and reacted in the reaction module; (4) on the reaction channel, stop valves 5 and 6 are used to prevent the backflow of the materials; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected into the sampling bottle In 8, the product was analyzed by LC.

3. There is no residual diphenyl sulfide in the reaction product, the purity of sulfoxide is 98.6%, and the purity of sulfone is 0.3% (LC analysis results). Yield 96%.

Example 5

1. Preparation of raw materials: Weigh 10.0 kg of 2-chloroethyl phenyl sulfide, pour it into a container containing 30.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 14.4 kilograms of 30% hydrogen peroxide (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 2 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains 2-chloroethyl phenyl sulfide enters microchannel reactor 7 by pump 3 in raw material tank 1, the oxidizing agent in raw material tank 2 30% hydrogen peroxide enters microchannel reactor 7 by pump 4; Phenyl phenyl sulfide+30 kilograms of acetic acid: 14.4 kilograms of 30% hydrogen peroxide (this ratio feeding), is mixed reaction under 85 ℃ at the set temperature; seconds, the two streams of materials are mixed and reacted in the reaction module; (4) the backflow of materials is prevented by stop valves 5 and 6 on the reaction channel; (5) after the mixed reaction in microchannel 7, the oxidation product is continuously discharged and collected into In bottle 8, the product was analyzed by LC.

3. The raw material 2-chloroethylbenzene sulfide has no residue in the reaction product, the purity of sulfoxide is 98.0%, and the purity of sulfone is 0.1% (LC analysis result). Yield 93%.

Example 6

1. Raw material preparation: Weigh 10.0 kg of 4-chlorothioanisole, pour it into a container containing 60.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 15.7 kilograms of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 2 device diagram of the present invention, according to following steps: (1) the acetic acid solution that contains 4-chloro-thioanisole enters microchannel reactor 7 by pump 3 in raw material tank 1, the oxygenant 30% in raw material tank 2 Hydrogen peroxide enters microchannel reactor 7 through pump 4; Kilogram acetic acid: 15.7 kilograms of 30% hydrogen peroxide (this ratio feeding), the temperature of setting is 90 ℃ of mixed reactions; (3) control the residence time of reaction material by the flow rate of regulating pump and be 8 seconds, two strands of materials are in Mixed reaction in the reaction module; (4) stop valves 5 and 6 are used to prevent the backflow of materials on the reaction channel; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product passes through LC analysis.

3. The raw material 4-chlorothioanisole in the reaction product has no residue, the purity of sulfoxide is 99.1%, and the purity of sulfone is 0.2% (LC analysis results). Yield 95%.

Example 7

1. Raw material preparation: Weigh 10.0 kg of 2-methoxythioanisole, pour it into a container containing 30.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 16.2 kilograms of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 2 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains 2-methoxyanisole thioanisole enters microchannel reactor 7 by pump 3 in raw material tank 1, the oxidizing agent in raw material tank 2 30% hydrogen peroxide enters microchannel reactor 7 through pump 4; The solution of thioanisole+30.0 kilograms of acetic acid: 16.2 kilograms of 30% hydrogen peroxide (feeding ratio), mixing and reacting at a set temperature of 80°C; (3) controlling the residence time of the reaction materials by adjusting the flow rate of the pump For 6 seconds, the two streams of materials are mixed and reacted in the reaction module; (4) the backflow of the materials is prevented by stop valves 5 and 6 on the reaction channel; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected In the sampling bottle 8, the product is analyzed by LC.

3. The raw material 2-methoxythioanisole in the reaction product has no residue, the purity of sulfoxide is 98.7%, and the purity of sulfone is 0.1% (LC analysis results). Yield 96%.

Example 8

1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 150.0 grams of acetic acid, then add 20.0 grams of concentrated sulfuric acid dropwise to the container at room temperature, and stir Mix well and seal. Then weigh 248.3 grams of hydrogen peroxide with a mass percentage of 50% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device diagram of the present invention, according to following steps: (1) the acetic acid solution that contains 2-(isopropyl sulfide group) nitrobenzene, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3 . The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 2.0 equivalents, and the latter one passes through pump 10, and stop valve 11 enters reactor 7, and consumption is 2.4 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material 2- (isopropylsulfide group) acetic acid solution of nitrobenzene, concentrated sulfuric acid and oxidant according to the above ratio (i.e. 100.0 grams of 2-(isopropylsulfide group) nitrobenzene+150.0 grams of acetic acid solution+10.0 grams of concentrated sulfuric acid: 248.3 grams of 50% hydrogen peroxide (the ratio of feed), through the metering pump into the microchannel reactor 7, mixed reaction at a set temperature of 110 ° C; (3) by adjusting the flow rate of the pump to control the residence time of the reaction material For 10 seconds, the three stocks of materials are mixed and reacted in the reaction module; (4) the backflow of materials is prevented by stop valves 5 and 6 on the reaction channel; (5) after the mixed reaction of the microchannel 7, the oxidation product is continuously discharged and collected In the sampling bottle 8, the product was analyzed by LC.

3. The raw material 2-(isopropylsulfide)nitrobenzene has no residue in the reaction product, the purity of sulfoxide is 0.6%, and the purity of sulfone is 94.7% (LC analysis results). Yield 92%.

Example 9

1. Raw material preparation: Weigh 100.0 g of dimethyl sulfide, pour it into a container containing 300.0 g of acetic acid, then add 10.0 g of concentrated sulfuric acid dropwise into the container at room temperature, stir to mix evenly, and then seal it. Then weigh 394.1 grams of hydrogen peroxide with a mass percentage of 50% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains dimethyl sulfide, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3. The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 2.0 equivalents, and the latter one passes through pump 10, and stop valve 11 enters reactor 7, and consumption is 1.6 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material dimethyl The acetic acid solution of base sulfide and concentrated sulfuric acid and the oxidizing agent are according to the above ratio (i.e. the solution of 100.0 grams of 2-methyl sulfide+300.0 grams of acetic acid+10.0 grams of concentrated sulfuric acid: 394.1 grams of 50% hydrogen peroxide feed), after metering The pump is driven into the microchannel reactor 7, and the set temperature is 100°C for mixed reaction; (3) the residence time of the reaction materials is controlled to be 10 seconds by adjusting the flow rate of the pump, and the three stocks of materials are mixed and reacted in the reaction module; ( 4) Stop valves 5 and 6 are used on the reaction channel to prevent material backflow; (5) After the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by GC.

3. The raw material dimethyl sulfide has no residue in the reaction product, the purity of sulfoxide is 0.4%, and the purity of sulfone is 94.7% (GC analysis result). Yield 94%.

Example 10

1. Raw material preparation: Weigh 100.0 g of diphenyl sulfide, pour it into a container containing 600.0 g of acetic acid, then add 15.0 g of concentrated sulfuric acid dropwise into the container at room temperature, stir to mix evenly, and then seal it. Then weigh 262.9 grams of hydrogen peroxide with a mass percentage of 50% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains diphenyl sulfide, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3. The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 5.0 equivalents, and the latter one passes through pump 10, and stop valve 11 enters reactor 7, and consumption is 2.2 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material diphenyl The acetic acid solution of thioether and concentrated sulfuric acid and the oxidizing agent are according to the above ratio (that is, the solution of 100.0 grams of 2-phenylene sulfide+300.0 grams of acetic acid+15 grams of concentrated sulfuric acid: 262.9 grams of 50% hydrogen peroxide). Squeeze into microchannel reactor 7, and the temperature of setting is 130 ℃ and mixed reaction; (3) control the residence time of reaction material by the flow rate of regulating pump to be 10 seconds, three strands of material are mixed reaction in reaction module; (4 ) on the reaction channel, stop valves 5 and 6 prevent the backflow of materials; (5) after the microchannel 7 mixed reaction, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. There is no residual diphenyl sulfide in the reaction product, the purity of sulfoxide is 0.1%, and the purity of sulfone is 94.3% (LC analysis results). Yield 92%.

Example 11

1. Raw material preparation: Weigh 10.0 kg of 2-chloroethyl phenyl sulfide, pour it into a container containing 30.0 kg of acetic acid, then add 1.0 kg of concentrated sulfuric acid dropwise into the container at room temperature, stir to make it evenly mixed After sealing. Then weigh 28.4 kilograms of 50% hydrogen peroxide (the said mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains 2-chloroethyl phenyl sulfide, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3. The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 5.0 equivalents, and the back one is by pump 10, and stop valve 11 enters reactor 7, and consumption is 2.2 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material 2- The acetic acid solution of chloroethyl phenyl sulfide, concentrated sulfuric acid and the oxidizing agent are according to the above ratio (i.e. the solution of 10.0 kg of 2-chloroethyl phenyl sulfide+30. kg of acetic acid+1.0 kg of concentrated sulfuric acid: the ratio of 28.4 kg of 50% hydrogen peroxide Feed), into the microchannel reactor 7 through the metering pump, mixed reaction at a set temperature of 105 ° C; (3) by adjusting the flow rate of the pump to control the residence time of the reaction materials to be 12 seconds, the three stocks of materials in the reaction Mixing reaction in the module; (4) Stop valves 5 and 6 are used on the reaction channel to prevent the backflow of materials; (5) After the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is passed through the LC analyze.

3. The raw material 2-chloroethylbenzene sulfide has no residue in the reaction product, the purity of sulfoxide is 0.2%, and the purity of sulfone is 95.1% (LC analysis results). Yield 93%.

Example 12

1. Raw material preparation: Weigh 1.0 kg of 4-chlorothioanisole, pour it into a container containing 4.0 kg of acetic acid, then add 0.1 kg of concentrated sulfuric acid dropwise into the container at room temperature, stir to make it evenly mixed and then seal it . Then take 3.1 kilograms of hydrogen peroxide with a mass percentage of 50% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device figure of the present invention, according to following steps: (1) the acetic acid solution that contains 4-chlorothioanisole, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3. The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 5.0 equivalents, and back one is by pump 10, and stop valve 11 enters reactor 7, and consumption is 2.2 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material 4- The acetic acid solution of thiochloroanisole and concentrated sulfuric acid and the oxidizing agent are according to the above ratio (i.e. the solution of 1.0 kilogram of 4-chlorothioanisole+4.0 kilogram of acetic acid+0.1 kilogram of concentrated sulfuric acid: 3.1 kilograms of 50% hydrogen peroxide feed), through The metering pump is driven into the microchannel reactor 7, and the reaction is mixed at a set temperature of 110°C; (3) the residence time of the reaction materials is controlled to be 15 seconds by adjusting the flow rate of the pump, and the three stocks of materials are mixed and reacted in the reaction module; (4) Stop valves 5 and 6 are used to prevent the backflow of materials on the reaction channel; (5) After the microchannel 7 mixed reaction, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. The raw material 4-chlorothioanisole in the reaction product has no residue, the purity of sulfoxide is 0.4%, and the purity of sulfone is 94.7% (LC analysis results). Yield 92%.

Example 13

1. Raw material preparation: Weigh 1.0 kg of 2-methoxythioanisole, pour it into a container containing 10.0 kg of acetic acid, then add 0.1 kg of concentrated sulfuric acid dropwise into the container at room temperature, stir to make it evenly mixed After sealing. Then weigh 3.2 kilograms of 50% hydrogen peroxide (the said mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 3 device diagram of the present invention, according to following steps: (1) the acetic acid solution that contains 2-methoxyanisole, the concentrated sulfuric acid enters microchannel reactor 7 by pump 3 in raw material tank 1. The oxidizing agent mass percentage in the raw material tank 2 is 50% hydrogen peroxide (the described mass percentage refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) and enters the microchannel reactor 7 in 2 shares, and the preceding one passes through the pump 4, Stop valve 6 enters reactor 7, and consumption is 5.0 equivalents, and the back one is by pump 10, and stop valve 11 enters reactor 7, and consumption is 2.2 equivalents; (2) adopt continuous flow microchannel reactor in the reaction process, raw material 2- The acetic acid solution of methoxyanisole, concentrated sulfuric acid and the oxidizing agent are prepared according to the above ratio (i.e. 1.0 kilogram of 2-methoxyanisole + 4.0 kilogram of acetic acid solution + 0.1 kilogram of concentrated sulfuric acid: 3.2 kilograms of 50% hydrogen peroxide). (3) by adjusting the flow of the pump to control the residence time of the reaction materials to be 10 seconds, the three stocks of materials are in the reaction module Internal mixing reaction; (4) stop valves 5 and 6 are used on the reaction channel to prevent material backflow; (5) after the microchannel 7 mixed reaction, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC .

3. There is no residue of the raw material 2-methoxythioanisole in the reaction product, the purity of sulfoxide is 0.5%, and the purity of sulfone is 93.2% (LC analysis results). Yield 92%.

Embodiment 14: the synthesis of omeprazole

1. Raw material preparation: Weigh 1.0 kg of omeprazole precursor thioether, pour it into a container containing 6.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then take 0.76 kilograms of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, in the heart-shaped microchannel that material is special glass, utilize device Fig. 2 of the present invention, according to subordinate steps: (1) the acetic acid solution that contains sulfide enters microchannel reactor 7 by pump 3 in raw material tank 1, raw material Oxidant 30% hydrogen peroxide in tank 2 enters microchannel reactor 7 by pump 4; The solution of the azole precursor thioether+6.0 kilograms of acetic acid: 0.76 kilograms of 30% hydrogen peroxide (the ratio of feed) is injected into the microchannel reactor 7 through a metering pump, and the set temperature is 70° C. Mixed reaction; (3) Control the residence time of the reaction material by the flow of the pump to be 6 seconds, and the two stocks of materials are mixed and reacted in the reaction module; (4) the backflow of the material is prevented by stop valves 5 and 6 on the reaction channel; (5) after passing through the micro After the mixed reaction in channel 7, the oxidation product is continuously discharged and collected into the sampling bottle 8, and the product is analyzed by LC.

3. There is no residue of raw material sulfide in the reaction product, the purity of omeprazole is 99.1%, and the purity of sulfone is 0.1% (LC analysis result). Yield 96%.

Embodiment 15: the synthesis of sulindac precursor

1. Raw material preparation: Weigh 1.0 kg of sulindac precursor thioether, pour it into a container containing 3.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 0.7 kg of 30% hydrogen peroxide (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize device Fig. 2 of the present invention, according to following steps: (1) the acetic acid solution that contains thioether enters microchannel reactor 7 by pump 3 in raw material tank 1, and the oxygenant 30% hydrogen peroxide in raw material tank 2 enters by pump 4 Microchannel reactor 7; (2) adopt continuous flow microchannel reactor in the reaction process, the acetic acid solution of raw material thioether and the oxidizing agent according to above ratio (being the solution of 1.0 kilograms of sulindac precursor thioethers+3.0 kilograms of acetic acid: 0.7 Kilogram 30% hydrogen peroxide (this ratio feeding), is squeezed into microchannel reactor 7 through metering pump, is mixed reaction under 75 ℃ at the set temperature; (3) control the residence time of reaction material by regulating the flow rate of pump 7 seconds, the two stocks of materials are mixed and reacted in the reaction module; (4) on the reaction channel, stop valves 5 and 6 are used to prevent the backflow of materials; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected In the sampling bottle 8, the product was analyzed by LC.

3. The raw material sulfide remains in the reaction product, the purity of the sulfoxide is 99.3%, and there is no sulfone (LC analysis result). Yield 98%.

Embodiment 16: the synthesis of pantoprazole

1. Raw material preparation: Weigh 1.0 kg of pandoprazole precursor thioether, pour it into a container containing 3.0 kg of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 0.64 kg of 30% hydrogen peroxide (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, in the heart-shaped microchannel that material is special glass, utilize device Fig. 2 of the present invention, according to subordinate steps: (1) the acetic acid solution that contains sulfide enters microchannel reactor 7 by pump 3 in raw material tank 1, raw material The oxygenant 30% hydrogen peroxide in tank 2 enters microchannel reactor 7 by pump 4; The solution of bulk thioether+3.0 kilograms of acetic acid: 0.64 kilograms of 30% hydrogen peroxide (this ratio feeding), is squeezed into microchannel reactor 7 through metering pump, is mixed reaction under 70 ℃ at the set temperature; (3) by regulating The flow rate of the pump is used to control the residence time of the reaction material to be 6 seconds, and the two stocks of materials are mixed and reacted in the reaction module; (4) on the reaction channel, stop valves 5 and 6 are used to prevent the backflow of the material; (5) after passing through the microchannel 7 After the mixed reaction, the oxidation product is discharged continuously and collected into the sampling bottle 8, and the product is analyzed by LC.

3. There is no residue of raw material sulfide in the reaction product, the purity of pandoprazole is 99.1%, and the purity of sulfone is 0.1% (LC analysis result). Yield 96%.

Comparative Example 1

1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 300.0 grams of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 126.4 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize device Fig. 2 of the present invention, according to following steps: (1) the acetic acid solution that contains 2-(isopropylsulfide base) nitrobenzene enters microchannel reactor 7 by pump 3 in raw material tank 1, raw material tank 2 The oxidizing agent 30% hydrogen peroxide enters microchannel reactor 7 through pump 4; Ratio (that is the solution of 2-(isopropyl sulfide group) nitrobenzene+300.0 gram acetic acid of 100.0 grams: this ratio feeding of 126.4 grams of 30% hydrogen peroxide), is squeezed into microchannel reactor 7 through metering pump, in setting The fixed temperature is a mixed reaction at 40°C; (3) the residence time of the reaction material is controlled to be 5 seconds by adjusting the flow rate of the pump, and the two stocks are mixed and reacted in the reaction module; (4) the reaction channel passes through the shut-off valve 5 and 6 to prevent the backflow of the material; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8, and the product is analyzed by LC.

3. 90.46% of the raw material 2-(isopropylsulfide)nitrobenzene remains in the reaction product, and the purity of sulfoxide is 7.6% (LC analysis result). Most are unresponsive.

Comparative Example 2

1. Raw material preparation: Weigh 100.0 g of diphenyl sulfide, pour it into a container containing 600.0 g of acetic acid, then add 15.0 g of concentrated sulfuric acid dropwise into the container at room temperature, stir to mix evenly, and then seal it. Then weigh 262.9 grams of hydrogen peroxide with a mass percentage of 50% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

2, utilize Fig. 2 device diagram of the present invention, according to following steps: (1) the acetic acid solution that contains diphenyl sulfide, the concentrated sulfuric acid in the raw material tank 1 enters microchannel reactor 7 by pump 3. The oxidizing agent mass percent in raw material tank 2 is 50% hydrogen peroxide (the said mass percent refers to the percentage that the quality of hydrogen peroxide accounts for the total mass of hydrogen peroxide) by pump 4, shut-off valve 6 enters reactor 7 (2) in the reaction process Adopt continuous flow microchannel reactor, the acetic acid solution of raw material diphenyl sulfide, concentrated sulfuric acid and oxidant according to above ratio (being the solution of 100.0 grams of 2-phenylene sulfide+300.0 grams of acetic acid+15 grams of concentrated sulfuric acid: 262.9 grams 50% The proportion of hydrogen peroxide feed), through the metering pump into the microchannel reactor 7, mixed reaction at a set temperature of 130 ° C; (3) by adjusting the flow rate of the pump to control the residence time of the reaction material is 10 seconds, The three materials are mixed and reacted in the reaction module; (4) the backflow of materials is prevented by stop valves 5 and 6 on the reaction channel; (5) after the mixed reaction in the microchannel 7, the oxidation product is continuously discharged and collected in the sampling bottle 8 , the product was analyzed by LC.

3. The raw material diphenyl sulfide in the reaction product is 28.6%, the purity of sulfoxide is 42.7%, and the purity of sulfone is 25.6% (LC analysis results).

While the invention has been explained in terms of various specific embodiments, it is to be understood that various modifications of the invention will become apparent to those skilled in the art upon reading the specification. It is therefore to be understood that the invention disclosed herein is intended to cover such modifications as come within the scope of the appended claims.

Claims (10)

1. a method for preparing sulfoxide or sulfone, is characterized in that comprising the following steps: the homogeneous solution that thioether 1 and solvent are formed, oxygenant is squeezed in the microchannel reactor through metering pump respectively, contacts in microchannel and Perform an oxidation reaction to obtain sulfoxide or sulfone, and the oxidation reaction time is 1 second to 300 seconds; Wherein, R ₁ and R ₂ are independently substituted or unsubstituted C ₁ -C ₆ alkyl, substituted or unsubstituted C ₅ -C ₁₀ aryl or substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aromatic The "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl The "substituted" mentioned in " means by C ₁ ~ C ₆ alkyl, C ₁ ~ C ₆ alkoxy, nitro, halogen, Substituted with one or more of "halogen-substituted C ₁ -C ₆ alkyl". When there are multiple substituents, the substituents are the same or different. 2. The method for preparing sulfoxide or sulfone according to claim 1, characterized in that: when the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" is substituted by C ₁ -C ₆ alkyl, the "C ₁ -C ₆ "Alkyl" is C ₁ ~ C ₄ alkyl; When the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" When the "substitution" mentioned in is substituted by C ₁ -C ₆ alkoxy, the said "C ₁ -C ₆ alkoxy" is methoxy; When the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" When the "substitution" in is substituted by halogen, the "halogen" is F, Cl, Br or I; When the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" When the "substitution" mentioned in is substituted by "halogen substituted C ₁ -C ₆ alkyl", the said "halogen substituted C ₁ -C ₆ alkyl" is "halogen substituted C ₁ -C ₄ Alkyl", said "halogen" is fluorine, chlorine or bromine. 3. the method for preparing sulfoxide or sulfone as claimed in claim 2, is characterized in that: When the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" When the "substitution" mentioned in is substituted by C ₁ ~C ₄ alkyl, the "C ₁ ~C ₄ alkyl" refers to methyl, ethyl, propyl, isopropyl, n-butyl, Isobutyl or tert-butyl; When the "substituted or unsubstituted C ₁ -C ₆ alkyl", "substituted or unsubstituted C ₅ -C ₁₀ aryl" or "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl" When the "substitution" mentioned in is substituted by "halogen substituted C ₁ -C ₄ alkyl", the said "halogen substituted C ₁ -C ₄ alkyl" is halogen substituted methyl, halogen substituted ethyl radical, halogen-substituted propyl, halogen-substituted isopropyl or halogen-substituted tert-butyl. 4. the method for preparing sulfoxide or sulfone as claimed in claim 1, is characterized in that: When the R ₁ and R ₂ are each independently a substituted or unsubstituted C ₁ -C ₆ alkyl, the "substituted or unsubstituted C ₁ -C ₆ alkyl" is a substituted or unsubstituted C ₁ ~C ₄ alkyl; When the R ₁ and R ₂ are each independently a substituted or unsubstituted C ₅ -C ₁₀ aryl group, the "substituted or unsubstituted C ₅ -C ₁₀ aryl group" is a substituted or unsubstituted C ₅ ~C ₆ aryl; When the R ₁ and R ₂ are each independently a substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl group, the "substituted or unsubstituted C ₄ -C ₁₀ heterocyclic aryl group" is " The heteroatom is a nitrogen or oxygen atom, and a substituted or unsubstituted C ₄ -C ₇ heterocyclic aryl group with 1-3 heteroatoms". 5. The method for preparing sulfoxide or sulfone as claimed in claim 4, characterized in that: when said R ₁ and R ₂ are each independently substituted or unsubstituted C ₁ -C ₄ alkyl, said The "substituted or unsubstituted C ₁ ~ C ₄ alkyl" is substituted or unsubstituted methyl, substituted or unsubstituted ethyl, substituted or unsubstituted propyl, substituted or unsubstituted isopropyl, substituted or unsubstituted n-butyl, substituted or unsubstituted isobutyl, or substituted or unsubstituted tert-butyl; When the R ₁ and R ₂ are each independently a substituted or unsubstituted C ₅ -C ₆ aryl group, the "substituted or unsubstituted C ₅ -C ₆ aryl group" is a substituted or unsubstituted phenyl; When said R ₁ and R ₂ are each independently "a substituted or unsubstituted C ₄ -C ₇ heterocyclic aryl group whose heteroatom is a nitrogen or oxygen atom and the number of heteroatoms is 1-3", said The "heteroatom is nitrogen or oxygen atom, substituted C ₄ ~ C ₇ heterocyclic aryl group with 1-3 heteroatoms" is "substituted or unsubstituted benzimidazolyl" or "substituted or unsubstituted pyridyl". 6. the method for preparing sulfoxide or sulfone as claimed in claim 5, is characterized in that: When said R ₁ and R ₂ are each independently substituted methyl, said "substituted methyl" is trifluoromethyl; When said R ₁ and R ₂ are each independently substituted or unsubstituted phenyl, said "substituted phenyl" is 2-nitrophenyl, 3-nitrophenyl, 4-nitro Phenyl or When said R ₁ and R ₂ are each independently a substituted benzimidazole group, said "substituted benzimidazole group" is or When said R ₁ and R ₂ are each independently substituted pyridyl, said "substituted pyridyl" is or 7. The method for preparing sulfoxide or sulfone according to claim 1, characterized in that: in the method for preparing sulfoxide or sulfone, the size of the microchannel of the microchannel reactor is 10um-1000um. 8. The method for preparing sulfoxide or sulfone as claimed in claim 1, characterized in that: In the method for preparing sulfoxide, the solvent is one or more of alcohol solvents, nitrile solvents, carboxylic acid solvents, halogenated hydrocarbon solvents and water; and / or, In the method for preparing sulfone, the solvent is one or more of carboxylic acid solvents, halogenated hydrocarbon solvents and water; and / or, In the method for preparing sulfoxide or sulfone, the mass ratio of the solvent to thioether 1 is 1:1 to 15:1; and / or, In the method for preparing sulfoxide or sulfone, the oxidizing agent is hydrogen peroxide; and / or, In the method for preparing sulfoxide or sulfone, the molar ratio of the oxidizing agent to thioether 1 is 1:1 to 8:1; and / or, The method for preparing sulfoxide or sulfone is carried out in the presence of a catalyst; and / or, In the method for preparing sulfoxide or sulfone, the oxidant is divided into 1 to 3 feeds, and the homogeneous solution is a single feed; and / or, In the method for preparing sulfoxide or sulfone, the temperature of the oxidation reaction is 40°C-150°C. 9. The method for preparing sulfoxide or sulfone as claimed in claim 8, characterized in that: In the method for preparing sulfoxide, the alcohol solvent is a C ₁ -C ₄ alcohol solvent; the nitrile solvent is acetonitrile; the carboxylic acid solvent is acetic acid; the halogenated hydrocarbon The solvent is a chlorinated hydrocarbon solvent; and / or, In the method for preparing sulfone, the carboxylic acid solvent is acetic acid; the halogenated hydrocarbon solvent is a chlorinated hydrocarbon solvent; and / or, In the method for preparing sulfoxide or sulfone, the mass ratio of the solvent to thioether 1 is 3:1 to 10:1; and / or, In the method for preparing sulfoxide or sulfone, when hydrogen peroxide is used as the oxidizing agent, the mass percentage of the hydrogen peroxide is 27% to 50%, and the mass percentage refers to the mass percentage of hydrogen peroxide in the total mass of hydrogen peroxide percentage; and / or, In the method for preparing sulfoxide or sulfone, the molar ratio of the oxidizing agent to the thioether 1 is 1.5:1-8:1; and / or, In the method for preparing sulfoxide or sulfone, when carried out in the presence of a catalyst, the catalyst is tetraisopropyl titanate, titanium tartrate, sodium tungstate, phosphomolybdic acid, iron acetylacetonate, hydrochloric acid or sulfuric acid; and / or, In the method for preparing sulfoxide or sulfone, when carried out in the presence of a catalyst, the mass ratio of the catalyst to the sulfide 1 is 0 to 0.3, but 0 is not included; and / or, In the method for preparing sulfoxide or sulfone, the temperature of the oxidation reaction is 50°C-130°C. 10. The method for preparing sulfoxide or sulfone as claimed in claim 9, characterized in that: In the reaction for preparing sulfoxide, when the reaction is carried out in the presence of a catalyst, the mass ratio of the catalyst to the sulfide 1 is 0.01-0.1; and / or, In the reaction for preparing sulfoxide, the temperature of the oxidation reaction is 70°C to 100°C; and / or, In the reaction for preparing sulfone, when the reaction is carried out in the presence of a catalyst, the mass ratio of the catalyst to the sulfide 1 is 0.1-0.2; and / or, In the reaction for preparing sulfone, the temperature of the oxidation reaction is 100°C to 130°C; and / or, In the method for preparing sulfoxide or sulfone, the oxidation reaction time is 1 second to 50 seconds.