CN111909062A - Method for preparing methylsulfonyl chloride by adopting microchannel reactor - Google Patents
Method for preparing methylsulfonyl chloride by adopting microchannel reactor Download PDFInfo
- Publication number
- CN111909062A CN111909062A CN201910389689.4A CN201910389689A CN111909062A CN 111909062 A CN111909062 A CN 111909062A CN 201910389689 A CN201910389689 A CN 201910389689A CN 111909062 A CN111909062 A CN 111909062A
- Authority
- CN
- China
- Prior art keywords
- reactor
- chlorine
- reaction
- methylsulfonyl chloride
- dimethyl disulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/16—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by oxidation of thiols, sulfides, hydropolysulfides, or polysulfides with formation of sulfo or halosulfonyl groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for continuously preparing methylsulfonyl chloride by adopting a reactor with a specific structure, belonging to the technical field of fine chemical engineering. The method is a process technology for preparing the methylsulfonyl chloride by continuously oxychlorinating the dimethyl disulfide in a reactor with a specific structure by using the dimethyl disulfide as a raw material, chlorine as a chlorinating agent and hydrochloric acid and methylsulfonyl chloride or chloroform as solvents. The method has the advantages of less sulfur value loss, high product selectivity, mild conditions, short reaction time, high product production efficiency, convenient realization of automation, safe and stable operation and suitability for large-scale production.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a method for preparing methylsulfonyl chloride by adopting a microchannel reactor.
Background
Methylsulfonyl chloride is an important intermediate of medicines, pesticides and fine chemicals, and the downstream product methylsulfonic acid is an emerging important electroplating solution in the electroplating industry.
The equation for preparing methylsulfonyl chloride from dimethyl disulfide is as follows:
side reactions of hydrolysis
Side reaction of main impurities
The reaction is a strong exothermic system, the exothermic quantity of each mol of reaction is about 651kJ, and 8mol of hydrogen chloride is discharged; the suitable temperature of the industrial batch kettle type reaction is 20-30 ℃; the raw material dimethyl disulfide and the product methylsulfonyl chloride are insoluble in hydrochloric acid, so the system is a liquid-gas three-phase reaction system. Therefore, the batch kettle reaction has the following obvious disadvantages:
the heat transfer area of the material per unit volume is small, and is below 2.5M2/M3, so that the chlorine introducing speed is slow, the reaction process is long, and one batch of reaction takes 20-25 hr. So that the productivity is low and the hydrolysis ratio of the product methylsulfonyl chloride is high.
10000 tons of methane sulfonyl chloride produced annually can be produced, more than 20 reactors are needed for a single reaction kettle, and the floor area of equipment is at least 3000M2 by adding supporting facilities.
The online liquid holdup of the reaction equipment is large, 10000 tons of methylsulfonyl chloride capacity are produced annually, and the online liquid holdup is up to 60M 3. Dimethyl disulfide is flammable and explosive, and the product methylsulfonyl chloride is extremely toxic. Such a large liquid hold-up has a great potential safety hazard.
The temperature control needs very low temperature of the heat exchange medium to make up for the defect caused by insufficient heat exchange area, so that the refrigeration efficiency is very low, and high power consumption is brought. The difficulty in controlling the temperature, the easiness in hydrolysis of methylsulfonyl chloride, and the large amount of chloromethylsulfonyl chloride impurity.
The kettle type reaction has poor mass transfer efficiency to liquid-gas three-phase reaction, so that chlorine cannot be completely utilized, and dimethyl disulfide cannot be completely reacted, thereby causing the phenomenon that the chlorine and the dimethyl disulfide in tail gas are remained.
Patent No. CN02123805 discloses a method for producing high-purity methylsulfonyl chloride by a batch process, which has the disadvantages of complicated process, complicated equipment and high labor intensity although the disadvantages are reduced to a certain extent by adopting a plurality of driving protection measures.
Previous continuous processes have been studied more and more, such as JP 2003342252, DE1811768, US3600136 granted in 1971, US3993692 granted in 1976, and EP675106 granted in 1995, which have not solved the disadvantages of the tank reaction well and have problems in practical application, and have not been reported to be applied industrially.
In patent CN201410020731 (application number), a method for producing high-purity methylsulfonyl chloride by using a membrane lift reactor continuous method is disclosed. Although the device has considerable improvement compared with the prior reaction mode, the device solves the prior problems to a considerable extent and has considerable advantages. But the stability is poor, the start and the stop are inconvenient, considerable time is needed from the start to the system stabilization, and a lot of intermediate materials are generated. The tiny factor change has great influence on the system stability, occasionally generates the phenomenon of pulse fluctuation and has great damage to equipment.
Therefore, we improved this and proposed a process for preparing methanesulfonyl chloride using a microchannel reactor.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for preparing methylsulfonyl chloride by adopting a microchannel reactor.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a method for preparing methylsulfonyl chloride by adopting a microchannel reactor, which comprises the following steps:
s1, using dimethyl disulfide as a substrate, chloroform as a solvent for dissolving the dimethyl disulfide, hydrochloric acid as a source of the solvent and water required by the reaction, and chlorine or liquid chlorine as an oxidant, and continuously oxidizing in a microchannel continuous flow reactor with different structures to prepare methylsulfonyl chloride;
s2, continuously pumping hydrochloric acid into a micro-channel reactor module through a metering pump at a certain temperature, continuously pumping chlorine or liquid chlorine, fully mixing the chlorine or liquid chlorine with the hydrochloric acid in a reactor, continuously pumping the chloroform solution of dimethyl disulfide into the reactor through the metering pump for reaction, and controlling the reaction temperature through an external circulation heat exchange system;
s3, controlling the feeding ratio by a method of feeding through a flow meter and a metering pump, and controlling the residence time of the material mixing reaction by controlling the flow rate and changing the length of a microchannel of the microchannel reactor module;
s4, after the reaction is finished, the material flows out from the end of the reactor, gas-liquid separation is carried out, the gas is washed and absorbed, hydrochloric acid is generated as a byproduct, the liquid is extracted by chloroform, the solvent is recovered by concentration and is rectified to obtain a finished product, the solvent is used indiscriminately, or the liquid is directly layered, the oil layer is rectified to obtain a product of methylsulfonyl chloride, and the water phase is used as hydrochloric acid and is used indiscriminately and returned to the reaction system.
In a preferred embodiment of the present invention, the oxidant in step S1 is chlorine, and the molar ratio of chlorine to dimethyl disulfide is 1.0-2:1, preferably 1.0-1.1: 1.
In a preferred embodiment of the present invention, the pressure of the feed inlet of the chlorine gas or liquid chlorine into the reactor in step S2 is 1-15bar, preferably 5-10 bar.
As a preferred technical solution of the present invention, the chloroform in step S1 is a solvent for dissolving dimethyl disulfide, the solvent for dissolving substrate dimethyl disulfide is one or more of chloroform, dichloroethane, dichloromethane, carbon tetrachloride, chlorobenzene, and methylsulfonyl chloride, and the mass ratio of the chloroform or methylsulfonyl chloride solvent to dimethyl disulfide is preferably 0-5:1, and preferably 0.5-2: 1.
In a preferred embodiment of the present invention, the concentration of the hydrochloric acid in step S1 is 0-40%, preferably 30-40%, and the mass ratio of the hydrochloric acid to the substrate dimethyl disulfide is 1-20:1, preferably 2-5: 1.
As a preferred technical scheme of the invention, the reaction temperature in the step S2 is 0-100 ℃, preferably 0-60 ℃, and more preferably 10-50 ℃.
As a preferred technical scheme of the invention, the reaction residence time of the step S3 is 0.1-30S, and the preferred residence time is 3-10S.
As a preferred technical scheme of the invention, the reaction solution obtained by gas-liquid separation in step S4 is subjected to solvent extraction, the extract is concentrated and rectified to obtain a product, or the liquid obtained by gas-liquid separation of the reactant is directly separated into an oil layer, and the oil layer is rectified to obtain a product, wherein the extraction solvent can be one or more of chloroform, dichloromethane, dichloroethane, carbon tetrachloride and chlorobenzene.
In a preferred embodiment of the present invention, the chlorine gas or the liquid chlorine in step S1 is first mixed with hydrochloric acid and then reacted with the dimethyl disulfide solution.
As a preferred technical scheme of the invention, all the reaction processes in the steps S1-S3 are continuously carried out in a microchannel reactor module with a specific structure, the microchannel reactor module is divided into a mass transfer enhancement type structure and a straight channel structure, wherein the mass transfer enhancement type module microstructure comprises a diamond structure, a heart-shaped structure, a triangular structure and a circular structure, and the straight channel module microstructure comprises a cylindrical structure and a rectangular structure.
The invention has the beneficial effects that:
1. the unit volume heat exchange area of the adopted microchannel equipment is 2500M2/M3 which is 1000 times of that of the kettle type equipment, and the mass transfer coefficient is 1000 times of that of the kettle type equipment.
2. The reaction time is short, only 3-10S, the productivity is high, and the production efficiency is high. The hydrolysis rate of the methylsulfonyl chloride is low and is less than 0.5 percent.
3. The occupied area of the equipment is small, 10000 tons of methylsulfonyl chloride can be produced annually, only the occupied area of a reaction area which is less than 30M2 is needed, and the post-treatment equipment and the post-treatment process are simple due to thorough reaction.
4. The liquid holdup is small, 10000 tons of methylsulfonyl chloride can be produced annually, and the liquid holdup of a reaction system is only less than 500L and less than one percent of the traditional kettle-type liquid holdup.
5. The reaction system is convenient for realizing automatic control, ensures that the safety production is essentially guaranteed, ensures that the product quality is stable, has low labor cost, ensures that the heat exchange medium only needs to have the same temperature with the reaction temperature almost, and has high heat exchange efficiency and low power consumption.
6. The reaction conversion is thorough, the dimethyl disulfide and the chlorine are well utilized, and the dimethyl disulfide and the chlorine in the by-product hydrochloric acid are both reduced to extremely low limit values; the selectivity is good, the hydrolysis reaction and the side reaction of chloromethyl sulfonyl chloride are effectively inhibited, and the method has obvious advantages in economy and essential environmental protection.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic process flow diagram of a process for preparing methanesulfonyl chloride using a microchannel reactor according to the present invention;
FIG. 2 is a schematic diagram of the structure of a continuous flow tubular reactor apparatus used in a process for preparing methanesulfonyl chloride using a microchannel reactor according to the present invention;
FIG. 3 is a schematic diagram of a module configuration of a continuous flow microchannel reactor for a process of producing methanesulfonyl chloride using a microchannel reactor according to the present invention;
FIG. 4 is a schematic diagram of the micro-structural structures of the microchannel module mass transfer enhancement type and the straight channel of the method for preparing methylsulfonyl chloride by using the microchannel reactor.
In the figure: 1. a hydrochloric acid solution feed tank; 2. a chlorine gas vaporizer; 3. a hydrochloric acid solution metering pump; 4. a dimethyl disulfide solution feed tank; 5. a metering pump of dimethyl disulfide solution; 6. a pre-mixing zone; 7. a reaction zone; 8. a cooling zone; 9. a product collection zone; 10. and a tail gas liquid caustic soda absorption area.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example (b): as shown in fig. 1, fig. 2, fig. 3 and fig. 4, the method for preparing methylsulfonyl chloride by using a microchannel reactor comprises the following steps:
s1, using dimethyl disulfide as a substrate, chloroform as a solvent for dissolving the dimethyl disulfide, hydrochloric acid as a source of the solvent and water required by the reaction, and chlorine or liquid chlorine as an oxidant, and continuously oxidizing in a microchannel continuous flow reactor with different structures to prepare methylsulfonyl chloride;
s2, continuously pumping hydrochloric acid into a micro-channel reactor module through a metering pump at a certain temperature, continuously pumping chlorine or liquid chlorine, fully mixing the chlorine or liquid chlorine with the hydrochloric acid in a reactor, continuously pumping the chloroform solution of dimethyl disulfide into the reactor through the metering pump for reaction, and controlling the reaction temperature through an external circulation heat exchange system;
s3, controlling the feeding ratio by a method of feeding through a flow meter and a metering pump, and controlling the residence time of the material mixing reaction by controlling the flow rate and changing the length of a microchannel of the microchannel reactor module;
s4, after the reaction is finished, the material flows out from the end of the reactor, gas-liquid separation is carried out, the gas is washed and absorbed, hydrochloric acid is generated as a byproduct, the liquid is extracted by chloroform, the solvent is recovered by concentration and is rectified to obtain a finished product, the solvent is used indiscriminately, or the liquid is directly layered, the oil layer is rectified to obtain a product of methylsulfonyl chloride, and the water phase is used as hydrochloric acid and is used indiscriminately and returned to the reaction system.
Wherein, the oxidant in step S1 is chlorine, and the molar ratio of chlorine to dimethyl disulfide is 1.0-2:1, preferably 1.0-1.1: 1.
Wherein the pressure of the chlorine gas or the liquid chlorine entering the feed inlet of the reactor in the step S2 is 1-15bar, preferably 5-10 bar.
In step S1, the chloroform is a solvent for dissolving dimethyl disulfide, the solvent for dissolving substrate dimethyl disulfide is one or more of chloroform, dichloroethane, dichloromethane, carbon tetrachloride, chlorobenzene, and methylsulfonyl chloride, and the mass ratio of chloroform or methylsulfonyl chloride solvent to dimethyl disulfide is preferably 0-5:1, and more preferably 0.5-2: 1.
Wherein, the concentration of the hydrochloric acid in the step S1 is 0-40%, preferably 30-40%, and the mass ratio of the hydrochloric acid to the substrate dimethyl disulfide is 1-20:1, preferably 2-5: 1.
Wherein, the reaction temperature in the step S2 is 0-100 ℃, preferably 0-60 ℃, and more preferably 10-50 ℃.
Wherein, the reaction residence time of the step S3 is 0.1-30S, and the preferred residence time is 3-10S.
Wherein, the liquid obtained by gas-liquid separation of the reaction liquid in the step S4 is extracted by a solvent, the extract liquid is concentrated and rectified to obtain a product, or the liquid obtained by gas-liquid separation of the reactant is directly separated into an oil layer, and the oil layer is rectified to obtain a product, and the extraction solvent can be one or more of chloroform, dichloromethane, dichloroethane, carbon tetrachloride and chlorobenzene.
Wherein, the chlorine gas or the liquid chlorine is firstly mixed with the hydrochloric acid and then reacts with the dimethyl disulfide solution in the step S1.
All the reaction processes in the steps S1-S3 are continuously carried out in a microchannel reactor module with a specific structure, the microchannel reactor module is divided into a mass transfer enhancement type structure and a straight channel structure, the mass transfer enhancement type module microstructure comprises a diamond structure, a heart-shaped structure, a triangular structure and a circular structure, and the straight channel module microstructure comprises a cylindrical structure and a rectangular structure.
The working principle is as follows:
the invention adopts a micro-channel reactor, and the micro-channel continuous flow reactor is a new generation reactor which is newly developed in recent years and is gradually applied to production, and has excellent heat transfer, mass transfer and mixing performances. For a liquid-gas three-phase strong heat release system prepared from methylsulfonyl chloride, the microchannel reactor is most suitable, the problems of mixing, mass transfer and heat transfer of various reactors in the prior art can be solved, and the microchannel reactor is well applied to the process for preparing the methylsulfonyl chloride from the dimethyl disulfide.
The specific embodiment is as follows:
example 1
(1) Referring to fig. 2, the connection mode of the tubular reactor is determined, the type of the micro-channel is (3b +3b +3a) enhanced channel structure module + direct-current channel module, and the heat exchange medium is high-temperature and low-temperature heat conduction oil.
(2) 5000g of dimethyl disulfide is dissolved by 5000g of chloroform, a mixed solution enters a reactor at the flow rate of 8g/min, 36% hydrochloric acid enters the reactor at the flow rate of 8g/min, chlorine enters at the flow rate of 560ml/min, the pressure of a chlorine inlet is 8.5bar, the reaction temperature is 40 ℃, the temperature is reduced to 10 ℃, the mixed solution enters a receiving zone, the continuous operation is carried out for 10 hours, gas-liquid separation is carried out, a receiving solution is subjected to layering, a water layer is extracted by chloroform, extract liquor is combined, concentrated and rectified, a product of 5700g is obtained, the purity is 99.8%, the product in the recovered chloroform is analyzed to contain about 80g of the product, so 5780g of methylsulfonyl chloride is obtained in total, the yield is 99%, about 0.5% of the yield is analyzed to be lost in the rectification process, about 0.2% of the yield is hydrolyzed into methylsulfonic acid, about 0.1% of the yield is lost.
The liquid holdup of the reactor system is about 200ml, the residence time is about 3s, and the occupied area of the reaction system is less than 0.4M 2.
The reactor was scaled up to produce about 4.16 tons of methanesulfonyl chloride annually, calculated as 7200hr of annual operation.
Example 2
(1) Referring to fig. 2, the connection mode of the tubular reactor is determined, the type of the micro-channel is (3a +3b +3a) direct-flow channel module + enhanced channel structure module + direct-flow channel module, and the heat exchange medium is high-low temperature heat conduction oil.
(2) 5000g of dimethyl disulfide is dissolved by 10000g of chloroform, a mixed solution enters a reactor at the flow rate of 9g/min, 36% hydrochloric acid enters the reactor at the flow rate of 15g/min, chlorine enters at the flow rate of 460ml/min, the pressure of a chlorine feeding hole is 8.5bar, the reaction temperature is 15 ℃, the temperature is reduced to 10 ℃, the mixed solution enters a receiving area, the continuous operation is carried out for 10 hours, gas-liquid separation is carried out, the receiving solution is layered, a water layer is extracted by chloroform, extract liquor is combined, concentrated and rectified, 4230g of a product with the purity of 99.8% is obtained, and the product in the chloroform is analyzed and recovered to contain about 70g of the product, so 4300g of methylsulfonyl chloride is obtained in total. About 0.5% of the yield was analyzed to be lost in the rectification, about 0.3% of the yield was hydrolyzed to methanesulfonic acid, about 0.9% of the yield was generated as chloromethylsulfonyl chloride, about 0.1% of the yield was lost in the hydrogen chloride byproduct, and about 50ppm of dimethyl disulfide was present in the hydrogen chloride byproduct.
The liquid holdup of the reactor system is about 200ml, the residence time is about 4s, and the occupied area of the reaction system is less than 0.4M 2.
The reactor was scaled up to produce about 3.1 tons of methanesulfonyl chloride annually, calculated as 7200hr of annual operation.
In summary, the following steps: the invention thoroughly solves the problems of uneven mixing, insufficient reaction of raw materials, high residue of oxidizable substances in the product sulfonyl chloride, serious loss of sulfur value in byproduct hydrogen chloride and the like in the existing production method; and the problems of difficult removal of reaction heat, high reaction temperature, more side reactions and poor selectivity caused by external cooling of the reactor are also solved. And the micro-channel reactor adopted by the invention has small liquid holdup of the system, high safety and good stability compared with a climbing film reaction. And because of good mixed mass transfer effect, the utilization rate of the chlorine is greatly improved, the chlorine can be equivalently fed, and residual chlorine and residual reduced sulfur in the reaction tail gas can be effectively controlled at the same time.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing methylsulfonyl chloride by adopting a microchannel reactor is characterized by comprising the following steps:
s1, using dimethyl disulfide as a substrate, chloroform as a solvent for dissolving the dimethyl disulfide, hydrochloric acid as a source of the solvent and water required by the reaction, and chlorine or liquid chlorine as an oxidant, and continuously oxidizing in a microchannel continuous flow reactor with different structures to prepare methylsulfonyl chloride;
s2, continuously pumping hydrochloric acid into a micro-channel reactor module through a metering pump at a certain temperature, continuously pumping chlorine or liquid chlorine, fully mixing the chlorine or liquid chlorine with the hydrochloric acid in a reactor, continuously pumping the chloroform solution of dimethyl disulfide into the reactor through the metering pump for reaction, and controlling the reaction temperature through an external circulation heat exchange system;
s3, controlling the feeding ratio by a method of feeding through a flow meter and a metering pump, and controlling the residence time of the material mixing reaction by controlling the flow rate and changing the length of a microchannel of the microchannel reactor module;
s4, after the reaction is finished, the material flows out from the end of the reactor, gas-liquid separation is carried out, the gas is washed and absorbed, hydrochloric acid is generated as a byproduct, the liquid is extracted by chloroform, the solvent is recovered by concentration and is rectified to obtain a finished product, the solvent is used indiscriminately, or the liquid is directly layered, the oil layer is rectified to obtain a product of methylsulfonyl chloride, and the water phase is used as hydrochloric acid and is used indiscriminately and returned to the reaction system.
2. The method of claim 1, wherein the oxidant in step S1 is chlorine gas, and the molar ratio of chlorine gas to dimethyl disulfide is 1.0-2:1, preferably 1.0-1.1: 1.
3. The method for preparing methylsulfonyl chloride with a microchannel reactor as set forth in claim 1, wherein the pressure of the feed port of the chlorine gas or liquid chlorine into the reactor in step S2 is 1-15bar, preferably 5-10 bar.
4. The method for preparing methylsulfonyl chloride with a microchannel reactor according to claim 1, wherein the chloroform in step S1 is a solvent for dissolving dimethyl disulfide, the solvent for dissolving substrate dimethyl disulfide is one or more of chloroform, dichloroethane, dichloromethane, carbon tetrachloride, chlorobenzene, and methylsulfonyl chloride, and the mass ratio of chloroform or methylsulfonyl chloride solvent to dimethyl disulfide is preferably 0-5:1, and more preferably 0.5-2: 1.
5. The method for preparing methylsulfonyl chloride using a microchannel reactor as claimed in claim 1, wherein the concentration of the hydrochloric acid in step S1 is 0-40%, preferably 30-40%, and the mass ratio of the hydrochloric acid to the substrate dimethyl disulfide is 1-20:1, preferably 2-5: 1.
6. The method for preparing methanesulfonyl chloride using a microchannel reactor as claimed in claim 1, wherein the reaction temperature in step S2 is 0-100 ℃, preferably 0-60 ℃, and more preferably 10-50 ℃.
7. The method for preparing methanesulfonyl chloride using a microchannel reactor as claimed in claim 1, wherein the reaction residence time in step S3 is 0.1-30S, preferably 3-10S.
8. The method of claim 1, wherein the liquid obtained by the gas-liquid separation of the reaction solution in step S4 is extracted with a solvent, the extract is concentrated and distilled to obtain a product, or the liquid obtained by the gas-liquid separation of the reactant is directly separated from an oil layer, and the oil layer is distilled to obtain a product, wherein the extraction solvent is one or more selected from chloroform, dichloromethane, dichloroethane, carbon tetrachloride and chlorobenzene.
9. The method of claim 1, wherein the chlorine gas or the liquid chlorine is mixed with hydrochloric acid and then reacted with the dimethyl disulfide solution in step S1.
10. The method of claim 1, wherein the whole reaction process of steps S1-S3 is continuously performed in a microchannel reactor module having a specific structure, the microchannel reactor module is divided into a mass transfer enhancement type structure and a straight channel structure, the mass transfer enhancement type module microstructure includes a diamond structure, a heart-shaped structure, a triangular structure and a circular structure, and the straight channel module microstructure includes a cylindrical structure and a rectangular structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910389689.4A CN111909062A (en) | 2019-05-10 | 2019-05-10 | Method for preparing methylsulfonyl chloride by adopting microchannel reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910389689.4A CN111909062A (en) | 2019-05-10 | 2019-05-10 | Method for preparing methylsulfonyl chloride by adopting microchannel reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111909062A true CN111909062A (en) | 2020-11-10 |
Family
ID=73242201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910389689.4A Pending CN111909062A (en) | 2019-05-10 | 2019-05-10 | Method for preparing methylsulfonyl chloride by adopting microchannel reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111909062A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594617A (en) * | 2022-07-29 | 2023-01-13 | 苏州翔实医药发展有限公司（Cn） | Synthesis method of difluoromethylsulfonyl chloride |
| CN115724727A (en) * | 2022-11-24 | 2023-03-03 | 河北工业职业技术学院 | Method for preparing cyazofamid intermediate 2,2-dichloro-4' -methylacetophenone |
| CN117024370A (en) * | 2023-08-24 | 2023-11-10 | 天津北方食品有限公司 | Microchannel reaction process for oxidation chlorination in saccharin production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112110A (en) * | 1994-03-31 | 1995-11-22 | 北美埃尔夫爱托化学股份有限公司 | Pressurized production of alkanesulfonyl chloride and alkanesulfonic acide |
| CN1465564A (en) * | 2002-07-04 | 2004-01-07 | 河北亚诺化工有限公司 | Interrupter method for producing high-purity methyl sulfonyl chloride |
| CN106117128A (en) * | 2016-06-26 | 2016-11-16 | 江苏扬农化工集团有限公司 | A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously |
| CN107488107A (en) * | 2016-06-12 | 2017-12-19 | 上海泰禾国际贸易有限公司 | A kind of method that phenols chlorination is carried out in the continuous flow reactor of microchannel |
-
2019
- 2019-05-10 CN CN201910389689.4A patent/CN111909062A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112110A (en) * | 1994-03-31 | 1995-11-22 | 北美埃尔夫爱托化学股份有限公司 | Pressurized production of alkanesulfonyl chloride and alkanesulfonic acide |
| CN1465564A (en) * | 2002-07-04 | 2004-01-07 | 河北亚诺化工有限公司 | Interrupter method for producing high-purity methyl sulfonyl chloride |
| CN107488107A (en) * | 2016-06-12 | 2017-12-19 | 上海泰禾国际贸易有限公司 | A kind of method that phenols chlorination is carried out in the continuous flow reactor of microchannel |
| CN106117128A (en) * | 2016-06-26 | 2016-11-16 | 江苏扬农化工集团有限公司 | A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594617A (en) * | 2022-07-29 | 2023-01-13 | 苏州翔实医药发展有限公司（Cn） | Synthesis method of difluoromethylsulfonyl chloride |
| CN115594617B (en) * | 2022-07-29 | 2024-02-06 | 苏州翔实医药发展有限公司 | Synthesis method of difluoromethyl sulfonyl chloride |
| CN115724727A (en) * | 2022-11-24 | 2023-03-03 | 河北工业职业技术学院 | Method for preparing cyazofamid intermediate 2,2-dichloro-4' -methylacetophenone |
| CN117024370A (en) * | 2023-08-24 | 2023-11-10 | 天津北方食品有限公司 | Microchannel reaction process for oxidation chlorination in saccharin production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111909062A (en) | Method for preparing methylsulfonyl chloride by adopting microchannel reactor | |
| CN109134231B (en) | Device and process for continuously producing chloroacetic acid by differential circulation | |
| CN108250176A (en) | A kind of quick continuous flow synthesis technology of fluorinated ethylene carbonate | |
| US2871097A (en) | Production of chlorine dioxide | |
| CN101921215A (en) | Method for producing 2-nitro-p-methylsullfonyl benzoic acid | |
| CN103724315A (en) | Method used for synthesizing cyclic carbonate in enhanced microreactor system | |
| CN106430129A (en) | Preparation method for difluorosulfonylimide salt | |
| CN112919504B (en) | Method and device for synthesizing lithium hexafluorophosphate by adopting continuous flow reactor | |
| CN112897488A (en) | Method for preparing bis (fluorosulfonyl) imide by using microchannel reactor | |
| CN106349126A (en) | Method for preparing 4,4'-dichloro sulfobenzide | |
| CN109701470B (en) | Tower type micro reaction device for continuously synthesizing 2-mercaptobenzothiazole | |
| US2863722A (en) | Chlorine dioxide production | |
| CN111517931A (en) | Method for synthesizing 2, 4-difluorobenzaldehyde by using microchannel reactor | |
| CN109836334B (en) | Method for continuously preparing cyclopropylamine | |
| CN103153847A (en) | Method for producing phosphorus pentafluoride | |
| US20240174628A1 (en) | Method for continuously preparing crude ethylene sulfate | |
| CN111039829B (en) | Method for producing p-acetamido benzene sulfonyl chloride by two-temperature zone two-stage method based on continuous flow reaction | |
| WO2018113628A1 (en) | Rapid continuous-flow synthesis process for fluoroethylene carbonate. | |
| CN108586296A (en) | A kind of method for continuously synthesizing of sodium p-nitrotoluene-2-sulfonic acid | |
| CN111116424B (en) | Method for preparing trifluoromethanesulfonic acid by continuous hydrolysis | |
| CN216236054U (en) | Lithium hexafluorophosphate continuous method synthesis system | |
| CN106966894B (en) | A kind of method of the pipe type continuously production chloro- 5- fluorobenzoyl chloride of 2,4- bis- | |
| JPH11255503A (en) | Production of aqueous solution of sodium hypochlorite having low common salt content | |
| CN109400506A (en) | A kind of synthetic method of high-purity chlorosulphonyl isocyanate | |
| CN114713164A (en) | Dibenzothiazole disulfide micro-reaction continuous synthesis system and synthesis method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |