A method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed
By carrying out continuous reactions of trifluoromethylsulfur chloride, chlorine and water in a fixed bed reactor, the problems of strict refrigeration requirements and low product yield in the prior art are solved, and the preparation of trifluoromethylsulfonyl chloride with high purity and high yield is achieved.
Patent Information
- Application Number
- CN202411479512.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2044-10-23
AI Technical Summary
The existing preparation methods of trifluoromethylsulfonyl chloride have problems such as strict refrigeration requirements and low product yields.
The method of synthesizing trifluoromethylsulfonyl chloride by continuous chlorination and oxidation of fixed beds is adopted. The reaction is carried out in a fixed bed reactor with few side reactions, high product purity, and yields above 90%.
The preparation of trifluoromethylsulfonyl chloride with high purity and high yield is achieved, simplifying the reaction process and reducing the refrigeration demand.
Abstract
Description
Technical Field
[0001] The invention relates to a method for synthesizing trifluoromethylsulfonyl chloride, in particular to a method for synthesizing trifluoromethylsulfonyl chloride through continuous chlorination and oxidation in a fixed bed. Background Art
[0002] Trifluoromethylsulfonyl chloride is a widely used pharmaceutical and electrolyte synthesis intermediate. It is an important synthetic raw material for many antibacterial drugs, weight loss drugs, anticancer drugs and adjuvants.
[0003] At present, the preparation of trifluoromethanesulfonyl chloride mainly includes: CN117720441A discloses a method for continuously preparing trifluoromethanesulfonyl chloride. The equipment used in this patent is a continuous flow microchannel reactor. The reaction raw materials are sulfonyl fluoride, trifluoromethane and diazabicyclic. This method requires the mixing temperature and reaction temperature to be between -30 and -10 ° C, and has strict requirements on refrigeration. CN115724774A discloses a method for preparing trifluoromethanesulfonyl chloride. This patent is a one-pot method for preparing trifluoromethanesulfonyl chloride. The preparation method is to use trifluoromethane to react with sulfonyl chloride in a solution under alkaline conditions to prepare the target product. The product yield of this method is low, only about 70%. Summary of the invention
[0004] In view of the shortcomings of the prior art, the present invention provides a method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination and oxidation in a fixed bed. The reaction is carried out in a fixed bed reactor, with few side reactions, high product purity and high yield, which is above 90%.
[0005] The present invention is achieved through the following technical solutions:
[0006] The invention provides a method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed. Trifluoromethylsulfonyl chloride, chlorine and water are continuously reacted under the action of a catalyst to generate trifluoromethylsulfonyl chloride.
[0007] The reaction formula is:
[0008] .
[0009] In the above method, the reaction is carried out in a fixed bed reactor, which can be a commonly used axial, radial, or tubular reactor.
[0010] Preferably, the material enters the fixed bed reactor in gaseous form. The gaseous material fully contacts the solid catalyst, increasing the material contact area and improving the reaction rate.
[0011] In the above method, the catalyst is activated carbon, resin, molecular sieve, etc., preferably activated carbon. The catalyst can catalyze the chlorination of trifluoromethylsulfonyl chloride to obtain trifluoromethylsulfonyl chloride.
[0012] In the above method, the molar ratio of trifluoromethyl sulfhydryl chloride, chlorine gas and water is 1:1-10:1-10, preferably 1:1.5-5:1.5-5, and more preferably 1:2.4:2.3.
[0013] In the above method, the reaction temperature is 20-150°C, preferably 50-120°C, more preferably 80-120°C, and most preferably 100-120°C; the present invention can achieve a good yield at a temperature of 100-120°C.
[0014] Space velocity: Space velocity refers to the amount of gas treated by a catalyst per unit volume per unit time under specified conditions, and the unit is m 3 / (m 3 catalyst·h), which can be simplified to h -1 The airspeed can be selected from 10 to 1000 h -1 , preferably 100~500 h -1 The catalyst is heated at a space velocity of 100-500 h -1 The catalytic efficiency is higher.
[0015] In the above method, the specific reaction includes the following steps: trifluoromethylsulfonyl chloride, chlorine gas and water are introduced into a fixed bed reactor containing a catalyst, and heated to react to obtain trifluoromethylsulfonyl chloride.
[0016] In the above method, the product obtained by the reaction is discharged from the top of the reactor, and the hydrogen chloride is absorbed by the hydrogen chloride absorption device, and the remaining product is condensed to obtain trifluoromethylsulfonyl chloride. The hydrogen chloride absorbed by the hydrogen chloride absorption device can be recycled and reused, and no waste water is generated, which is beneficial to environmental protection.
[0017] Preferably, the hydrogen chloride absorption temperature is 40-60° C. At this temperature, hydrogen chloride can be effectively recovered.
[0018] Preferably, the condensation temperature is 0° C. Excess chlorine gas enters the chlorine gas absorption device for absorption, and liquid alkali absorption can be selected.
[0019] Compared with the prior art, the present invention has the following advantages:
[0020] 1. The present invention uses trifluoromethylsulfonyl chloride, chlorine and water as raw materials to synthesize trifluoromethylsulfonyl chloride in one step, and the reaction process is simple and easy to control.
[0021] 2. The present invention carries out catalytic reaction in a fixed bed, has few side reactions, and trifluoromethanesulfonyl chloride synthesized by the fixed bed reactor is continuously collected from the reaction outlet, with a product yield of more than 90%. DETAILED DESCRIPTION
[0022] The present invention is further described below by specific examples, which are exemplary only and are not intended to limit the content. In the following examples, unless otherwise specified, all reagents used can be purchased from the market. In the following examples, the terms not described in detail have the meanings reported in the prior art, and the operations and methods not described in detail can all refer to the operations of the prior art. The specifications of the fixed beds selected in the following examples are the same.
[0023] The treatment method of activated carbon is as follows: the activated carbon is columnar activated carbon with a diameter of 2.5mm, and is pretreated to remove the metal ions therein. The method is to soak it in dilute hydrochloric acid for 6 hours, then replace it with deionized water to neutrality, and then dry it for use.
[0024] Molecular sieve catalyst: Any molecular sieve catalyst that can achieve catalytic reaction can be used. H-type molecular sieve is preferred. Titanium-silicon-aluminum molecular sieve can also be selected, selected from at least one of titanium-silicon-aluminum molecular sieve with MFI structure, titanium-silicon-aluminum molecular sieve with MEL structure, titanium-silicon-aluminum molecular sieve with BEA structure, titanium-silicon-aluminum molecular sieve with MWW structure, titanium-silicon-aluminum molecular sieve with MOR structure, titanium-silicon-aluminum molecular sieve with TUN structure and titanium-silicon-aluminum molecular sieve with two-dimensional hexagonal structure.
[0025] Resin catalyst: also called polymer porous microspheres, any porous microspheres that can achieve catalytic reactions can be used.
[0026] .
[0027] Example 1
[0028] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 10 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed in gaseous form for reaction. The reaction product passes through the bed and exits from the top of the reactor, entering the hydrogen chloride absorption device, the hydrogen chloride absorption temperature is set at 50°C, the product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption, and the product trifluoromethylsulfonyl chloride is obtained. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 73.73 grams of product, the GC detection content is 99.21%, and the yield is 91.76%.
[0029] Example 2
[0030] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 100 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 732 grams of product, the GC detection content is 99.30%, and the yield is 91.18%.
[0031] Example 3
[0032] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed in gaseous form for reaction. The reaction product passes through the bed and exits from the top of the reactor, entering the hydrogen chloride absorption device, the hydrogen chloride absorption temperature is set at 50°C, the product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption, and obtains the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2211 grams of product, the GC detection content is 99.18%, and the yield is 91.69%.
[0033] Example 4
[0034] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 500 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 3111 grams of product, the GC detection content is 99.32%, and the yield is 77.52%.
[0035] Example 5
[0036] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 700 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2,300 grams of product, the GC detection content is 99.19%, and the yield is 40.88%.
[0037] Example 6
[0038] In a fixed bed reactor filled with activated carbon (fixed bed diameter 15 mm, length 1 m, filled with activated carbon catalyst), trifluoromethyl sulfhydryl chloride and chlorine, water (molar ratio 1:2.4:2.3, space velocity 1000 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 1211 grams of product, the GC detection content is 99.32%, and the yield is 15.09%.
[0039] Example 7
[0040] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:1:1, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 1101 grams of product, the GC detection content is 99.32%, and the yield is 91.45%.
[0041] Example 8
[0042] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:10:10, space velocity of 300 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2209 grams of product, the GC detection content is 99.11%, and the yield is 91.55%.
[0043] Example 9
[0044] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:5:5, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2207 grams of product, the GC detection content is 99.13%, and the yield is 91.48%.
[0045] Example 10
[0046] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:10:5, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2205 grams of product, the GC detection content is 99.13%, and the yield is 91.40%.
[0047] Embodiment 11
[0048] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:5:10, space velocity of 300 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2200 grams of product, the GC detection content is 99.11%, and the yield is 91.17%.
[0049] Example 12
[0050] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 120°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2212 grams of product, the GC detection content is 98.32%, and the yield is 90.94%.
[0051] Example 13
[0052] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfide, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 80°C, and the material enters the bed in gaseous form for reaction. The reaction product passes through the bed and exits from the top of the reactor, entering the hydrogen chloride absorption device, the hydrogen chloride absorption temperature is set at 50°C, the product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption, and obtains the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2000 grams of product, the GC detection content is 98.11%, and the yield is 82.05%.
[0053] Embodiment 14
[0054] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 60°C, and the material enters the bed in gaseous form for reaction. The reaction product passes through the bed and exits from the top of the reactor, entering the hydrogen chloride absorption device, the hydrogen chloride absorption temperature is set at 50°C, the product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption, and obtains the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 1442 grams of product, the GC detection content is 98.12%, and the yield is 59.16%.
[0055] Embodiment 15
[0056] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 50°C, and the material enters the bed in gaseous form for reaction. The reaction product passes through the bed and exits from the top of the reactor, entering the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 677 grams of product, the GC detection content is 98.12%, and the yield is 27.78%.
[0057] Example 16
[0058] In a fixed bed reactor filled with activated carbon, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 20°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 406 grams of product, the GC detection content is 98.22%, and the yield is 16.67%.
[0059] Embodiment 17
[0060] In a fixed bed reactor equipped with molecular sieves, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 110°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2201 grams of product, the GC detection content is 99.11%, and the yield is 91.21%.
[0061] Embodiment 18
[0062] In a fixed bed reactor filled with resin, trifluoromethyl sulfhydryl chloride, chlorine, and water (molar ratio of 1:2.4:2.3, space velocity of 300 h -1 ) enters from the bottom of the fixed bed, the tower kettle and the fixed bed are heated, the temperature is set to 120°C, and the material enters the bed layer in gaseous form for reaction. The reaction product passes through the bed layer and exits from the top of the reactor, and enters the hydrogen chloride absorption device. The hydrogen chloride absorption temperature is set at 50°C. The product trifluoromethylsulfonyl chloride enters 0°C for condensation and liquefaction after hydrogen chloride absorption to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine enters the liquid alkali for absorption. The reaction is continuously fed for 6 hours to obtain 2204 grams of product, the GC detection content is 99.33%, and the yield is 91.54%.
[0063] Comparative Example 1
[0064] In a reactor filled with activated carbon, trifluoromethylsulfonyl chloride, chlorine and water (molar ratio of 1:2.4:2.3) were introduced, the reactor temperature was 110°C, the reaction time was 4h, the product came out from the top of the reactor and entered the hydrogen chloride absorption device, the hydrogen chloride absorption setting temperature was 50°C, the product trifluoromethylsulfonyl chloride was absorbed by hydrogen chloride and then entered 0°C for condensation and liquefaction to obtain the product trifluoromethylsulfonyl chloride. Excess chlorine was absorbed by liquid alkali. 654g of product was obtained, the GC detection content was 91.5%, and the yield was 76.4%.
Claims
1. A method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed, characterized in that: Trifluoromethyl sulfonyl chloride, chlorine and water react continuously under the action of a catalyst to generate trifluoromethyl sulfonyl chloride; the reaction is carried out in a fixed bed reactor; trifluoromethyl sulfonyl chloride, chlorine and water enter the fixed bed reactor in gaseous form; the catalyst is activated carbon, resin or molecular sieve; the reaction temperature is 50-120°C; the space velocity is 100~500 h -1 .
2. The method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed according to claim 1, characterized in that: The molar ratio of trifluoromethyl sulfoxide, chlorine gas and water is 1:1~10:1~10.
3. The method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed according to claim 2, characterized in that: The molar ratio of trifluoromethyl sulfhydryl chloride, chlorine and water is 1:1.5~5:1.5~5; the reaction temperature is 50~120℃, and the space velocity is 100~500 h -1 .
4. The method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed according to any one of claims 1 to 3, characterized in that: Trifluoromethylsulfonyl chloride, chlorine and water are introduced into a fixed bed reactor containing a catalyst, and heated to react continuously to obtain trifluoromethylsulfonyl chloride.
5. The method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed according to claim 4, characterized in that: The product obtained by the reaction is discharged from the top of the reactor, and is absorbed by a hydrogen chloride absorption device, and the remaining product is condensed to obtain trifluoromethylsulfonyl chloride.
6. The method for synthesizing trifluoromethylsulfonyl chloride by continuous chlorination oxidation in a fixed bed according to claim 5, characterized in that: The absorption temperature of hydrogen chloride is 40~60℃; the condensation temperature is 0℃.
Citation Information
Patent Citations
Preparation method of trifluoromethylsulfonyl chloride
CN115724774A
Method for continuously preparing trifluoromethylsulfonyl chloride
CN117720441A