Device for continuously producing methylsulfonyl fluoride

Abstract

The utility model relates to the technical field of methylsulfonyl fluoride preparation, in particular to a device for continuously producing methylsulfonyl fluoride. Comprising a reactor, a top feed port of the reactor is connected with a methylsulfonyl chloride storage tank, a bottom feed port of the reactor is connected with a hydrogen fluoride steel cylinder, a bottom discharge port of the reactor is connected with a methylsulfonyl fluoride storage tank, and a top gas outlet of the reactor is connected with a hydrogen fluoride reflux device. A liquid outlet of the hydrogen fluoride reflux device is connected with the side wall of the reactor, a gas outlet of the hydrogen fluoride reflux device is connected with a hydrogen chloride storage tank, and a discharge hole in the bottom of the reactor is also connected with an online analysis system. According to the utility model, through a bubbling mode, the reaction is more sufficient, and the volatilized hydrogen fluoride gas returns to the reactor through the reflux device and continuously participates in the reaction. According to the utility model, an on-line analysis system is adopted, regular sampling is carried out, products are collected after the products are qualified, otherwise, the reaction is continued, and continuous production of methylsulfonyl fluoride is realized.

Description

TECHNICAL FIELD

[0001] The utility model relates to methylsulfonyl fluoride preparation technical field, concretely relates to a kind of device for continuous production methylsulfonyl fluoride. BACKGROUND

[0002] Methylsulfonyl fluoride is an important raw material for preparing trifluoromethanesulfonyl fluoride, which is insoluble in water and soluble in anhydrous hydrogen fluoride. There are two methods for producing methylsulfonyl fluoride at present. One is to use potassium fluoride as a fluorinating agent to react with methylsulfonyl chloride, and the other is to use hydrogen fluoride as a fluorinating agent to react with methylsulfonyl chloride.

[0003] Chinese patent CN101747238B discloses a method for separating and preparing methylsulfonyl fluoride from the reaction mixture of methylsulfonyl chloride and potassium fluoride. The specific steps are as follows: (1) mixing water, potassium fluoride and methylsulfonyl chloride, or mixing aqueous potassium fluoride solution with methylsulfonyl chloride to undergo fluorination reaction; (2) adding a neutralizing agent for neutralization reaction; (3) cooling and crystallizing; (4) solid-liquid separation of the obtained material; (5) liquid-liquid separation of the liquid phase obtained in the previous step, and the oil phase enters the next step; (6) adding a dehydrating agent for dehydration treatment; (7) solid-liquid separation of the material obtained in the previous step; (8) vacuum distillation separation of the liquid phase obtained in the previous step, and the gaseous phase is condensed to obtain methylsulfonyl fluoride. However, in this method, water is used as a solvent to generate methylsulfonyl fluoride using potassium fluoride as a fluorinating agent, and there is a large amount of water in the methylsulfonyl fluoride. The water needs to be removed by distillation to obtain high-quality methylsulfonyl fluoride, and the preparation process is complicated. Chinese patent CN112661676B discloses a method for preparing methylsulfonyl fluoride from methylsulfonyl chloride. However, in this method, hydrogen fluoride is used as a fluorinating agent, and methylsulfonyl chloride is mixed with hydrogen fluoride and then added to a reaction kettle. As the temperature rises in the reaction kettle, most of the hydrogen fluoride will vaporize and be discharged into the tail gas absorption system, which reduces the content of hydrogen fluoride in the reaction kettle and lowers the yield of methylsulfonyl fluoride. Moreover, this method is a batch operation, and the mixture needs to be sampled and reacted after each kettle is qualified, which cannot realize continuous production.

[0004] In summary, the existing technology for producing trifluoromethanesulfonyl fluoride still has the problems of complicated preparation process or inability to realize continuous production. Therefore, there is an urgent need to develop a device for continuous production of methylsulfonyl fluoride to solve the problems existing in the prior art. UTILITY MODEL CONTENT

[0005] To solve the problems of complicated preparation process or inability to realize continuous production in the existing technology for producing trifluoromethanesulfonyl fluoride, the utility model provides a device for continuous production of methylsulfonyl fluoride to realize continuous production of trifluoromethanesulfonyl fluoride.

[0006] The technical solution adopted by the utility model is as follows:

[0007] A device for continuously producing methylsulfonyl fluoride comprises a reactor, wherein a top feed port of the reactor is connected to a methylsulfonyl chloride storage tank, a bottom feed port of the reactor is connected to a hydrogen fluoride cylinder, a bottom discharge port of the reactor is connected to a methylsulfonyl fluoride storage tank, a top gas outlet of the reactor is connected to a hydrogen fluoride reflux device, a liquid outlet of the hydrogen fluoride reflux device is connected to the top of the reactor, a gas outlet of the hydrogen fluoride reflux device is connected to a hydrogen chloride storage tank, and the bottom discharge port of the reactor is also connected to an online analysis system.

[0008] Preferably, a flow meter is provided on the connecting pipeline between the feed port at the top of the reactor and the methylsulfonyl chloride storage tank for monitoring the flow of methylsulfonyl chloride.

[0009] Preferably, a stirring mechanism is provided inside the reactor, the stirring mechanism comprises a stirring shaft and stirring blades, and the stirring shaft is driven by a motor provided outside the reactor.

[0010] Preferably, the stirring shaft and stirring blades are made of Monel alloy.

[0011] Preferably, the outer wall of the reactor is provided with a jacket, a heating rod is provided inside the jacket, and circulating water is installed inside the jacket.

[0012] Preferably, a three-way element is provided at the bottom discharge port of the reactor, and the three interfaces of the three-way element are respectively connected to the reactor, the methylsulfonyl fluoride storage tank and the online analysis system.

[0013] Preferably, the online analysis system is used to detect whether the product is qualified, and automatically takes samples for detection every 1 hour; the online analysis system includes a sampler and a detection instrument.

[0014] Preferably, the detection instrument is a high performance liquid chromatograph.

[0015] Preferably, the hydrogen fluoride reflux device is a graphite shell and tube heat exchanger.

[0016] Compared with the prior art, the beneficial effects of the present invention are:

[0017] (1) In the present invention, hydrogen fluoride and methylsulfonyl chloride are fully contacted by bubbling, the contact area is increased, and the reaction is more complete. The volatilized hydrogen fluoride gas is refluxed into the reactor through the hydrogen fluoride reflux device and continues to react with the methylsulfonyl chloride, thereby reducing the volatilization of hydrogen fluoride.

[0018] (2) The utility model adopts an online analysis system, which automatically samples and tests every hour. After the sampling and testing are qualified, the discharge valve is opened to release the methylsulfonyl fluoride product into the methylsulfonyl fluoride storage tank. Then, the reactor feed valve is opened to add the raw materials to the reactor, and the reaction is continued to sample and collect the product. This cycle realizes the continuous production of methylsulfonyl fluoride. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following briefly describes the drawings required for the specific embodiments or the description of the prior art. Similar elements or parts are generally identified by similar reference numerals throughout the drawings. Elements or parts in the drawings are not necessarily drawn to scale.

[0020] Figure 1 The present invention provides a schematic diagram of a device for continuously producing methylsulfonyl fluoride.

[0021] Explanation of the accompanying symbols: 1. Methanesulfonyl chloride storage tank; 2. Hydrogen fluoride cylinder; 3. Reactor; 4. Hydrogen fluoride reflux device; 5. Methanesulfonyl fluoride storage tank; 6. Hydrogen chloride storage tank; 7. Flow meter; 8. Online analysis system. DETAILED DESCRIPTION

[0022] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the utility model, the following is a detailed description of the specific implementation method, structure, characteristics and functions of the present invention in combination with the accompanying drawings and preferred embodiments.

[0023] Example 1

[0024] This embodiment provides a device for continuously producing methylsulfonyl fluoride. Figure 1 The reactor 3 comprises a top feed port connected to a methylsulfonyl chloride storage tank 1, a bottom feed port connected to a hydrogen fluoride cylinder 2, a bottom discharge port connected to a methylsulfonyl fluoride storage tank 5, a top gas outlet connected to a hydrogen fluoride reflux device 4, a liquid outlet of the hydrogen fluoride reflux device 4 connected to the top of the reactor 3, a gas outlet of the hydrogen fluoride reflux device 4 connected to a hydrogen chloride storage tank 6, and a bottom discharge port connected to an online analysis system 8 for testing product quality by automatically sampling and testing every hour. The online analysis system 8 includes a sampler and a detection instrument, which may be a high-performance liquid chromatograph.

[0025] A flow meter 7 is provided on the connecting pipe between the top feed port of the reactor 3 and the methylsulfonyl chloride storage tank 1. The flow meter 7 is used to monitor the flow rate of the methylsulfonyl chloride. The flow rate range of the flow meter 7 can be 300 to 500 g / h.

[0026] A stirring mechanism is provided inside the reactor 3, and the stirring mechanism includes a stirring shaft and a stirring blade, and the stirring shaft is driven by a motor provided outside the reactor 3. The material of the stirring shaft and the stirring blade is monel alloy.

[0027] The outer wall of the reactor 3 is provided with a jacket, a heating rod is provided inside the jacket, and circulating water is filled inside the jacket.

[0028] A three-way element is provided at the bottom discharge port of the reactor 3 , and the three-way element is respectively connected to the reactor 3 , the methylsulfonyl fluoride storage tank 5 and the online analysis system 8 .

[0029] The hydrogen fluoride reflux device 4 is a graphite shell and tube heat exchanger.

[0030] The implementation principle of this application:

[0031] First, the reactor 3 of the present application is used to react and generate methylsulfonyl fluoride; after the reaction starts, the methylsulfonyl chloride in the methylsulfonyl chloride storage tank 1 enters the reactor 3 from the top feed port of the reactor 3, and the hydrogen fluoride in the hydrogen fluoride cylinder 2 enters the reactor 3 from the feed port at the bottom of the reactor 3. After the methylsulfonyl chloride and hydrogen fluoride enter the reactor 3, they react under the action of the stirring mechanism. During the reaction, the partially volatilized hydrogen fluoride and the hydrogen chloride produced by the reaction enter the hydrogen fluoride reflux device 4 from the top gas outlet of the reactor 3. The hydrogen fluoride returns to the reactor 3 again under the condensation of the reflux device, and the hydrogen chloride enters the hydrogen chloride storage tank 6 through the gas outlet of the hydrogen fluoride reflux device 4. The methylsulfonyl fluoride generated by the reaction is tested for quality by the online analysis system 8 connected to the bottom of the reactor 3. Sampling and detection are performed every 1h. If qualified, the discharge valve is opened to put the methylsulfonyl fluoride fine product into the methylsulfonyl fluoride storage tank 5. If unqualified, the reaction is continued. Such a cycle realizes the continuous production of methylsulfonyl fluoride.

[0032] Among them, the outer wall of the reactor 3 is provided with a jacket, and a heating rod is provided inside the jacket for heating the reactor 3, and the jacket is filled with circulating water for serving as a heating medium; a flow meter 7 is provided on the connecting pipe between the top feed port of the reactor 3 and the methylsulfonyl chloride storage tank 1 for controlling the feed rate of methylsulfonyl chloride, and the flow range of the flow meter 7 is 300 to 500 g / h; the material of the stirring mechanism inside the reactor 3 is monel alloy, and the stirring mechanism includes a stirring shaft and a stirring blade, and the stirring shaft is driven by a motor provided outside the reactor 3; the reactor 3, the methylsulfonyl fluoride storage tank 5 and the online analysis system 8 are connected by a three-way element; the online analysis system includes a sampler and a detection instrument, and the detection instrument is a high performance liquid chromatograph; the hydrogen fluoride reflux device 4 is a graphite tube heat exchanger.

[0033] According to the above technical solutions, a kind of continuous production methylsulfonyl fluoride device provided by the utility model. Hydrogen fluoride is fully contacted with methylsulfonyl chloride by bubbling mode, contact area is increased, reaction is more sufficient, and the hydrogen fluoride gas volatilized is refluxed into reactor 3 by hydrogen fluoride reflux condenser, continues to react with methylsulfonyl chloride, reduces the volatilization of hydrogen fluoride. The utility model adopts online analysis system 8, and automatic sampling detection is carried out every 1h. After sampling detection is qualified, discharge valve is opened and methylsulfonyl fluoride fine product is put into methylsulfonyl fluoride storage tank 5. Then reactor 3 feed valves are opened again and raw material is added into reactor 3, reaction sampling is continued and fine product is collected, and the continuous production of methylsulfonyl fluoride is realized in this cycle.

[0034] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as a preferred embodiment as above, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments using the technical contents disclosed above without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A device for continuously producing methylsulfonyl fluoride, characterized in that: The invention comprises a reactor (3), wherein the top feed port of the reactor (3) is connected to a methylsulfonyl chloride storage tank (1), the bottom feed port of the reactor (3) is connected to a hydrogen fluoride cylinder (2), the bottom discharge port of the reactor (3) is connected to a methylsulfonyl fluoride storage tank (5), the top gas outlet of the reactor (3) is connected to a hydrogen fluoride reflux device (4), the liquid outlet of the hydrogen fluoride reflux device (4) is connected to the top of the reactor (3), the gas outlet of the hydrogen fluoride reflux device (4) is connected to a hydrogen chloride storage tank (6), and the bottom discharge port of the reactor (3) is also connected to an online analysis system (8).

2. A device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that, A flow meter (7) is provided on the connecting pipeline between the top feed port of the reactor (3) and the methylsulfonyl chloride storage tank (1) for monitoring the flow of methylsulfonyl chloride.

3. A device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that, A stirring mechanism is provided inside the reactor (3), and the stirring mechanism comprises a stirring shaft and stirring blades. The stirring shaft is driven by a motor provided outside the reactor (3).

4. A device for continuously producing methylsulfonyl fluoride according to claim 3, characterized in that, The material of the stirring shaft and the stirring blade is Monel alloy.

5. The device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that: The outer wall of the reactor (3) is provided with a jacket, a heating rod is provided inside the jacket, and circulating water is contained inside the jacket.

6. The device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that: A three-way element is provided at the bottom discharge port of the reactor (3), and the three interfaces of the three-way element are respectively connected to the reactor (3), the methylsulfonyl fluoride storage tank (5) and the online analysis system (8).

7. The device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that: The online analysis system (8) is used to detect whether the product is qualified, and automatically takes samples for detection every hour; the online analysis system (8) includes a sampler and a detection instrument.

8. The device for continuously producing methylsulfonyl fluoride according to claim 7, characterized in that: The detection instrument is a high performance liquid chromatograph.

9. The device for continuously producing methylsulfonyl fluoride according to claim 1, characterized in that: The hydrogen fluoride reflux device (4) is a graphite tube heat exchanger.

Images