An apparatus for preparing triflate

Abstract

The utility model relates to fluorine kind organic compound synthetic equipment technical field provides a device for preparing trifluoromethanesulfonamide, including horizontal tubular reactor, the spiral subassembly of being located in horizontal tubular reactor, the raw material gas inlet of being located in horizontal tubular reactor upper portion, the liquid inlet of being located in horizontal tubular reactor lower part and the filter component of being located in horizontal tubular reactor discharge gate. The raw material gas inlet is connected with the mixed pipeline, and trifluoromethanesulfonyl fluoride gas inlet and ammonia gas inlet are communicated with the mixed pipeline. The utility model realizes material mixing through the agitation of spiral subassembly, the effect of fast reaction, and the filter component of being arranged in the tubular reactor export end carries out ammonium fluoride retention collection, obtains trifluoromethanesulfonamide, acetone solution enters subsequent drying system, recycles acetone and obtains pure trifluoromethanesulfonamide to realize continuous preparation.

Description

Technical Field

[0001] This utility model relates to the technical field of equipment for synthesizing fluorine-based organic compounds, and in particular to an apparatus for preparing trifluoromethanesulfonamide. Background Technology

[0002] Trifluoromethanesulfonamide, due to its structural characteristics, possesses high electrochemical stability and conductivity, making it an excellent additive for organic electrolytes. It can also serve as an intermediate in the further synthesis of higher value-added lithium bis(trifluoromethanesulfonyl)imide. Furthermore, as a common organic synthetic chemical reagent, it can undergo condensation reactions with carboxylic acid compounds in the presence of condensing agents to yield corresponding amide derivatives. In recent years, with the gradual maturation of small- and pilot-scale acylation processes and the growth of market demand, the industrialization process has accelerated. Consequently, the demand for high-purity trifluoromethanesulfonamide has increased dramatically, and its production process has attracted considerable attention.

[0003] CN111253292B discloses a method for preparing a trifluoromethanesulfonyl compound: trifluoromethylsulfinate, a halogenated compound, and boron trifluoride diethyl ether are added to an organic solvent for reaction to obtain the trifluoromethanesulfonyl compound. The method described in this invention exhibits significant fluctuations in yield and product purity, high instability, and the batch process requires stepwise feeding, resulting in long reaction times, the need for gradient acoustic wave control, high energy consumption, and limited production capacity. The generated ammonium chloride solid easily clogs pipelines, requiring frequent shutdowns for filtration, leading to interruptions in production continuity and intermittent reaction, which is detrimental to industrialization.

[0004] CN116462614A discloses a method for preparing trifluoromethanesulfonamide, which uses CF3SO2Cl, anhydrous acetonitrile, and ammonia. The mixture is filtered, distilled under reduced pressure, and dried under reduced pressure to obtain crude trifluoromethanesulfonamide. This invention first purifies the crude product by reduced pressure distillation, then performs intermittent reduced pressure distillation to further remove trace impurities such as fluoride ions, yielding high-purity trifluoromethanesulfonamide. However, because an intermittent reactor is used, the trifluoromethanesulfonyl chloride and ammonia react in a pure gas phase. In this gas-liquid heterogeneous reaction, the ammonia is unevenly dispersed, and local overheating can easily trigger side reactions, resulting in a low product conversion rate.

[0005] The above methods and equipment used in the production process are not suitable for continuous production, resulting in low production efficiency and low product conversion rate. Utility Model Content

[0006] The present invention aims to provide an apparatus for preparing trifluoromethanesulfonamide, which facilitates continuous production.

[0007] To achieve the above objectives, the technical solution of this utility model is implemented as follows:

[0008] An apparatus for preparing trifluoromethanesulfonamide includes a horizontal tubular reactor, a spiral assembly disposed within the horizontal tubular reactor, a raw material inlet disposed at the upper part of the horizontal tubular reactor, a liquid inlet disposed at the lower part of the horizontal tubular reactor, and a filter assembly disposed at the discharge outlet of the horizontal tubular reactor.

[0009] The raw material inlet is connected to a mixing pipeline, and a trifluoromethanesulfonyl fluoride inlet and an ammonia inlet are connected to the mixing pipeline.

[0010] Furthermore, the horizontal tubular reactor includes a tube with a reaction chamber, and a partition plate arranged radially therein is provided in the tube, the partition plate dividing the reaction chamber into a stirring chamber and a conveying chamber;

[0011] The partition plate is provided with a through hole connecting the stirring chamber and the conveying chamber.

[0012] Furthermore, the spiral assembly includes a drive unit and a spiral shaft disposed at the power output end of the drive unit. The spiral shaft extends along the axial direction of the tube body and passes through the partition plate.

[0013] A stirring blade is provided on the spiral shaft located in the stirring chamber. Several stirring blades are evenly distributed on the spiral shaft around the circumference. A spiral plate is provided on the spiral shaft located in the conveying chamber. The conveying direction of the spiral plate is towards one end of the discharge port.

[0014] Furthermore, flow meters and regulating valves are provided at the trifluoromethanesulfonyl fluoride inlet, the ammonia inlet, and the liquid inlet.

[0015] Furthermore, the pipe body is horizontally arranged on the ground, the outlet is located at the end of the pipe body, and the outlet is connected to the filter assembly through the outlet pipe.

[0016] Furthermore, the filtration assembly includes a filter tank with a cavity, a spray section communicating with the discharge pipe inside the filter tank, and a first screen and a second screen disposed below the spray section.

[0017] Furthermore, the first screen includes a first mesh size of 50-100 μm, and the second screen includes a second mesh size of 20-50 μm.

[0018] Furthermore, the filter tank is provided with an intermediate plate, which is located between the first screen and the second screen, and the intermediate plate has downward flow holes;

[0019] A first screening chamber is formed between the first screen and the intermediate plate, and a second screening chamber is formed between the intermediate plate and the lower part of the filter tank.

[0020] Furthermore, a pressure tank is provided between the first screening chamber and the second screening chamber. The inlet of the pressure tank is connected to the first screening chamber through a liquid inlet pipe, and the outlet of the pressure tank is connected to the side of the second screen through a liquid outlet pipe.

[0021] Furthermore, the second screen includes several screen layers, and several second mesh openings are evenly distributed on the screen layers;

[0022] The second mesh includes a second hole and a third hole;

[0023] The second hole in the upper layer is staggered with the third hole in the adjacent layer;

[0024] A guide plate is provided between the second hole in the upper layer and the third hole in the adjacent layer. One end of the guide plate abuts against the second hole in the upper layer, and the other end extends into the two adjacent third holes in the lower layer.

[0025] Compared with the prior art, this utility model has the following advantages:

[0026] The apparatus for preparing trifluoromethanesulfonamide described in this invention uses a horizontal tubular reactor with a spiral assembly to transport the raw materials. Trifluoromethanesulfonyl fluoride and ammonia are pre-mixed and then fed into the raw material inlet at the top of the tubular reactor. The liquid inlet at the bottom is used to transport acetone solution. The spiral assembly agitates the materials to achieve a rapid reaction. Ammonium fluoride is collected and retained by a filter assembly at the outlet of the tubular reactor. The resulting trifluoromethanesulfonamide and acetone solution enter a subsequent drying system. The acetone is recovered to obtain pure trifluoromethanesulfonamide, thus achieving continuous preparation. Attached Figure Description

[0027] The accompanying drawings, which form part of this utility model, are used to provide a further understanding of the utility model. The illustrative embodiments of the utility model and their descriptions are used to explain the utility model and do not constitute an undue limitation of the utility model. In the drawings:

[0028] Figure 1 This is a schematic diagram of the overall structure of the apparatus for preparing trifluoromethanesulfonamide according to an embodiment of the present invention;

[0029] Figure 2 This is a cross-sectional schematic diagram of the horizontal tubular reactor, spiral assembly, and filter assembly described in an embodiment of the present invention;

[0030] Figure 3 for Figure 2 A magnified view of a section at point I;

[0031] Figure 4 This is a cross-sectional schematic diagram of the second screen described in an embodiment of the present invention;

[0032] Figure 5 for Figure 4 A magnified view of section II in the middle.

[0033] Explanation of reference numerals in the attached figures:

[0034] 1. Trifluoromethanesulfonyl fluoride inlet; 2. Ammonia inlet; 3. Liquid inlet; 4. Horizontal tubular reactor; 5. Spiral assembly; 6. Filter assembly; 7. Mixing pipeline; 8. Discharge pipe; 9. Pressure tank; 10. Liquid outlet pipe;

[0035] 401. Pipe body; 402. Divider plate; 403. Stirring chamber; 404. Conveying chamber; 405. Through hole;

[0036] 501. Drive unit; 502. Spiral shaft; 503. Stirring blades; 504. Spiral plate;

[0037] 601. Filter tank; 602. Spray section; 603. First screen; 604. Second screen; 605. Second screening chamber; 606. Intermediate plate; 607. First screening chamber;

[0038] 6041, sieve layer; 6042, second hole; 6043, third hole; 6044, guide plate. Detailed Implementation

[0039] It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.

[0040] In the description of this utility model, it should be noted that the terms "upper," "lower," "inner," and "back," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0041] Furthermore, in the description of this utility model, unless otherwise explicitly defined, the terms "installation," "connection," "joining," and "connector" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model in light of the specific circumstances.

[0042] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0043] Example 1

[0044] This embodiment relates to an apparatus for preparing trifluoromethanesulfonamide, generally speaking, as Figure 1 As shown, the apparatus for preparing trifluoromethanesulfonamide includes a horizontal tubular reactor 4, a spiral assembly 5 disposed within the horizontal tubular reactor 4, a raw material inlet located at the upper part of the horizontal tubular reactor 4, a liquid inlet 3 located at the lower part of the horizontal tubular reactor 4, and a filter assembly 6 located at the outlet of the horizontal tubular reactor 4. The raw material inlet is connected to a mixing pipeline 7, and a trifluoromethanesulfonyl fluoride inlet 1 and an ammonia inlet 2 are connected to the mixing pipeline 7.

[0045] Based on the above configuration, this embodiment uses a spiral assembly 5 inside a horizontal tubular reactor 4 to transport raw materials. Trifluoromethanesulfonyl fluoride and ammonia are pre-mixed and then fed into the raw material inlet at the top of the tubular reactor. The liquid inlet 3 at the bottom is used to transport acetone solution. The material mixing and rapid reaction are achieved by the stirring of the spiral assembly 5. Ammonium fluoride is intercepted and collected by the filter assembly 6 at the outlet of the tubular reactor. The resulting trifluoromethanesulfonamide and acetone solution enter the subsequent drying system. The acetone is recovered to obtain pure trifluoromethanesulfonamide for continuous preparation.

[0046] Based on the above overall description, an exemplary structure of the apparatus for preparing trifluoromethanesulfonamide in this embodiment is as follows: Figure 1 As shown, the horizontal tubular reactor 4 is installed parallel to the ground by a support frame, and the device performs the following reaction:

[0047] CF3SO2F+2NH3→CF3SO2NH2+NH4F.

[0048] In this embodiment, the raw material inlet is a mixing pipeline 7. The trifluoromethanesulfonyl fluoride inlet 1 and the ammonia inlet 2 are respectively connected to the mixing pipeline 7 to achieve premixing of the two raw materials. No additional premixing equipment is required, and the structure is more streamlined.

[0049] As a preferred embodiment, such as Figure 1 and Figure 2 As shown, the horizontal tubular reactor 4 includes a tube 401 with a reaction chamber. A partition plate 402 is provided within the tube 401, arranged radially therein. The partition plate 402 divides the reaction chamber into a stirring chamber 403 and a conveying chamber 404. A through hole 405 is provided on the partition plate 402 connecting the stirring chamber 403 and the conveying chamber 404. In this embodiment, a separate stirring chamber 403 is provided to improve the mixing uniformity of the gas and liquid phases. Mixing the gaseous raw materials first and then mixing them with the liquid acetone helps to improve the conversion rate.

[0050] Furthermore, such as Figure 1 and Figure 2 As shown, the spiral assembly 5 includes a drive unit 501 and a spiral shaft 502 located at the power output end of the drive unit 501. The spiral shaft 502 extends axially along the tube body 401 and passes through the partition plate 402. Agitator blades 503 are provided on the spiral shaft 502 located in the stirring chamber 403, with several agitator blades 503 evenly distributed circumferentially on the spiral shaft 502. A spiral plate 504 is provided on the spiral shaft 502 located in the conveying chamber 404, with the conveying direction of the spiral plate 504 facing the discharge port.

[0051] In this embodiment, the drive unit 501 uses a geared motor or a servo motor. The motor drives the spiral shaft 502 to rotate, which in turn drives the stirring blades 503 to stir the raw materials, further improving the mixing uniformity of the gas and liquid phases. After stirring, the mixture flows through the through hole 405 to the conveying chamber 404 for conveying. During the long-distance conveying process, the solution and gas are transported and mixed along the conveying direction of the spiral plate 504, thereby improving the reaction effect. The produced ammonium fluoride is pushed to the discharge port and intercepted by the filter assembly 6.

[0052] Preferably, flow meters and regulating valves are installed at the trifluoromethanesulfonyl fluoride inlet 1, the ammonia inlet 2, and the liquid inlet 3. The flow meters facilitate the measurement and monitoring of the gaseous and liquid raw materials, while the regulating valves allow for the adjustment of the feed rate, ensuring the precision of trifluoromethanesulfonamide preparation.

[0053] Furthermore, such as Figure 2 As shown, the pipe body 401 is horizontally arranged on the ground, and the discharge port is located at the end of the pipe body 401. The discharge port is connected to the filter assembly 6 through the discharge pipe 8.

[0054] In addition, such as Figure 2 and Figure 3 As shown, the filter assembly 6 includes a filter tank 601 with a cavity, a spray section 602 communicating with the discharge pipe 8 inside the filter tank 601, and a first screen 603 and a second screen 604 disposed below the spray section 602. In this embodiment, the spray section 602 consists of a water pipe communicating with the discharge pipe 8 and a plurality of nozzles disposed on the water pipe. The stirred gaseous solution flows into the filter tank 601 through the discharge pipe 8 and is sprayed onto the first screen 603 in a spray manner.

[0055] By setting it to a spray mode to form micron-sized droplet clusters, unreacted ammonia and trace amounts of trifluoromethanesulfonyl chloride vapor in the reaction tail gas are efficiently captured, preventing the leakage of toxic gases and enhancing the gas-liquid-solid three-phase mass transfer efficiency.

[0056] Preferably, the first screen 603 includes a first mesh size of 50-100 μm, and the second screen 604 includes a second mesh size of 20-50 μm. In this embodiment, both the first screen 603 and the second screen 604 are made of stainless steel and use double-layer filtration to separate ammonium chloride crystals in the spray liquid, achieving continuous solid-liquid separation, avoiding intermittent processes, and reducing filter clogging.

[0057] In addition, such as Figure 3 As shown, the filter tank 601 is provided with an intermediate plate 606, which is located between the first screen 603 and the second screen 604. The intermediate plate 606 has downward flow holes. The first screen 603 and the intermediate plate 606 form a first screening chamber 607, and the intermediate plate 606 and the lower part of the filter tank 601 form a second screening chamber 605.

[0058] Furthermore, such as Figure 3 As shown, a pressure tank 9 is provided between the first screening chamber 607 and the second screening chamber 605. The inlet of the pressure tank 9 is connected to the first screening chamber 607 through a liquid inlet pipe, and the outlet of the pressure tank 9 is connected to the side of the second screen 604 through a liquid outlet pipe 10. Some of the liquid in the first screening chamber 607 enters the pressure tank 9. The pressure tank 9 is equipped with a detector to detect high ammonium chloride content. When the ammonium chloride content exceeds the standard, it indicates that the second screen 604 is blocked. The pressure tank 9 adjusts the pressure, and the liquid stored in the pressure tank 9 applies pressurized liquid to the side of the second screen 604 to flush it, ensuring the unobstructed flow of the second mesh.

[0059] Furthermore, such as Figure 4 and Figure 5 As shown, the second screen 604 includes several screen layers 6041, with several second mesh openings evenly distributed on the screen layers 6041. The second mesh openings include second holes 6042 and upper-layer second holes 6042 interleaved with the third holes 6043 of adjacent layers. A guide plate 6044 is provided between the upper-layer second holes 6042 and the adjacent-layer third holes 6043. One end of the guide plate 6044 abuts against the upper-layer second mesh opening, and the other end extends into two adjacent lower-layer third holes 6043. Liquid passes through the upper-layer second holes 6042, is guided by the guide plate 6044, and enters the third holes 6043. The guide plates 6044 in each layer reduce continuous clogging of the upper-layer mesh openings, increasing filtration smoothness.

[0060] The preparation method of trifluoromethanesulfonamide in this embodiment includes the following steps:

[0061] B1. Start the horizontal tubular reactor 4 and the spiral assembly 5 for spiral stirring;

[0062] B2. Open the bottom solvent inlet regulating valve and the top trifluoromethanesulfonyl fluoride and ammonia gas inlet regulating valve of the horizontal tubular reactor 4.

[0063] B3. By controlling the mass flow ratio of the above substances to 7:4:1 through the regulating valve, 89g of trifluoromethanesulfonyl fluoride and 22.2g of ammonia are continuously introduced into the horizontal tubular reactor 4. Theoretically, 86.7g of trifluoromethanesulfonamide should be produced.

[0064] B4. After running for a cumulative 60-70 hours, stop the intake reaction and clean the ammonium fluoride from filter assembly 6.

[0065] B5. The product was weighed in the downstream solvent recovery unit area and the weight was 81.7g. The conversion rate of this batch was calculated to be 94.2%.

[0066] Example 2

[0067] This embodiment relates to an apparatus for preparing trifluoromethanesulfonamide, and the method for preparing trifluoromethanesulfonamide using this apparatus includes the following steps:

[0068] B1. Start the horizontal tubular reactor 4 and the spiral assembly 5 for spiral stirring;

[0069] B2. Open the bottom solvent inlet regulating valve and the top trifluoromethanesulfonyl fluoride and ammonia gas inlet regulating valve of the horizontal tubular reactor 4.

[0070] B3. By controlling the mass flow ratio of the above substances to 7:4:1 through the regulating valve, 94g of trifluoromethanesulfonyl fluoride and 23.5g of ammonia are continuously introduced into the horizontal tubular reactor 4. Theoretically, 91.5g of trifluoromethanesulfonamide should be produced.

[0071] B4. After running for a cumulative 60-70 hours, stop the intake reaction and clean the ammonium fluoride from filter assembly 6.

[0072] B5. The product was weighed in the downstream solvent recovery unit area and the weight was 86.6g. The conversion rate of this batch was calculated to be 94.6%.

[0073] Example 3

[0074] This embodiment relates to an apparatus for preparing trifluoromethanesulfonamide, and the method for preparing trifluoromethanesulfonamide using this apparatus includes the following steps:

[0075] B1. Start the horizontal tubular reactor 4 and the spiral assembly 5 for spiral stirring;

[0076] B2. Open the bottom solvent inlet regulating valve and the top trifluoromethanesulfonyl fluoride and ammonia gas inlet regulating valve of the horizontal tubular reactor 4.

[0077] B3. By controlling the mass flow ratio of the above substances to 7:4:1 through the regulating valve, 91g of trifluoromethanesulfonyl fluoride and 22.8g of ammonia are continuously introduced into the horizontal tubular reactor 4. Theoretically, 88.6g of trifluoromethanesulfonamide should be produced.

[0078] B4. After running for a cumulative 60-70 hours, stop the intake reaction and clean the ammonium fluoride from filter assembly 6.

[0079] B5. The product was weighed in the downstream solvent recovery unit area and the weight was 83.0g. The conversion rate of this batch was calculated to be 93.7%.

[0080] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An apparatus for preparing trifluoromethanesulfonamide, characterized in that: It includes a horizontal tubular reactor (4), a spiral assembly (5) disposed in the horizontal tubular reactor (4), a raw material air inlet disposed at the upper part of the horizontal tubular reactor (4), a liquid inlet (3) disposed at the lower part of the horizontal tubular reactor (4), and a filter assembly (6) disposed at the discharge port of the horizontal tubular reactor (4). The raw material inlet is connected to a mixing pipeline (7), and a trifluoromethanesulfonyl fluoride inlet (1) and an ammonia inlet (2) are connected to the mixing pipeline (7).

2. The apparatus for preparing trifluoromethanesulfonamide according to claim 1, characterized in that: The horizontal tubular reactor (4) includes a tube (401) with a reaction chamber. The tube (401) is provided with a partition plate (402) arranged radially therein. The partition plate (402) divides the reaction chamber into a stirring chamber (403) and a conveying chamber (404). The partition plate (402) is provided with a through hole (405) connecting the stirring chamber (403) and the conveying chamber (404).

3. The apparatus for preparing trifluoromethanesulfonamide according to claim 2, characterized in that: The spiral assembly (5) includes a drive unit (501) and a spiral shaft (502) disposed at the power output end of the drive unit (501). The spiral shaft (502) extends along the axial direction of the tube body (401) and passes through the partition plate (402). A stirring blade (503) is provided on the spiral shaft (502) located in the stirring chamber (403). A plurality of stirring blades (503) are evenly distributed on the spiral shaft (502) around the circumference. A spiral plate (504) is provided on the spiral shaft (502) located in the conveying chamber (404). The conveying direction of the spiral plate (504) is towards one end of the discharge port.

4. The apparatus for preparing trifluoromethanesulfonamide according to claim 3, characterized in that: The trifluoromethanesulfonyl fluoride inlet (1), ammonia inlet (2), and liquid inlet (3) are all equipped with flow meters and regulating valves.

5. The apparatus for preparing trifluoromethanesulfonamide according to claim 4, characterized in that: The pipe body (401) is horizontally arranged on the ground, and the discharge port is located at the end of the pipe body (401). The discharge port is connected to the filter assembly (6) through the discharge pipe (8).

6. The apparatus for preparing trifluoromethanesulfonamide according to claim 5, characterized in that: The filter assembly (6) includes a filter tank (601) with a cavity, a spray section (602) communicating with the discharge pipe (8) inside the filter tank (601), and a first screen (603) and a second screen (604) located below the spray section (602).

7. The apparatus for preparing trifluoromethanesulfonamide according to claim 6, characterized in that: The first screen (603) includes a first mesh size of 50-100 μm, and the second screen (604) includes a second mesh size of 20-50 μm.

8. The apparatus for preparing trifluoromethanesulfonamide according to claim 7, characterized in that: The filter tank (601) is provided with an intermediate plate (606), which is located between the first screen (603) and the second screen (604). The intermediate plate (606) has downward flow holes. A first screening chamber (607) is formed between the first screen (603) and the intermediate plate (606), and a second screening chamber (605) is formed between the intermediate plate (606) and the lower part of the filter tank (601).

9. The apparatus for preparing trifluoromethanesulfonamide according to claim 8, characterized in that: A pressure tank (9) is provided between the first screening chamber (607) and the second screening chamber (605). The inlet of the pressure tank (9) is connected to the first screening chamber (607) through a liquid inlet pipe, and the outlet of the pressure tank (9) is connected to the side of the second screen (604) through a liquid outlet pipe (10).

10. The apparatus for preparing trifluoromethanesulfonamide according to claim 9, characterized in that: The second screen (604) includes a plurality of screen layers (6041), and a plurality of second mesh openings are evenly distributed on the screen layers (6041); The second mesh includes a second hole (6042) and a third hole (6043); The second hole (6042) in the upper layer is staggered with the third hole (6043) in the adjacent layer; A guide plate (6044) is provided between the second hole (6042) in the upper layer and the third hole (6043) in the adjacent layer. One end of the guide plate (6044) abuts against the second hole (6042) in the upper layer, and the other end extends into the two adjacent third holes (6043) in the lower layer.

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