Continuous reaction equipment for preparing dimethyl sulfoxide

Abstract

The present invention provides a continuous reaction device for preparing dimethyl sulfoxide, comprising a first storage tank, a second storage tank, a microreactor and a collection reaction tank. The first storage tank can hold dimethyl sulfide. The first storage tank is provided with a first discharge pipeline. The second storage tank can hold hydrogen peroxide. The second storage tank is provided with a second discharge pipeline, and the second discharge pipeline is provided with a plurality of branch pipelines. The microreactor has a flow reaction channel, and one end of the flow reaction channel is connected to the first discharge pipeline and one of the branch pipelines. The microreactor is provided with a plurality of auxiliary feeding ports arranged at intervals along the transmission path of the flow reaction channel, and each auxiliary feeding port is connected to each other branch pipeline in a one-to-one correspondence. The collection reaction tank is connected to the other end of the flow reaction channel. The continuous reaction device for preparing dimethyl sulfoxide provided by the present invention realizes multi-point feeding, can disperse reaction heat, can also adjust material ratio, ensure reaction effect, and has strong practicality.

Description

Technical Field

[0001] This invention belongs to the technical field of mixed reaction devices, specifically relating to a continuous reaction device for the preparation of dimethyl sulfoxide. Background Technology

[0002] Dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound with high polarity, high boiling point, good thermal stability, aprotic properties, and water miscibility. It is soluble in most organic compounds such as ethanol, propanol, benzene, and chloroform, and can be used as an organic solvent, reaction medium, and intermediate in organic synthesis. DMSO is also used as a dyeing solvent for synthetic fibers, a pesticide additive, an antifreeze agent, a metal paint remover, a degreasing agent, a capacitor dielectric, a rare metal extractant, and a sulfur dioxide absorbent. The preparation of DMSO typically involves the reaction of dimethyl sulfide with hydrogen peroxide, in which the dimethyl sulfide is oxidized. This reaction is mild, has a simple process route, requires low investment, and the hydrogen peroxide used reacts to produce water, causing no pollution. It is an economical, resource-efficient, and environmentally friendly process.

[0003] In existing technologies, the raw materials used in the preparation of dimethyl sulfoxide are all fluids, thus microreactors are typically employed. For example, patent application number CN202310724840.1, entitled "A Method for Preparing Dimethyl Sulfoxide Using a Microreactor," describes a process where dimethyl sulfide and hydrogen peroxide are mixed via a three-way valve and fed into a microreactor to allow for a complete reaction. However, this method involves exothermic mixing and reaction, leading to concentrated heat, temperature increases, and the potential for side reactions from excessive hydrogen peroxide, thus affecting the preparation efficiency. Summary of the Invention

[0004] This invention provides a continuous reaction apparatus for the preparation of dimethyl sulfoxide, which aims to solve the problem of poor practicality of existing reaction equipment used in the preparation of dimethyl sulfoxide.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is: to provide a continuous reaction apparatus for the preparation of dimethyl sulfoxide, comprising:

[0006] The first storage tank is used to hold dimethyl sulfide; the first storage tank is equipped with a first discharge pipeline.

[0007] The second storage tank is used to hold hydrogen peroxide; the second storage tank is equipped with a second discharge pipeline, and the second discharge pipeline is equipped with multiple branch pipelines.

[0008] The microreactor has a flow reaction channel, one end of which is connected to the first discharge pipe and one of the branch pipes; the microreactor is provided with a plurality of auxiliary feeding ports spaced apart along the conveying path of the flow reaction channel, and each of the auxiliary feeding ports is connected to each of the other branch pipes in a corresponding manner.

[0009] The collection reaction vessel is connected to the other end of the flow reaction channel.

[0010] In one possible implementation, a first delivery pump is provided on the first discharge pipeline.

[0011] In one possible implementation, each of the branch pipes is equipped with a second delivery pump.

[0012] In one possible implementation, the microreactor includes:

[0013] The micro-reaction unit is provided in multiples, and the micro-reaction units are arranged at intervals. Each micro-reaction unit has a serpentine material flow channel; an interval space is formed between any two adjacent micro-reaction units.

[0014] Multiple connecting pipes are provided, each connecting pipe corresponding to each of the interval spaces, and each connecting pipe connects the serpentine material flow channels to form the flow reaction channel;

[0015] Each of the auxiliary feeding ports is located on a portion of the connecting pipeline.

[0016] In one possible implementation, each of the micro-reaction units includes:

[0017] The outer casing has a receiving cavity, with a water inlet at the bottom and a water outlet at the top. The water inlet and the water outlet are connected to an external circulating water supply module.

[0018] An upper connecting seat is disposed in the accommodating cavity and fixedly connected to the outer shell; straight channels are respectively provided at both ends of the upper connecting seat, and an outlet pipe is provided at the top of each of the two straight channels, with each outlet pipe extending out of the outer shell from the top of the accommodating cavity; multiple first U-shaped channels are provided on the upper connecting seat;

[0019] The lower connector is disposed in the accommodating cavity and located below the upper connector, and the lower connector is provided with a plurality of second U-shaped channels;

[0020] The transmission structure is provided in multiple ways. Each transmission structure is disposed between the upper connecting seat and the lower connecting seat, and is connected to each of the first U-shaped channels, each of the second U-shaped channels and each of the straight channels, so as to form the serpentine material feeding channel in combination with each of the first U-shaped channels, each of the second U-shaped channels and each of the straight channels.

[0021] In one possible implementation, each of the transmission structures includes:

[0022] Transmission straight pipe;

[0023] Two perforated frames are provided, and the two perforated frames are spaced apart in the cavity of the straight transmission pipe;

[0024] A rotating shaft is coaxially arranged with the straight transmission tube, and the rotating shaft is rotatably mounted on the perforated frame; an agitator is spirally wound around the outer wall of the rotating shaft;

[0025] An impeller is coaxially fixed at both ends of the rotating shaft and is used to drive the rotating shaft to rotate as the mixed fluid flows.

[0026] In one possible implementation, each port of the first U-shaped channel, each port of the second U-shaped channel, and the other end of the straight channel are provided with a connecting pipe; each of the transmission straight pipes is detachably connected to each of the connecting pipes.

[0027] In one possible implementation, the agitator is made of titanium.

[0028] In one possible implementation, the collection reaction vessel includes:

[0029] The tank body has a tank cavity and a feeding port that communicates with the flow reaction channel, and a feeding port on the top;

[0030] A stirring structure is provided on the tank body and has a stirring part extending into the tank cavity.

[0031] In this implementation, the flow reaction channel in the microreactor allows for the mixing and reaction of dimethyl sulfide from the first storage tank and hydrogen peroxide from the second storage tank, ensuring effective reaction. The second discharge pipe on the second storage tank is equipped with multiple branch pipes, each connected to the flow reaction channel in the microreactor, enabling multi-point feeding. This structure disperses reaction heat, distributing the heat generated during the reaction to different areas, mitigating temperature fluctuations, and suppressing runaway. Furthermore, it allows for adjustment of the material ratio to achieve a starved reaction, reducing side reactions, ensuring optimal reaction results, and demonstrating strong practicality. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of the structure of the continuous reaction apparatus for preparing dimethyl sulfoxide provided in an embodiment of the present invention;

[0033] Figure 2 Schematic diagram of the microreactor structure in the continuous reaction apparatus for preparing dimethyl sulfoxide provided in the embodiments of the present invention. Figure 1 (Hidden outer shell);

[0034] Figure 3 This is a schematic cross-sectional view of the microreaction unit in the continuous reaction apparatus for preparing dimethyl sulfoxide provided in an embodiment of the present invention;

[0035] Figure 4 for Figure 3 The diagram shows an enlarged structural schematic of point A in the continuous reaction apparatus for the preparation of dimethyl sulfoxide.

[0036] Figure 5 Schematic diagram of the microreactor structure in the continuous reaction apparatus for preparing dimethyl sulfoxide provided in the embodiments of the present invention. Figure 2 ;

[0037] Explanation of reference numerals in the attached figures:

[0038] 10. First storage tank; 11. First discharge pipeline; 12. First conveying pump;

[0039] 20. Second storage tank; 21. Second discharge pipeline; 22. Branch pipeline; 23. Second transfer pump;

[0040] 30. Microreactor; 31. Microreactor Unit; 311. Shell; 312. Connecting Pipe; 313. Inlet; 314. Outlet; 315. Upper Connecting Seat; 316. Lower Connecting Seat; 317. First U-shaped Channel; 318. Second U-shaped Channel; 319. Conveyor Structure; 3191. Conveyor Straight Pipe; 3192. Rotating Shaft; 3193. Perforated Frame; 3194. Impeller; 3195. Stirring Unit; 32. Connecting Pipeline; 33. Auxiliary Feed Port;

[0041] 40. Reaction vessel; 41. Vessel body; 42. Stirring structure. Detailed Implementation

[0042] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0043] Please also refer to Figure 1 and Figure 2The continuous reaction apparatus for preparing dimethyl sulfoxide provided by the present invention will now be described. The continuous reaction apparatus for preparing dimethyl sulfoxide includes a first storage tank 10, a second storage tank 20, a microreactor 30, and a collection reaction tank 40. The first storage tank 10 is capable of holding dimethyl sulfide. A first discharge pipe 11 is provided on the first storage tank 10. The second storage tank 20 is capable of holding hydrogen peroxide. A second discharge pipe 21 is provided on the second storage tank 20, and multiple branch pipes 22 are provided on the second discharge pipe 21. The microreactor 30 has a flow reaction channel, one end of which is connected to the first discharge pipe 11 and one of the branch pipes 22. The microreactor 30 has multiple auxiliary feed ports 33 spaced along the conveying path of the flow reaction channel, each auxiliary feed port 33 corresponding to each of the other branch pipes 22. The collection reaction tank 40 is connected to the other end of the flow reaction channel.

[0044] The continuous reaction apparatus for preparing dimethyl sulfoxide provided in this embodiment, compared with the prior art, allows the flow reaction channel in the microreactor 30 to mix dimethyl sulfide transferred from the first storage tank 10 and hydrogen peroxide transferred from the second storage tank 20, simultaneously enabling their reaction and ensuring the reaction effect. The second discharge pipe 21 on the second storage tank 20 is equipped with multiple branch pipes 22, which are connected to the flow reaction channel in the microreactor 30, achieving multi-point feeding. This structure can disperse the reaction heat, distributing the heat generated during the reaction to different parts, mitigating temperature fluctuations, and suppressing runaway. Furthermore, it allows for adjustment of the material ratio to achieve a starved reaction, reducing the occurrence of side reactions, ensuring reaction effect, and demonstrating strong practicality.

[0045] It should be noted that for reactions with large volumes, this type of dispersed feed allows for adjustment of the feed volume ratio. For reactions with many side reactions, it can induce a starved reaction, reducing the occurrence of side reactions, and is suitable for reactions that are vigorous and exothermic.

[0046] In some embodiments, the first discharge pipe 11 described above can be as follows: Figure 2 The structure shown. See also Figure 2 A first conveying pump 12 is installed on the first discharge pipeline 11.

[0047] The first delivery pump 12 can ensure the pressure delivery of dimethyl sulfide, while also controlling the feed rate of dimethyl sulfide. It has a simple structure and strong practicality.

[0048] In this embodiment, a back pressure valve may be installed on the connecting pipe between the first discharge pipe 11 and the microreactor 30.

[0049] In some embodiments, the branch pipe 22 may be adopted as follows: Figure 2 The structure shown. See also Figure 2 Each branch pipeline 22 is equipped with a second delivery pump 23.

[0050] Each of the second delivery pumps 23 can ensure the pressure delivery of hydrogen peroxide, while also controlling the feed rate and volume ratio of hydrogen peroxide. It has a simple structure and strong practicality.

[0051] In this embodiment, a back pressure valve may be installed on the connecting pipe between the second discharge pipe 21 and the microreactor 30.

[0052] In some embodiments, the microreactor 30 described above can be employed as follows: Figure 2 The structure shown. See also Figure 2 The microreactor 30 includes microreaction units 31 and connecting pipes 32. Multiple microreaction units 31 are provided, spaced apart, and each microreaction unit 31 has a serpentine material flow channel. An interval space is formed between any two adjacent microreaction units 31. Multiple connecting pipes 32 are provided, each corresponding to one of the interval spaces, and each connecting pipe 32 connects the serpentine material flow channels to form a flow reaction channel.

[0053] Multiple micro-reaction units 31 are connected in series through connecting pipes 32, which can ensure the length of the flow reaction channel is extended. The serpentine material flow channel in each micro-reaction unit 31 can further extend the length of the flow reaction channel, thereby ensuring that the material reacts fully. At the same time, each micro-reaction unit 31 is set independently, which makes it easier to control the temperature in segments and is suitable for situations where the heat release in the front section is large and the heat release in the back section is small.

[0054] Specifically, each auxiliary feeding port 33 is located on part of the connecting pipe 32. This structure can ensure multi-point feeding of hydrogen peroxide, thereby ensuring the dispersion of reaction heat, slowing down temperature fluctuations, and ensuring the reaction effect.

[0055] It should be noted that a back pressure valve is installed on the connecting pipe 32 with the auxiliary feeding port 33. The back pressure valve is located between the inlet of the connecting pipe 32 and the auxiliary feeding port 33 to prevent reverse flow.

[0056] In some embodiments, the microreaction unit 31 described above may employ, as follows: Figure 2 , Figure 3 and Figure 5 The structure shown. See also Figure 2 , Figure 3 and Figure 5Each microreactor unit 31 includes a housing 311, an upper connecting seat 315, a lower connecting seat 316, and a transmission structure 319. The housing 311 has a receiving cavity, with an inlet 313 at the bottom and an outlet 314 at the top. The inlet 313 and outlet 314 are connected to an external circulating water supply module. The upper connecting seat 315 is disposed in the receiving cavity and fixedly connected to the housing 311. Straight channels are provided at both ends of the upper connecting seat 315, and each straight channel has an outlet pipe at its top, extending out of the housing 311 from the top of the receiving cavity. Multiple first U-shaped channels 317 are provided on the upper connecting seat 315. The lower connecting seat 316 is disposed in the receiving cavity and located below the upper connecting seat 315, and multiple second U-shaped channels 318 are provided on the lower connecting seat 316. Multiple transmission structures 319 are provided, each of which is located between the upper connecting seat 315 and the lower connecting seat 316, and is connected to each of the first U-shaped channels 317, the second U-shaped channels 318 and the straight channels, so as to form a serpentine material feeding channel in combination with each of the first U-shaped channels 317, the second U-shaped channels 318 and the straight channels.

[0057] The serpentine material flow channel formed by the interconnection of the upper connecting seat 315, the lower connecting seat 316, and the transmission structure 319 ensures an extended reaction stroke and guarantees the reaction effect. In addition, the water inlet 313 and water outlet 314 provided on the outer shell 311 ensure the circulation of warm water and guarantee a constant reaction temperature in each micro-reaction unit 31.

[0058] It should be noted that the outer casing 311 may include a cylindrical body, a top cover connected to the top flange of the cylindrical body, and a bottom cover connected to the bottom flange of the cylindrical body.

[0059] In this embodiment, the upper connecting seat 315 can be sealed to the outer casing 311 by bolts.

[0060] In another embodiment, the upper connecting seat 315 and the lower connecting seat 316 can ensure two mating split seats, as can be seen in [reference needed]. Figure 2 and Figure 3 After the two are combined and locked with bolts, a first U-shaped channel 317 and a second U-shaped channel 318 are formed.

[0061] In some embodiments, the above-described transmission structure 319 may adopt the following... Figures 3 to 4 The structure shown. See also Figures 3 to 4Each transmission structure 319 includes a transmission straight pipe 3191, a perforated frame 3193, a rotating shaft 3192, and an impeller 3194. Two perforated frames 3193 are provided, each spaced apart within the cavity of the transmission straight pipe 3191. The rotating shaft 3192 is coaxially mounted with the transmission straight pipe 3191 and rotatably mounted on the perforated frame 3193. An agitator 3195 is spirally wound around the outer wall of the rotating shaft 3192. The impeller 3194 is coaxially fixed at both ends of the rotating shaft 3192 and can drive the rotating shaft 3192 to rotate with the flow of the mixed fluid.

[0062] The fluid material passing through the straight pipe 3191 drives the impeller 3194 to rotate, which in turn drives the shaft 3192 to rotate. The agitator 3195 on the shaft 3192 stirs the fluid passing through the straight pipe 3191, achieving a stirring effect and further ensuring the full reaction of the two materials. The spirally wound agitator 3195 can also rotate with the flow of fluid, making it easier to rotate the shaft 3192 and thus ensuring the stirring effect.

[0063] Each straight transmission pipe 3191 has an inlet and an outlet, and needs to be arranged according to the direction of the fluid.

[0064] The perforated frame 3193 includes a circular plate fixed in the straight transmission pipe 3191. A rotating hole, rotatably connected to the rotating shaft 3192, is located at the axial position of the circular plate. Multiple perforations are spaced around the rotating hole. One impeller 3194 is located between two perforated frames 3193, closer to the inlet end of the frame 3193, while the other impeller 3194 is located outside the other perforated frame 3193. This structure increases the fluid velocity through perforation, ensuring that the impeller 3194 can be driven even at low flow rates, thus guaranteeing a good mixing effect. Simultaneously, as the pressure increases, the rotational speed of the rotating shaft 3192 increases, allowing for some energy utilization and preventing sudden pressure increases. This also prevents pressure changes caused by sudden increases in flow velocity, protecting the straight transmission pipe 3191.

[0065] In some embodiments, the upper connecting seat 315 and the lower connecting seat 316 may be adopted as follows: Figure 3 The structure shown. See also Figure 3 Each port of the first U-shaped channel 317, each port of the second U-shaped channel 318, and the other end of the straight channel are provided with a connecting pipe 312. Each transmission straight pipe 3191 and each connecting pipe 312 are detachably connected, which can be by thread or by flange, for easy disassembly and assembly.

[0066] For details regarding the flanges that can be installed on each connecting pipe 312 to engage with the U-shaped channel, please refer to [link / reference]. Figure 3 .

[0067] In some embodiments, the agitator 3195 may employ, for example... Figure 3 The structure shown. See also Figure 3 The stirring part 3195 is made of titanium. The titanium will rotate with the rotating shaft 3192, thus ensuring the stirring of the material and increasing the contact area with the material. As a catalyst, titanium can further ensure the reaction effect.

[0068] In some embodiments, the above-mentioned collection reaction vessel 40 may be adopted as follows: Figure 1 The structure shown. See also Figure 1 The collection reaction vessel 40 includes a vessel body 41 and a stirring structure 42. The vessel body 41 has a vessel cavity and a feed port communicating with the flow reaction channel, and a feeding port at the top. The stirring structure 42 is disposed on the vessel body 41 and has a stirring part extending into the vessel cavity.

[0069] Tank 41 can ensure the receipt and storage of the reacted materials. In addition, if there is an excess of hydrogen peroxide, dimethyl sulfide can be added into tank 41 to allow the remaining hydrogen peroxide to react again.

[0070] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A continuous reaction device for preparing dimethyl sulfoxide, characterized in that: include: A first storage tank is used to hold dimethyl sulfide; the first storage tank is provided with a first discharge pipeline; A second storage tank is used to hold hydrogen peroxide; the second storage tank is provided with a second discharge pipeline, and the second discharge pipeline is provided with a plurality of branch pipelines; A microreactor, having a flow reaction channel, one end of which is connected to the first discharge pipeline and one of the branch pipelines; the microreactor is provided with a plurality of auxiliary feeding ports arranged at intervals along the transmission path of the flow reaction channel, and each of the auxiliary feeding ports is connected to each of the other branch pipelines in a one-to-one correspondence; the microreactor comprises a microreaction unit and a connecting pipeline; the microreaction unit is provided with a plurality of microreaction units, each of which is arranged at intervals, and each of the microreaction units has a serpentine feeding channel; an interval space is formed between any two adjacent microreaction units; the connecting pipeline is provided with a plurality of connecting pipelines, and each of the connecting pipelines is connected to each of the interval pipelines; The spaces correspond one to one, and each of the connecting pipelines connects the serpentine material channels to form the flow reaction channel; each of the auxiliary feeding ports is located on part of the connecting pipelines; each of the micro-reaction units includes an outer shell, an upper connecting seat, a lower connecting seat and a transmission structure; the outer shell has a accommodating cavity, a water inlet is provided at the bottom of the outer shell, and a water outlet is provided at the top, and the water inlet and the water outlet are connected to an external circulating water supply module; the upper connecting seat is arranged in the accommodating cavity and is fixedly connected to the outer shell; straight channels are respectively provided at both ends of the upper connecting seat, and outlet pipes are provided at the tops of the two straight channels, and each outlet The tube extends out of the shell at the top of the accommodating cavity; a plurality of first U-shaped channels are arranged on the upper connecting seat; the lower connecting seat is arranged in the accommodating cavity and is located below the upper connecting seat, and a plurality of second U-shaped channels are arranged on the lower connecting seat; a plurality of transmission structures are provided, each of which is arranged between the upper connecting seat and the lower connecting seat, and is connected one by one with each of the first U-shaped channels, each of the second U-shaped channels and each of the straight channels, so as to form the serpentine material feeding channel in combination with each of the first U-shaped channels, each of the second U-shaped channels and each of the straight channels; each of the transmission structures includes a transmission straight pipe, a porous frame, a rotating shaft and Impeller; two porous frames are provided, and the two porous frames are arranged at intervals in the tube cavity of the transmission straight pipe; the porous frame is a circular plate, provided with a rotating hole for rotationally connecting the rotating shaft, and a plurality of punching holes are arranged at intervals around the rotating hole; the rotating shaft is coaxially arranged with the transmission straight pipe, and the rotating shaft is rotatably arranged on the porous frame; a stirring part is spirally wound on the outer wall of the rotating shaft; the impellers are coaxially fixed at both ends of the rotating shaft, and are used to drive the rotating shaft to rotate with the flow of the mixed fluid; one of the impellers is located between the two porous frames and close to the porous frame at the inlet end, and the other impeller is located on the outside of the other porous frame; A collection reaction tank is connected to the other end of the flow reaction channel.

2. The continuous reaction equipment for preparing dimethyl sulfoxide according to claim 1, characterized in that: The first discharge pipeline is provided with a first delivery pump.

3. The continuous reaction equipment for preparing dimethyl sulfoxide according to claim 1, characterized in that: Each of the branch pipelines is provided with a second delivery pump.

4. The continuous reaction equipment for preparing dimethyl sulfoxide according to claim 1, characterized in that: Each port of the first U-shaped channel, each port of the second U-shaped channel and the other end of the straight channel are provided with a butt joint pipe; each of the transmission straight pipes is detachably connected to each of the butt joint pipes.

5. The continuous reaction equipment for preparing dimethyl sulfoxide according to claim 1, characterized in that: The stirring part is made of titanium.

6. The continuous reaction equipment for preparing dimethyl sulfoxide according to claim 1, characterized in that: The collection reaction tank comprises: The tank body has a tank cavity, a feeding port connected to the flow reaction channel, and a feeding port on the top; The stirring structure is arranged on the tank body and has a stirring portion extending into the tank cavity.

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