Continuous channel reaction device and method for preparing solution thereof

By combining the mixing and separation modules of the continuous channel reaction device with microchannel technology and centrifugal separation, the problems of environmental pollution and high cost in the production of methyl mercaptoacetate have been solved, and efficient and stable product preparation has been achieved.

CN115869870BActive Publication Date: 2025-12-30CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202111142811.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-09-28
Publication Date
2025-12-30
Estimated Expiration
2041-09-28

AI Technical Summary

Technical Problem

The existing production process for methyl mercaptoacetate has serious environmental pollution, significant safety hazards, uncontrollable product quality, lengthy process flow, and high equipment costs. In addition, the reliance on imported raw materials leads to high production costs.

Method used

The device employs a continuous channel reaction apparatus, including a mixing reaction module and a reaction separation module. It utilizes a micron-scale mixing reaction module and a centimeter-scale reaction separation module, combined with microchannel technology to achieve the coupling of material mixing, reaction and separation. A spring mixing structure promotes liquid mixing, centrifugal force is used to achieve oil-water separation, and a heat exchange module is used for temperature control.

Benefits of technology

This has resulted in improved product quality stability, shortened preparation processes, reduced equipment and environmental costs, increased reaction efficiency, and enabled green and environmentally friendly continuous production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to the technical field of process intensification, and discloses a continuous channel reaction device and a method for preparing a solution by using the same. The reaction device comprises a mixing reaction module and a reaction separation module. The mixing reaction module has a fluid mixing reaction channel inside, and a plurality of mixing structures are arranged in the fluid mixing reaction channel at intervals. The reaction separation module comprises a fluid reaction separation channel, and the fluid reaction separation channel is communicated with the fluid mixing reaction channel. The method for preparing the solution comprises the following steps: filling the fluid mixing reaction channel and the fluid reaction separation channel with a first liquid-phase raw material as a medium, and adjusting the temperature and pressure of the device to a set value; introducing a second liquid-phase raw material, so that the second liquid-phase raw material is contacted with the first liquid-phase raw material, and then the second liquid-phase raw material is mixed and reacted through the mixing structures, and the reaction product flows into the reaction separation module; the reaction product continues to react in the fluid reaction separation channel, and is separated under the action of centrifugal force, so that an oil-phase product and an aqueous-phase product are obtained.
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Description

Technical Field

[0001] This invention relates to the field of process intensification technology, and more specifically to a continuous channel reaction apparatus and a method for preparing solutions therefrom. Background Technology

[0002] Methyl mercaptoacetate (MGA) is an important fine chemical and a derivative of the mercaptoacetic acid series. It is a crucial intermediate in the synthesis of pesticides, pharmaceuticals, tobacco flavorings, and food flavorings. In the pesticide field, MGA is an intermediate in the synthesis of the pesticide thifensulfuron. In the pharmaceutical field, MGA can be used to synthesize methyl 5-chloro-2-carboxylate-3-methylaminosulfonylthiophene, an intermediate for the nonsteroidal anti-inflammatory drug articaine hydrochloride. MGA can also be used to synthesize heat stabilizers for plastics, such as organotin heat stabilizers for PVC.

[0003] Currently, the main synthetic methods for methyl mercaptoacetate (MGA) use mercaptoacetic acid and methanol as raw materials, supplemented by a catalyst. Industrially, concentrated sulfuric acid is commonly used as a catalyst, as it is inexpensive, readily available, and has high catalytic efficiency, but it poses serious environmental pollution and safety hazards. Regarding MGA synthesis technology: my country only began researching the synthesis methods of MGA and its derivatives in the 1970s, resulting in relatively lagging research, outdated production processes, and significant environmental pollution. Furthermore, the high price of raw material mercaptoacetic acid, with partial reliance on imports, leads to high production costs. Given the deficiencies in domestic MGA production processes regarding product yield and reactant recovery, relevant domestic enterprises are now strengthening their research in this field. Chinese invention patent CN101580485A discloses a method for producing MGA, which improves catalytic efficiency by using p-toluenesulfonic acid as an activator, thereby increasing product yield and purity. However, this method still has obvious shortcomings: First, it uses a batch reactor process for production, and the product quality is uncontrollable between batches; second, the use of sulfuric acid as a catalyst and the introduction of p-toluenesulfonic acid as an auxiliary agent increase the safety risks and environmental pollution of the system; finally, in order to obtain high-purity methyl mercaptoacetate, a complex separation and purification process is required, which is lengthy and has high equipment and operating costs. Summary of the Invention

[0004] To solve the above-mentioned technical problems, or at least partially solve them, the present invention provides a continuous channel reaction apparatus and a method for preparing solutions thereon.

[0005] This invention provides a continuous channel reaction apparatus, comprising:

[0006] The mixing reaction module has an internal fluid mixing reaction channel with two first inlet channels and one first outlet channel. The internal spaced fluid mixing reaction channel is provided with multiple mixing structures for mixing the liquids.

[0007] The reaction separation module includes a disc-shaped fluid reaction separation channel with a second inlet channel and at least two second outlet channels. The second inlet channel is located in the middle of the reaction separation module and is used to communicate with the first outlet channel. After the liquid is centrifuged through the fluid reaction separation channel, it flows out through the multiple second outlet channels.

[0008] Preferably, the mixing structure is a spring mixing structure, which includes a plurality of springs spaced apart along the length of the fluid mixing reaction channel. The axial direction of the springs is perpendicular to the length of the fluid mixing reaction channel, and the diameter of the springs gradually decreases along their axial direction.

[0009] Preferably, the spring mixing structure is positioned within the fluid mixing reaction channel via a positioning groove, and the distance between any two adjacent spring mixing structures is 0.5-5 cm.

[0010] Preferably, the fluid mixing reaction channel has a disc-shaped structure, with two first inlet channels located on the outer periphery of the mixing reaction module, and a first outlet channel located in the middle of the fluid mixing reaction channel, and the positions of the first outlet channel and the second inlet channel being opposite.

[0011] Preferably, the two first inlet channels are positioned opposite each other, and the line connecting the two first inlet channels is aligned with the radial direction of the mixing reaction module.

[0012] Preferably, there are two second outlet channels, which are arranged side by side along the radial direction of the reaction separation module. The second outlet channel on the outer side is the oil phase product outlet channel, and the second outlet channel on the inner side is the aqueous phase product outlet channel.

[0013] Preferably, the inner side of the fluid reaction separation channel is provided with a hydrophilic and oleophobic layer.

[0014] Preferably, it also includes a temperature control device, which is a heat exchange module, and at least one heat exchange module is attached to the side of both the mixing reaction module and the reaction separation module.

[0015] Preferably, there are three heat exchange modules, which are spaced apart. The mixing reaction module and the reaction separation module are respectively located between two adjacent heat exchange modules. The heat exchange module has a heat exchange channel inside, which has a heat exchange fluid inlet and a heat exchange fluid outlet. Both the heat exchange fluid inlet and the heat exchange fluid outlet are connected to a through-plate channel, which is connected to the adjacent mixing reaction module or reaction separation module.

[0016] The present invention also provides a method for preparing a solution using the above-described continuous channel reaction apparatus, comprising the following steps:

[0017] Using a first liquid raw material as a medium, the first liquid raw material is introduced into the first inlet channel at the end and fills the fluid mixing reaction channel and the fluid reaction separation channel, and the temperature and pressure of the mixing reaction module and the reaction separation module are adjusted to the set value;

[0018] The second liquid raw material is introduced through another first inlet channel, so that it comes into contact with the first liquid raw material in the fluid mixing reaction channel, and reacts after being mixed through the mixing structure. The reaction product flows into the reaction separation module.

[0019] The reaction products continue to react within the fluid reaction separation channel, and during the flow inside the fluid reaction separation channel, the reaction products are separated under the action of centrifugal force, and then oil phase products and aqueous phase products are obtained at the two second outlet channels respectively.

[0020] The technical solution provided by the embodiments of the present invention has the following advantages compared with the prior art:

[0021] The continuous channel reaction device provided by this invention connects a micrometer-scale mixing reaction module and a centimeter-scale reaction separation module in series, achieving coupling of the mixing, reaction, and separation processes. Utilizing microchannel technology, it enables precise control of material mixing, reaction, and separation, significantly improving reaction efficiency and product quality. Furthermore, it allows for continuous production, ensuring product quality stability while drastically reducing the preparation process. The preparation process also boasts high atom economy and is entirely green and environmentally friendly, significantly reducing equipment, environmental, and safety costs. Attached Figure Description

[0022] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0023] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 This is a schematic diagram of the mixing reaction module according to an embodiment of the present invention;

[0025] Figure 2 This is a schematic diagram of the reaction separation module described in an embodiment of the present invention;

[0026] Figure 3 This is a schematic diagram of the heat exchange module according to an embodiment of the present invention;

[0027] Figure 4 This is a schematic diagram of the spring hybrid structure described in an embodiment of the present invention.

[0028] Explanation of reference numerals in the attached figures

[0029] 1. Mixing reaction module; 11. Fluid mixing reaction channel; 12. First inlet channel; 13. First outlet channel; 2. Spring mixing structure; 21. Spring; 3. Reaction separation module; 31. Fluid reaction separation channel; 32. Second inlet channel; 33. Oil phase product outlet channel; 34. Aqueous phase product outlet channel; 4. Heat exchange module; 41. Heat exchange fluid inlet; 42. Heat exchange fluid outlet; 43. Through-plate channel. Detailed Implementation

[0030] To better understand the above-mentioned objectives, features, and advantages of the present invention, the solutions of the present invention will be further described below. It should be noted that, unless otherwise specified, the embodiments and features of the present invention can be combined with each other.

[0031] The following description sets forth many specific details in order to provide a full understanding of the invention, but the invention may also be practiced in other ways different from those described herein; obviously, the embodiments described in the specification are only some, not all, of the embodiments of the invention.

[0032] Combination Figure 1 and Figure 2 As shown, the continuous channel reaction device provided in this embodiment of the invention includes a mixing reaction module 1 and a reaction separation module 3.

[0033] like Figure 1As shown, the mixing reaction module 1 has a fluid mixing reaction channel 11 inside. The fluid mixing reaction channel 11 has two first inlet channels 12 and one first outlet channel 13. Multiple mixing structures for mixing liquids are spaced apart inside the fluid mixing reaction channel 11. The two first inlet channels 12 are used to introduce different liquid phase raw materials, allowing the two liquid phase raw materials to contact, mix, and react within the fluid mixing reaction channel 11. The mixing structures enhance the mixing effect of the two liquid phase raw materials, making the reaction faster. Furthermore, by setting the mixing structures, the liquid mixes and reacts more quickly within the unit size of the fluid mixing reaction channel 11, thus meeting the reaction requirements without requiring an excessively long fluid mixing reaction channel 11, effectively shortening the size of the fluid mixing reaction channel 11 and reducing the space occupied. The mixing reaction module 1 includes two circular plates, upper and lower. Both circular plates are formed with identical surface grooves through high-precision machining and then sealed together to form a micron-level fluid mixing reaction channel 11.

[0034] Specifically, the fluid mixing reaction channel 11 has a disc-shaped structure. This disc shape is achieved by bending the fluid mixing reaction channel 11 into a ring-shaped channel structure, thereby reducing space occupation and ensuring a smooth, rounded transition inside the fluid mixing reaction channel 11, avoiding local back-mixing caused by right-angle bends. Both first inlet channels 12 are located on the outer periphery of the mixing reaction module 1, meaning both first inlet channels 12 are connected to the outer ring of the fluid mixing reaction channel 11, and one of the first inlet channels 12 is connected to the end of the fluid mixing reaction channel 11. Further optimized, the two first inlet channels 12 are positioned opposite each other, and the line connecting the two first inlet channels 12 is aligned with the radial direction of the mixing reaction module 1. The first inlet channel 12 not connected to the end of the fluid mixing reaction channel 11 preferably forms a 90° tangential angle with the fluid, increasing the mixing effect. Furthermore, the first outlet channel 13 is located in the middle of the fluid mixing reaction channel 11, ensuring that the fluid flows from the outside to the inside within the fluid mixing reaction channel 11.

[0035] In some embodiments, the hydraulic diameters of the two first inlet channels 12 are 500-2000 μm, preferably 800-1000 μm. The hydraulic diameter of the first outlet channel 13 is 500-2000 μm, preferably 800-1000 μm. The maximum radius of curvature of the fluid mixing reaction channel 11 is 1-10 cm, preferably 3-6 cm, and the hydraulic diameter is 200-800 μm, preferably 400-600 μm. The liquid holding capacity of the mixing reaction module 1 is 5-50 ml, preferably 10-40 ml.

[0036] like Figure 2As shown, the reaction separation module 3 includes a disc-shaped fluid reaction separation channel 31. The disc shape refers to the channel being bent into an annular structure to reduce space occupation while allowing the fluid inside to move circumferentially. The fluid reaction separation channel 31 has a second inlet channel 32 and at least two second outlet channels. The second inlet channel 32 is located in the middle of the reaction separation module 3 and communicates with the first outlet channel 13, ensuring that the liquid moves from the inside to the outside within the fluid reaction separation channel 31. After centrifugal separation through the fluid reaction separation channel 31, the liquid flows out through multiple second outlet channels, achieving liquid separation.

[0037] There are two secondary outlet channels. The reaction products include oil and water. The two secondary outlet channels are arranged side by side along the radial direction of the reaction separation module 3. The outer secondary outlet channel is the oil phase product outlet channel 33, and the inner secondary outlet channel is the water phase product outlet channel 34. During the flow of the reaction products inside the fluid reaction separation channel 31, the oil and water are separated into layers through centrifugal force and the action of the oil-water separation surface. Finally, the oil phase and water phase products are discharged separately through the oil phase product outlet channel 33 and the water phase product outlet channel 34.

[0038] Further optimized, the inner side of the fluid reaction separation channel 31 is provided with a hydrophilic and oleophobic layer, and the inner side of the aqueous product outlet channel 34 is also provided with a hydrophilic and oleophobic layer. That is, both the inner sides of the fluid reaction separation channel 31 and the inner side of the aqueous product outlet channel 34 are coated with a hydrophilic and oleophobic film using a spraying process. The substrate material of the hydrophilic and oleophobic film is selected from one or more of titanium dioxide, silicon dioxide, and zirconium oxide, preferably titanium dioxide. Furthermore, various groups or ions are loaded onto the surface of the substrate material to achieve the hydrophilic and oleophobic effect. The loading material is selected from one or more of sodium ions, potassium ions, lithium ions, fluorine groups, chloride groups, and bromine groups, more preferably a combination of sodium ions and fluorine groups.

[0039] Further optimized, the positions of the first outlet channel 13 and the second inlet channel 32 are opposite, allowing the mixing reaction module 1 and the reaction separation module 3 to be arranged side by side, reducing the space occupied. The reaction separation module 3 includes two circular plates, one above the other. Both circular plates are formed with identical surface grooves through high-precision machining and then sealed together to form a centimeter-level fluid reaction separation channel 31.

[0040] In some embodiments, the hydraulic diameter of the second inlet channel 32 is 500-2000 μm, preferably 800-1000 μm. The maximum radius of curvature of the fluid reaction separation channel 31 is 1-10 cm in length, preferably 3-6 cm, and the hydraulic diameter is 0.5-2 cm, preferably 1-1.5 cm. The length of the two second outlet channels is 1-2 cm, and the hydraulic diameter is 0.2-1.5 cm. The liquid holding capacity of the reaction separation module 3 is 10-200 ml, preferably 30-150 ml.

[0041] The materials used for the mixing reaction module 1 and the reaction separation module 3 of the present invention are selected from one or more of glass, metal, and ceramic, preferably from one or more of metal, and more preferably from one or more of stainless steel 316L and Hastelloy C. Furthermore, the thickness of the mixing reaction module 1 and the reaction separation module 3 is 1-2 cm.

[0042] The continuous channel reaction device provided by this invention connects a micrometer-scale mixing reaction module 1 and a centimeter-scale reaction separation module 3 in series. The diameter of the fluid mixing reaction channel 11 is smaller than the diameter of the fluid reaction separation channel 31. Specifically, the diameter of the fluid mixing reaction channel 11 in the mixing reaction module 1 is on the micrometer scale. Its surface force is greater than the inertial force of the fluid, and a mixing structure is provided inside. Therefore, during the fluid flow inside, the centrifugal force is not significant, and liquid separation does not occur internally, facilitating the liquid mixing reaction. The diameter of the fluid reaction separation channel 31 in the reaction separation module 3 is on the centimeter scale. The increased size leads to increased centrifugal force, thus achieving phase separation and stratification. Therefore, the continuous channel reaction device provided by this invention achieves the coupling of mixing, reaction, and separation processes, utilizing microchannel technology to achieve precise control of material mixing, reaction, and separation, significantly improving reaction efficiency and product quality.

[0043] like Figure 4 As shown, the mixing structure is a spring mixing structure 2, which includes multiple springs 21 spaced apart along the length of the fluid mixing reaction channel 11. The axial direction of the springs 21 is perpendicular to the length of the fluid mixing reaction channel 11, and the diameter of the springs 21 gradually decreases along their axial direction. The springs 21 are micrometer-sized, with a diameter of 5-30 μm and 5-20 working turns. The spring mixing structure 2 is positioned within the fluid mixing reaction channel 11 by positioning grooves, and the distance between any two adjacent spring mixing structures 2 is 0.5-5 cm, preferably 1-2 cm. The springs 21 create disturbances in the flow field, disrupting the laminar flow structure of the fluid and generating turbulence to promote mixing.

[0044] The present invention also includes a temperature control device, which is a heat exchange module 4. At least one heat exchange module 4 is attached to the side of both the mixing reaction module 1 and the reaction separation module 3. Specifically, there are three heat exchange modules 4, spaced apart. The mixing reaction module 1 and the reaction separation module 3 are respectively positioned between two adjacent heat exchange modules 4. That is, the mixing reaction module 1 is positioned between the two heat exchange modules 4 located in the middle and at the top, and the reaction separation module 3 is positioned between the two heat exchange modules 4 located in the middle and at the bottom. Furthermore, to enable communication between the mixing reaction module 1 and the reaction separation module 3, a through hole can be formed in the middle of the heat exchange module 4 located in the middle position.

[0045] The heat exchange module 4 has an internal heat exchange channel with a heat exchange fluid inlet 41 and a heat exchange fluid outlet 42. Both the heat exchange fluid inlet 41 and the heat exchange fluid outlet 42 are connected to a through-plate channel 43, which communicates with the adjacent mixing reaction module 1 or reaction separation module 3. Preferably, the thickness of the heat exchange module 4 is 2-4 cm. By setting the heat exchange module 4, heat exchange between the mixing reaction module 1 and the reaction separation module 3 is achieved, thereby heating them to a set temperature. Simultaneously, the through-plate channel 43 allows the heat exchange medium to flow into the interior of the mixing reaction module 1 and the reaction separation module 3, directly contacting the outside of the fluid mixing reaction channel 11 and the fluid reaction separation channel 31, increasing the heat exchange effect and efficiency. This design ensures that each heat exchange module 4 has a heat exchange fluid inlet 41 and a heat exchange fluid outlet 42. The heat exchange fluid flows through the heat exchange fluid inlet 41 to the mixing reaction module 1 or the reaction separation module 3 and then flows out through the heat exchange fluid outlet 42 of the heat exchange module 4.

[0046] In addition, such as Figure 3 As shown, multiple heat exchange modules 4 can also be connected sequentially, with the top heat exchange module 4 having a heat exchange fluid inlet 41 and the bottom heat exchange module 4 having a heat exchange fluid outlet 42. The heat exchange fluid flows through the top heat exchange module 4 to the mixing reaction module 1, then to the middle heat exchange module 4, and so on, finally flowing out through the heat exchange fluid outlet 42 of the bottom heat exchange module 4, thus circulating.

[0047] This design allows the mixing reaction module 1, reaction separation module 3, and heat exchange module 4 to be stacked alternately, reducing space requirements. Furthermore, the airtightness of the system is ensured by pressing and sealing the channels during the connection process. The sealing material is selected from one or more of polytetrafluoroethylene, EPDM rubber, perfluororubber, and graphite.

[0048] In some embodiments, the hydraulic diameters of the heat exchange fluid inlet 41 and the heat exchange fluid outlet 42 are 1-12 mm, preferably 6-8 cm. The hydraulic diameter of the heat exchange channel is 1-6 cm, preferably 2-3 cm. The hydraulic diameter of the through-plate channel 43 is 500-2000 μm, preferably 800-1000 μm.

[0049] In one embodiment, the mixing reaction module 1, the reaction separation module 3, and the heat exchange module 4 are made of 316L stainless steel. The mixing reaction module 1 and the reaction separation module 3 are 2cm thick, and the heat exchange module 4 is 3cm thick. Five circular modules are stacked alternately, and each interface is sealed with a perfluororubber ring. After being tightened, a continuous channel reaction device is formed.

[0050] In the mixing reaction module 1, the hydraulic diameters of the two first inlet channels 12 are both 1000 μm. The first outlet channel 13 is 1 cm long and has a hydraulic diameter of 1000 μm. The radius of curvature of the fluid mixing reaction channel 11 is 5 cm, and its hydraulic diameter is 500 μm. In the reaction separation module 3, the radius of curvature of the fluid reaction separation channel 31 is 5 cm, and its hydraulic diameter is 1.2 cm. The width of the oil phase product outlet channel 33 is 0.8 cm, and the width of the aqueous phase product outlet channel 34 is 0.4 cm. In the heat exchange module 4, the hydraulic diameters of the heat exchange fluid inlet 41 and the heat exchange fluid outlet 42 are 6 cm, and the hydraulic diameter of the through-plate channel 43 is 1000 μm. The hydraulic diameter of the heat exchange channel is 2 cm.

[0051] The fluid mixing reaction channel 11 is embedded with a spring mixing structure 2, which includes multiple micron-sized metal springs 21 with continuously decreasing radii of curvature. The springs 21 have a diameter of 20 μm, 10 working turns, and a spacing of 1.5 cm between two adjacent spring mixing structures 2.

[0052] Both the inner side of the fluid reaction separation channel 31 and the aqueous product outlet channel 34 are treated with hydrophilic and oleophobic surfaces. A hydrophilic and oleophobic film is coated by spraying. The substrate material of the hydrophilic and oleophobic film is titanium dioxide, and the surface is loaded with sodium ions and fluorine groups to achieve efficient oil-water separation.

[0053] The present invention also provides a method for preparing a solution using the above-described continuous channel reaction apparatus, comprising the following steps:

[0054] In step S1, a first liquid raw material is introduced into the fluid mixing reaction channel 11 and the fluid reaction separation channel 31 through the first inlet channel 12 at the end, using the first liquid raw material as the medium. The temperature and pressure of the mixing reaction module 1 and the reaction separation module 3 are then adjusted to set values. Specifically, the temperature of the mixing reaction module 1 and the reaction separation module 3 can be adjusted through the heat exchange module 4 or by improving the overall working environment.

[0055] In step S2, a second liquid raw material is introduced through another first inlet channel 12, allowing it to contact the first liquid raw material in the fluid mixing reaction channel 11. The mixture then reacts with the first liquid raw material through the mixing structure, and the reaction product flows into the reaction separation module 3. Specifically, the reaction product flows into the fluid reaction separation channel 31 through the first outlet channel 13 and the second inlet channel 32.

[0056] In step S3, the reaction products continue to react within the fluid reaction separation channel 31. During the flow within the fluid reaction separation channel 31, the reaction products are separated under the action of centrifugal force, resulting in oil phase products and aqueous phase products at the two second outlet channels, respectively. Specifically, efficient oil-water two-phase separation is achieved through the combined centrifugal force and hydrophilic-oleophobic surface interaction of the annular fluid reaction separation channel 31. Finally, the products are collected through the oil phase product outlet channel 33 and the aqueous phase product outlet channel 34, respectively.

[0057] In one embodiment, taking the synthesis of methyl mercaptoacetate as an example, the synthesis method includes the following steps: methanol as a raw material is input through the first inlet channel 12 at the end and fills the entire device; the reaction environment inside the device is raised to the specified reaction temperature and pressure; methanol circulates between units and the flow rate is controlled by a mass flow meter to the required flow rate for the reaction. Mercaptoacetic acid containing 0.5% p-toluenesulfonic acid enters the mixing reaction module 1 through another first inlet channel 12 according to the stoichiometric ratio for contact; after efficient mixing by the spring mixing structure 2, it reacts in the fluid mixing reaction channel 11 and flows out through the first outlet channel 13 into the reaction separation module 3; the reaction system undergoes a reaction separation coupling process in the reaction separation module 3, achieving efficient oil-water two-phase separation through the centrifugal action of the annular fluid reaction separation channel 31 combined with the hydrophilic and oleophobic surface interaction; finally, the products are collected through the oil phase product outlet channel 33 and the aqueous phase product outlet channel 34, respectively, with methyl mercaptoacetate being the main component of the oil phase product. Gas chromatography analysis shows that the yield of methyl mercaptoacetate during the reaction is 93.5%, and the selectivity of methyl mercaptoacetate is greater than 96.8%.

[0058] The solution preparation method provided by this invention can be applied to liquid-liquid mixing reaction separation coupling processes, specifically, it can be used to synthesize methyl mercaptoacetate. Using this method to prepare the solution enables continuous production of the product, ensuring product quality stability while significantly reducing the preparation process. Furthermore, the preparation process exhibits high atom economy and is environmentally friendly throughout, greatly reducing equipment, environmental, and safety costs. In addition, multiple sets of continuous channel reaction devices can be used in parallel during operation to scale up production.

[0059] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0060] The above description is merely a specific embodiment of the present invention, enabling those skilled in the art to understand or implement the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention is not to be limited to the embodiments described herein, but is to be accorded the widest scope consistent with the principles and novel features of the invention herein.

Claims

1. A continuous channel reactor apparatus, characterized by, The application relates to a mixing and reaction device, which comprises: a mixing and reaction module (1), the inside of the mixing and reaction module (1) is provided with a fluid mixing and reaction channel (11), the fluid mixing and reaction channel (11) is provided with two first inlet channels (12) and one first outlet channel (13), a plurality of mixing structures for mixing liquid are arranged in the inside of the fluid mixing and reaction channel (11) at intervals, the mixing structure is a spring mixing structure (2), the spring mixing structure (2) comprises a plurality of springs (21) arranged at intervals along the length direction of the fluid mixing and reaction channel (11), the axis direction of the spring (21) is perpendicular to the length direction of the fluid mixing and reaction channel (11), the diameter of the spring (21) gradually decreases along the axial direction, and the fluid mixing and reaction channel (11) is in a disc structure; and a reaction and separation module (3), the reaction and separation module (3) comprises a disc-shaped fluid reaction and separation channel (31), the fluid reaction and separation channel (31) is provided with one second inlet channel (32) and two second outlet channels, the second inlet channel (32) is arranged in the middle of the reaction and separation module (3) and is used for being communicated with the first outlet channel (13), the two second outlet channels are arranged side by side along the radial direction of the reaction and separation module (3), the second outlet channel on the outer side is an oil phase product outlet channel (33), the second outlet channel on the inner side is a water phase product outlet channel (34), and liquid flows out through the two second outlet channels after being centrifugally separated in the fluid reaction and separation channel (31), wherein the two first inlet channels (12) are arranged on the outer periphery of the mixing and reaction module (1), the first outlet channel (13) is arranged in the middle of the fluid mixing and reaction channel (11), and the first outlet channel (13) is opposite to the position of the second inlet channel (32).

2. The continuous channel reaction apparatus according to claim 1, characterized by The spring mixing structure (2) is positioned in the fluid mixing and reaction channel (11) through positioning grooves, and the distance between every two adjacent spring mixing structures (2) is 0.5-5 cm.

3. The continuous channel reaction apparatus according to claim 1, wherein The two first inlet channels (12) are opposite to each other, and the line connecting the two first inlet channels (12) is consistent with the radial direction of the mixing and reaction module (1).

4. The continuous channel reaction apparatus according to claim 1, wherein The inner side of the fluid reaction and separation channel (31) is provided with a hydrophilic and oleophobic layer.

5. The continuous channel reaction apparatus according to any one of claims 1 to 4, characterized by, The device further comprises a temperature adjusting device, the temperature adjusting device is a heat exchange module (4), and at least one heat exchange module (4) is attached to the side of the mixing and reaction module (1) and the reaction and separation module (3).

6. The continuous channel reaction apparatus according to claim 5, wherein The heat exchange module (4) is three, three said heat exchange module (4) interval setting, said mixing reaction module (1) and said reaction separation module (3) are respectively arranged between two adjacent said heat exchange module (4), the inside of said heat exchange module (4) is equipped with heat exchange channel, said heat exchange channel has heat exchange fluid inlet (41) and heat exchange fluid outlet (42), said heat exchange fluid inlet (41) and said heat exchange fluid outlet (42) are connected with the through plate channel (43), said through plate channel (43) and its adjacent said mixing reaction module (1) or said reaction separation module (3) are communicated.

7. A method of producing a solution by means of the continuous channel reactor according to any one of claims 1 to 6, characterized in that, Comprising the following steps: The first liquid phase raw material is introduced from the first inlet channel (12) at the end and fills the fluid mixing reaction channel (11) and the fluid reaction separation channel (31) as a medium, and the temperature and pressure of the mixing reaction module (1) and the reaction separation module (3) are adjusted to the set value; The second liquid phase raw material is introduced through another first inlet channel (12), and is contacted with the first liquid phase raw material in the fluid mixing reaction channel (11), and is mixed and reacted after mixing through the mixing structure, and the reaction product flows into the reaction separation module (3); The reaction product continues to react in the fluid reaction separation channel (31), and during the flow in the fluid reaction separation channel (31), the reaction product is separated under the action of centrifugal force, and then the oil phase product and the water phase product are obtained at the two second outlet channels respectively.

Citation Information

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