Microchannel reaction device and method for matching solution thereof

By using multiple tandem reaction chips and a swirling mixing structure in a microchannel reaction device, the problem of impurity control in the synthesis of ε-caprolactone was solved, achieving efficient mixing and precise reaction, reducing impurity content, and improving production efficiency and product purity.

CN115869869BActive Publication Date: 2025-12-30CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202111141721.0
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

Existing microchannel reaction technology presents challenges in controlling impurity levels during the preparation of ε-caprolactone, affecting product selectivity, increasing separation costs, and hindering large-scale production.

Method used

Multiple reaction chips connected in series are used, each chip is equipped with a fluid reaction channel and a swirling mixing structure. Combined with temperature and pressure control devices, the swirling mixing structure enables graded reaction and efficient mixing of materials, shortens the length of the fluid reaction channel, and reduces the amount of raw materials used and the residence time.

Benefits of technology

It achieves precise reaction, reduces the content of residual impurities in crude products, improves raw material utilization efficiency, simplifies subsequent separation processes, and enhances product purity and production efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to the field of micro-channel device, disclose a kind of micro-channel reaction device and the method of its proportioning solution.The micro-channel reaction device includes multiple reaction chips, the inside of each reaction chip is equipped with fluid reaction channel, the inside of each fluid reaction channel is spaced apart and equipped with multiple cyclone mixing structure, and each reaction chip is connected with temperature regulating device and pressure regulating device.The proportioning solution method includes the following steps: each fluid reaction channel is filled with solvent as inert medium;Reaction substrate and oxidizing agent enter into fluid reaction channel through the most upstream inlet channel, and after mixing reaction through cyclone mixing structure, flow to the next stage fluid reaction channel;Reaction system continues to carry out mixing reaction in the next stage fluid reaction channel, mixes reaction system with newly introduced oxidizing agent through cyclone mixing structure, and the reaction product after mixing flows into the next stage fluid reaction channel downstream, and so on, until the reaction product flows out through outlet channel.
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Description

Technical Field

[0001] This invention relates to the field of microchannel devices, and more specifically to a microchannel reaction device and a method for preparing solutions thereon. Background Technology

[0002] Microchannel technology refers to process enhancement techniques that utilize three-dimensional process fluid channels with characteristic dimensions at the micrometer level to perform chemical reactions, heat exchange, mixing, and separation. It can significantly improve heat and mass transfer efficiency and space utilization, achieve precise control of reaction conditions, and possess inherent safety. In recent years, microchannel reaction technology has experienced rapid development in the fields of fine chemicals and pharmaceutical chemicals. Due to its ability to achieve efficient conversion and continuous production, microchannel reaction technology offers significant advantages and broad application prospects compared to traditional batch reactor processes for the synthesis of fine chemicals with severe thermal effects. Many complex reaction processes exist in fine chemicals, and the production processes of many high-value-added fine chemical products involve multiple processes such as heat transfer, mixing, reaction, and separation. Precise control of the product production process through microchannel reactors can significantly improve the atom economy and economic added value of the process.

[0003] ε-Caprolactone is a typical high-value-added fine chemical, primarily used in the production of polycaprolactone, a biodegradable high-end medical material. However, the subsequent production process of polycaprolactone requires strict control over the impurity content in the crude caprolactone. Chinese invention patent CN103539770A discloses a microchannel reaction technology for preparing ε-caprolactone based on the oxidation of cyclohexanone with peracetic acid; Chinese invention patent CN106279093A discloses a microchannel reaction technology for preparing ε-caprolactone based on the oxidation of cyclohexanone with m-chloroperoxybenzoic acid. Both processes achieve efficient mixing and reaction in heterogeneous systems, but they lack specific measures for controlling impurity content, affecting the selectivity of the final product and increasing subsequent separation costs, posing a challenge for large-scale production. Summary of the Invention

[0004] To solve the above-mentioned technical problems, or at least partially solve them, the present invention provides a microchannel reaction device and a method for preparing the solution.

[0005] This invention provides a microchannel reaction device, comprising multiple reaction chips connected in series. Each reaction chip has a fluid reaction channel inside, with one outlet channel and at least two inlet channels. The outlet channel of the fluid reaction channel is connected to one of the inlet channels of another fluid reaction channel downstream of it. Each fluid reaction channel has multiple swirling mixing structures spaced apart inside. Each reaction chip is connected to a temperature regulating device for regulating its internal temperature and a pressure regulating device for regulating its internal pressure.

[0006] Preferably, the swirling mixing structure includes multiple menisci with different phases disposed inside the fluid reaction channel, with the multiple menisci arranged alternately.

[0007] Preferably, the meniscus is periodically circulated at phases of 0°, 45°, 90°, 135°, 180°, 225°, 270° and 315° to form a swirling mixing structure.

[0008] Preferably, the plane of the meniscus is inclined at an angle of 15-75° toward the direction of fluid flow.

[0009] Preferably, the distance between two adjacent menisci is 500-50000 μm.

[0010] Preferably, the length of each swirl mixing structure is 5-10 cm, and the distance between two adjacent swirl mixing structures is 0.5-2 m.

[0011] Preferably, the temperature control device is a heat exchange chip, and at least one heat exchange chip is attached to the side of each reaction chip. The heat exchange chip has a heat exchange channel inside, and the heat exchange channel 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, and the through-plate channel is connected to the adjacent reaction chip.

[0012] Preferably, multiple heat exchange chips and multiple reaction chips are stacked alternately, and the connection between the through-plate channel and the reaction chip and the connection between the through-plate channel and the heat exchange chip are pressed and sealed. The sealing material is one or more of polytetrafluoroethylene, EPDM rubber, perfluororubber, and graphite.

[0013] Preferably, the materials of the reaction chip and the heat exchange chip are one or more of glass, metal and ceramic.

[0014] The present invention also provides a method for preparing solutions using the above-mentioned microchannel reaction device, comprising the following steps:

[0015] The solvent is used as an inert medium to fill each fluid reaction channel, and the temperature and pressure of the reaction chip are adjusted to the set value by a temperature control device and a pressure control device.

[0016] The liquid substrate and liquid oxidant enter the fluid reaction channel through the upstream inlet channel at the same volume flow rate, and after being mixed and reacted by the swirling mixing structure, they flow into the downstream secondary fluid reaction channel.

[0017] The reaction system continues to mix and react in the secondary fluid reaction channel. New oxidant liquid phase raw materials are introduced through the secondary inlet channel and the reaction system is mixed with the newly introduced oxidant liquid phase raw materials through the swirling mixing structure. The mixed reaction products flow into the downstream secondary fluid reaction channel, and so on, until the reaction products flow out through the outlet channel.

[0018] The technical solution provided by the embodiments of the present invention has the following advantages compared with the prior art:

[0019] The microchannel reaction device provided by this invention utilizes a multi-stage reaction chip to achieve graded reaction behavior of materials and segmented feeding, reducing the amount of raw materials used and increasing the reaction rate. By setting a swirling mixing structure, efficient mixing of materials can be achieved at a lower pressure drop, and the length of the fluid reaction channel can be shortened, reducing the residence time of easily decomposed materials in the reaction channel, greatly improving the utilization efficiency of raw materials, thereby achieving precise reaction and reducing the content of residual impurities in the crude product. Attached Figure Description

[0020] 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.

[0021] 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.

[0022] Figure 1 This is a schematic diagram of the microchannel reaction device according to an embodiment of the present invention;

[0023] Figure 2 This is a schematic diagram of the primary reaction chip described in an embodiment of the present invention;

[0024] Figure 3 This is a schematic diagram of the secondary reaction chip described in an embodiment of the present invention;

[0025] Figure 4 This is a schematic diagram of the heat exchange chip according to an embodiment of the present invention;

[0026] Figure 5 This is a schematic diagram of the swirling mixing structure described in an embodiment of the present invention.

[0027] Explanation of reference numerals in the attached figures

[0028] 1. Primary reaction chip; 2. Secondary reaction chip; 3. Fluid reaction channel; 4. First inlet channel; 5. Second inlet channel; 6. Third inlet channel; 7. Outlet channel; 8. Swirl mixing structure; 81. Meniscus; 9. Heat exchange chip; 91. Heat exchange channel; 92. Heat exchange fluid inlet; 93. Heat exchange fluid outlet; 94. Through-plate channel; Detailed Implementation

[0029] 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.

[0030] 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.

[0031] Combination Figures 1 to 3 As shown, the microchannel reaction device provided in this embodiment of the invention includes multiple reaction chips connected in series. The shape of the reaction chips is not limited and can be set according to actual needs. The thickness of the reaction chips is preferably 1-2 cm. Each reaction chip has a fluid reaction channel 3 inside. To increase the residence time of the fluid, the fluid reaction channel 3 adopts a disc-shaped structure, and the spiraling method of the fluid reaction channel 3 is not limited, as long as space is utilized reasonably. The fluid reaction channel 3 has one outlet channel 7 and at least two inlet channels. The outlet channel 7 of the fluid reaction channel 3 is connected to one of the inlet channels of another fluid reaction channel 3 downstream of it. For ease of description and understanding, the upstream reaction chip is referred to as the primary reaction chip 1, and the other reaction chips are referred to as secondary reaction chips 2. Figure 2 As shown, the primary reaction chip 1 preferably has two inlet channels, each used to introduce different raw materials. Figure 3 As shown, the secondary reaction chip 2 preferably has three inlet channels. One of the inlet channels of the uppermost secondary reaction chip 2 is connected to the outlet channel 7 of the primary reaction chip 1. The remaining inlet channels are used to introduce oxidant, allowing the oxidant to be filled in stages, thus increasing the reaction efficiency. During use, 2-10 secondary reaction chips 2 are used, preferably 4-6. The liquid holding capacity of the reaction chip is 6-60 ml, preferably 18-48 ml, and more preferably 24-36 ml.

[0032] Combination Figure 2 and Figure 3As shown, each fluid reaction channel 3 is internally equipped with multiple swirling mixing structures 8 at intervals. These swirling mixing structures 8 accelerate the mixing speed and reaction rate of the materials, increasing the raw material conversion rate. Each reaction chip is connected to a temperature regulating device for adjusting its internal temperature and a pressure regulating device for adjusting its internal pressure, thereby regulating the temperature and pressure of the reaction chip to set values ​​to facilitate smooth reaction. Both the fluid reaction channel 3 and the swirling mixing structures 8 are formed internally using high-precision laser processing technology to ensure structural accuracy.

[0033] In some embodiments, the inlet channel of the primary reaction chip 1 is a first inlet channel 4, the length of which is 1-5 cm, preferably 2-4 cm, and the mechanical diameter is 500-2000 μm, preferably 800-1000 μm. The outlet channel 7 has a length of 1-2 cm and a hydraulic diameter of 500-2000 μm, preferably 800-1000 μm; the fluid reaction channel 3 has a length of 1-10 m, preferably 4-6 m, and a hydraulic diameter of 200-800 μm, preferably 400-600 μm. The included angle between the two inlet channels of the primary reaction chip 1 is 30-120°, preferably 45-90°, to facilitate the entry and mixing of raw materials.

[0034] The inlet channel of the secondary reaction chip 2, which connects to the outlet channel 7, is a second inlet channel 5. The length of the second inlet channel 5 is 1-5 cm, preferably 2-3 cm, and its hydraulic diameter is 500-2000 μm, preferably 800-1000 μm. The remaining two inlet channels are third inlet channels 6. The length of the third inlet channel 6 is 3-6 cm, preferably 4-5 cm, and its hydraulic diameter is 500-2000 μm, preferably 800-1000 μm. The included angle between the two third inlet channels 6 is 15-90°, preferably 30-60°. Further optimized, the included angle between the two third inlet channels 6 and the second inlet channel 5 is the same. The length of the outlet channel 7 is 1-2 cm, and its hydraulic diameter is 500-2000 μm, preferably 800-1000 μm. The length of the fluid reaction channel 3 is 1-10m, preferably 4-6m, and the hydraulic diameter is 200-800μm, preferably 400-600μm.

[0035] The microchannel reaction device provided by this invention utilizes a multi-stage reaction chip to achieve graded reaction behavior of materials and segmented feeding, reducing the amount of raw materials used and increasing the reaction rate. By setting a swirling mixing structure 8, efficient mixing of materials can be achieved at a lower pressure drop, and the length of the fluid reaction channel 3 can be shortened, reducing the residence time of easily decomposed materials in the reaction channel, greatly improving the utilization efficiency of raw materials, thereby achieving precise reaction and reducing the content of residual impurities in the crude product.

[0036] In some implementations, such as Figure 5 As shown, the swirling mixing structure 8 includes multiple menisci 81 with different phases disposed inside the fluid reaction channel 3, and the multiple menisci 81 are arranged alternately. Specifically, the menisci 81 are periodically circulated and discharged according to phases of 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° to form the swirling mixing structure 8. The plane of the menisci 81 forms a certain angle with the axis of the fluid reaction channel 3; specifically, the angle of inclination of the plane of the menisci 81 toward the fluid flow direction is 15-75°, preferably 30-60°. The distance between two adjacent menisci 81 is 500-50000 μm, preferably 1000-2000 μm. The length of each swirling mixing structure 8 is 5-10 cm, preferably 6-8 cm, and the distance between two adjacent swirling mixing structures 8 is 0.5-2 m, preferably 1-1.5 m.

[0037] Combination Figure 1 and Figure 4 As shown, the temperature control device is a heat exchange chip 9. At least one heat exchange chip 9 is attached to the side of each reaction chip. The heat exchange chip 9 has an internal heat exchange channel 91, which has a heat exchange fluid inlet 92 and a heat exchange fluid outlet 93. Both the heat exchange fluid inlet 92 and the heat exchange fluid outlet 93 are connected to a through-plate channel 94, which communicates with the adjacent reaction chip. By setting up the heat exchange chips 9, heat exchange is achieved in the reaction chips, thereby heating them to the set temperature. Simultaneously, by setting up the through-plate channel 94, the heat exchange medium can flow into the interior of the reaction chip, directly contacting the outside of the fluid reaction channel 3, increasing the heat exchange effect and efficiency.

[0038] The heat exchange channel 91 is formed internally using high-precision laser processing technology, increasing its accuracy. The thickness of the heat exchange chip 9 is preferably 2-4 cm. The materials of the reaction chip and the heat exchange chip 9 are one or more selected from glass, metal, and ceramic. Preferably, they are selected from one or more selected from glass, and more preferably, they are selected from one or more selected from borosilicate glass and quartz.

[0039] The lengths of the heat exchange fluid inlet 92 and outlet 93 are 1-5 cm, preferably 2-3 cm, and the hydraulic diameters are 1-12 mm, preferably 6-8 cm. The length of the heat exchange channel 91 is 0.4-1.2 m, preferably 0.8-1.0 m, and the width is 1-6 cm, preferably 2-3 cm. The hydraulic diameter of the through-plate channel 94 is 500-2000 μm, preferably 800-1000 μm. The liquid holding capacity of the heat exchange chip 9 is 10-200 ml, preferably 30-150 ml, and more preferably 48-96 ml.

[0040] like Figure 1As shown, multiple heat exchange chips 9 and multiple reaction chips are alternately stacked. The connections between the through-plate channel 94 and the reaction chip, as well as the connections between the through-plate channel 94 and the heat exchange chip 9, are press-sealed. The sealing material is one or more of polytetrafluoroethylene, EPDM rubber, perfluororubber, and graphite, thereby ensuring the airtightness of the entire system. This design effectively reduces the volume of the microchannel reactor, saving space. In use, the heat exchange medium flows in through the heat exchange fluid inlet 92. Part of the heat exchange medium flows to the heat exchange channel 91 and through the heat exchange fluid outlet 93, while another part flows into the interior of the reaction chip through the through-plate channel 94 and then out through another through-plate channel 94, thus realizing the heat exchange process.

[0041] In some embodiments, borosilicate glass is used to fabricate the reaction chip and heat exchange chip 9, wherein the reaction chip is 1.5 cm thick and the heat exchange chip 9 is 3 cm thick. Five reaction chips and four heat exchange chips 9 are alternately stacked, and the interfaces are sealed with perfluororubber rings. After tightening, a microchannel reaction device is formed. The five reaction chips include one primary reaction chip 1 and four secondary reaction chips 2.

[0042] The first inlet channel 4 of the primary reaction chip 1 has a length of 3 cm and a hydraulic diameter of 1000 μm. The included angle between the two first inlet channels 4 is 60°. The outlet channel 7 of the primary reaction chip 1 has a length of 1 cm and a hydraulic diameter of 1000 μm. The fluid reaction channel 3 of the primary reaction chip 1 has a length of 5 m and a hydraulic diameter of 500 μm.

[0043] The second inlet channel 5 and the third inlet channel 6 of the secondary reaction chip 2 are 4 cm in length and have a hydraulic diameter of 1000 μm. The included angle between the second inlet channel 5 and the third inlet channel 6 is 45°. The outlet channel 7 and the fluid reaction channel 3 of the secondary reaction chip 2 are the same in size as those of the primary reaction chip 1.

[0044] The menisci 81 in the fluid reaction channel 3 are arranged alternately. The menisci 81 are arranged in groups of eight with phases of 0°, 45°, 90°, 135°, 180°, 225°, 270° and 315°, and are periodically circulated. The plane of the menisci 81 is at a certain angle to the axis of the fluid reaction channel 3. The plane of the menisci 81 is tilted at an angle of 55° towards the direction of fluid flow. The distance between two adjacent menisci 81 is 2000μm. The length of each swirling mixing structure 8 is 8cm, and the distance between two adjacent swirling mixing structures 8 is 1m.

[0045] The heat exchange fluid inlet 92 and outlet 93 are 3 cm long and have a hydraulic diameter of 6 mm. The through-plate channel 94 has a hydraulic diameter of 1000 μm. The heat exchange channel 91 is 1 m long and 3 cm wide.

[0046] The present invention also provides a method for preparing solutions using the above-mentioned microchannel reaction device, comprising the following steps:

[0047] Step S1: Fill each fluid reaction channel 3 with a solvent as an inert medium, and adjust the temperature and pressure of the reaction chip to the set value by a temperature control device and a pressure control device. The solvent is preferably one or more of acetone, ethyl acetate, ethyl propionate, and propionic acid.

[0048] In step S2, the liquid substrate and liquid oxidant enter the fluid reaction channel 3 through the upstream inlet channel at equal volume flow rates. After being mixed and reacted by the swirling mixing structure 8, they flow into the downstream secondary fluid reaction channel 3. Specifically, the liquid substrate and liquid oxidant enter the fluid reaction channel 3 through two first inlet channels 4 to react.

[0049] In step S3, the reaction system continues to mix and react in the secondary fluid reaction channel 3. New oxidant liquid phase raw materials are introduced through the secondary inlet channel. The reaction system and the newly introduced oxidant liquid phase raw materials are efficiently mixed by the swirling mixing structure 8 and reacted in the fluid reaction channel 3. The mixed reaction products flow into the downstream secondary fluid reaction channel 3, and so on, until the reaction products flow out through the outlet channel 7.

[0050] The above methods can be applied to liquid-liquid mixture reactions, and can be specifically used to synthesize ε-caprolactone.

[0051] Specifically, the reactants in the primary reaction chip enter the fluid reaction channel 3 of the secondary reaction chip 2 through the second inlet channel 5, and the fresh oxidant liquid phase raw material enters the fluid reaction channel 3 through the third inlet channel 6. The reactants and the fresh oxidant liquid phase raw material are in focused contact in the fluid reaction channel 3, and are mixed and reacted by swirling mixing structure 8. Finally, they enter the next secondary reaction chip 2 through the outlet channel 7, and so on.

[0052] In some embodiments, propionic acid is used as an inert medium to fill each fluid reaction channel 3, and the temperature and pressure of the reaction chip are adjusted to set values ​​by temperature and pressure regulating devices. The inert medium circulates between units, and the flow rate is controlled by a mass flow meter to the required flow rate for the reaction. Cyclohexanone and 20% perpropionic acid solution enter the fluid reaction channel 3 through two first inlet channels 4 at equal volume flow rates for contact. After efficient mixing by the swirl mixing structure 8, the mixture reacts in the fluid reaction channel 3 and finally flows to the secondary reaction chip 2 through the outlet channel 7. The reaction system continues to mix and react in the secondary fluid reaction channel 3. The reactants in the primary reaction chip enter the fluid reaction channel 3 of the secondary reaction chip 2 through the second inlet channel 5, and fresh 20% perpropionic acid solution enters the fluid reaction channel 3 through the third inlet channel 6. Specifically, the total input of fresh 20% perpropionic acid solution is consistent with that of the primary reaction chip and enters the fluid reaction channel 3 in proportion through the two third inlet channels 6. After the three materials come into contact, they are efficiently mixed through the swirling mixing structure 8 and then react in the fluid reaction channel 3. Finally, they flow out through the outlet channel 7 into the next secondary reaction chip 2. After undergoing the above process three more times in the secondary reaction chips 2, the synthesis of caprolactone is completed, and crude caprolactone is obtained at the downstream outlet channel 7 of the microchannel reactor. Liquid chromatography analysis showed that the cyclohexanone conversion rate was 99.8%, the caprolactone selectivity was 99.5%, and the crude caprolactone contained 0.24% residual cyclohexanone and 0.5% residual peroxypropionic acid.

[0053] 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.

[0054] 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 microchannel reactor apparatus, characterized by, The reaction chip comprises a plurality of reaction chips connected in series, each of the reaction chips is internally provided with a fluid reaction channel (3), the fluid reaction channel (3) has an outlet channel (7) and at least two inlet channels, the outlet channel (7) of the fluid reaction channel (3) is communicated with one of the inlet channels of another fluid reaction channel (3) downstream of the fluid reaction channel (3), and a plurality of rotational flow mixing structures (8) are arranged at intervals in the interior of each of the fluid reaction channels (3), and each of the reaction chips is connected with a temperature adjusting device for adjusting the temperature in the interior of the reaction chip and a pressure adjusting device for adjusting the pressure in the interior of the reaction chip; The rotational flow mixing structure (8) comprises a plurality of menisci (81) with different phases arranged in the interior of the fluid reaction channel (3), the plurality of menisci (81) are arranged alternately, the plane of the meniscus (81) is arranged at an angle with the axis of the fluid reaction channel (3), and the menisci (81) are arranged periodically in the phases of 0°, 45°, 90°, 135°, 180°, 225°, 270° and 315° to form the rotational flow mixing structure (8).

2. The microchannel reaction apparatus according to claim 1, wherein The angle at which the plane of the meniscus (81) is inclined to the fluid flow direction is 15-75°.

3. The microchannel reaction apparatus according to claim 1, wherein The distance between two adjacent menisci (81) is 500-50000 μm.

4. The microchannel reaction apparatus according to claim 1, wherein The length of each of the rotational flow mixing structures (8) is 5-10 cm, and the distance between two adjacent rotational flow mixing structures (8) is 0.5-2 m.

5. The microchannel reaction apparatus according to any one of claims 1 to 4, characterized by The temperature adjusting device is a heat exchange chip (9), at least one heat exchange chip (9) is attached to the side surface of each of the reaction chips, the interior of the heat exchange chip (9) is provided with a heat exchange channel (91), the heat exchange channel (91) has a heat exchange fluid inlet (92) and a heat exchange fluid outlet (93), the heat exchange fluid inlet (92) and the heat exchange fluid outlet (93) are connected with a through-plate channel (94), and the through-plate channel (94) is communicated with the adjacent reaction chip.

6. The microchannel reaction apparatus according to claim 5, wherein A plurality of heat exchange chips (9) and a plurality of reaction chips are alternately superimposed, the connection between the through-plate channel (94) and the reaction chip and the connection between the through-plate channel (94) and the heat exchange chip (9) are compression sealed, and the sealing material is one or more of polytetrafluoroethylene, ethylene-propylene-diene rubber, perfluorinated rubber and graphite.

7. The microchannel reaction apparatus according to claim 5, wherein The material of the reaction chip and the heat exchange chip (9) is one or more of glass, metal and ceramic.

8. A method of proportioning solutions by the microchannel reaction apparatus according to any one of claims 1 to 7, characterized by, The method comprises the following steps: Each fluid reaction channel (3) is filled with a solvent as an inert medium, and the temperature and pressure of the reaction chip are adjusted to a set value by the temperature adjusting device and the pressure adjusting device; Reaction substrate liquid raw materials and oxidant liquid raw materials enter the fluid reaction channel (3) through the most upstream inlet channel according to equal volume flow, and are mixed and reacted by the rotational flow mixing structure (8) and then flow into the next fluid reaction channel (3) downstream of the fluid reaction channel (3); The reaction system continues to mix and react in the secondary fluid reaction channel (3), new oxidizing agent liquid raw materials are introduced through the secondary inlet channel, and the reaction system is mixed with the newly introduced oxidizing agent liquid raw materials through the cyclone mixing structure (8), and the mixed reaction product flows downstream into the secondary fluid reaction channel (3). In this way, the reaction product flows out through the outlet channel (7).

Citation Information

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