An electrochemical synthesis microreactor and its preparation method and application method
By optimizing the structure of the electrochemical synthesis microreactor and the design of the separation membrane, the problems of difficulty and high cost of separation of reaction by-products are solved, and timely separation and efficient electrochemical synthesis of reaction by-products are achieved.
Patent Information
- Application Number
- CN202211584681.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-09
- Publication Date
- 2025-02-11
- Estimated Expiration
- 2042-12-09
AI Technical Summary
In electrochemical synthesis, the difficulty in separation of reaction by-products and the high cost problems lead to a large inventory of reaction liquid, excessive reaction cycle, low current efficiency and high energy consumption.
By optimizing the structure of the electrochemical synthesis micro reactor, combining the design of the insulating microchannel layer and support substrate, and the use of separation membranes, a separation chamber is formed to achieve timely separation of reaction by-products, and the reaction liquid is increased through the two-sided separation membrane. The contact area with the separation membrane improves separation efficiency.
Timely separation of reaction by-products is achieved, side reactions are suppressed, system complexity and energy consumption per unit product are reduced, and the production efficiency of the reactor and product yield are improved.
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Figure CN115928115B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of electrochemical synthesis, and in particular relates to an electrochemical synthesis microreactor and a preparation method and an application method thereof. Background Art
[0002] In electrochemical synthesis, reactants synthesize target products by gaining and losing electrons on electrode plates, without the need for the addition of oxidants and reductants. Compared with traditional organic synthesis processes, it has many advantages such as environmental friendliness, mild reaction conditions, and flexible reaction start and stop. Studies have shown that in electrochemical synthesis, reactants usually react only within a very thin layer of liquid film on the surface of the electrode. Therefore, traditional electrochemical reactors need to continuously circulate the reaction solution through the electrode plates to reach the specified conversion rate. The resulting material backmixing increases the reaction residence time accordingly, and even requires multi-stage electrolysis to complete the reaction target within an acceptable time range, resulting in a large inventory of reaction solution, a long reaction cycle, low current efficiency, and high energy consumption. At the same time, in order to increase the conductivity of the reactants and inhibit the occurrence of side reactions, researchers need to select suitable electrolytes, and in the subsequent separation stage, the products need to be separated from the electrolyte, which makes the cost of organic electrolysis systems high and becomes a bottleneck restricting the development of this field.
[0003] To solve the above problems, researchers combined electrochemical reactors and microchannels, taking advantage of the large specific surface area of microchannels to strengthen the material mass transfer process, reduce concentration polarization, and greatly shorten the electrochemical reaction cycle and system liquid storage volume. At the same time, the shortened plate distance means that the reaction does not require the addition of additional conductive electrolyte, reducing the requirements for subsequent separation processes and providing a new development direction for organic electrochemical synthesis. However, researchers have found that in some scenarios of organic electrochemical synthesis, the generation of reaction by-products (such as water) has a significant adverse effect on the main reaction, especially in electrochemical synthesis microreactors. Due to the narrow spatial structure, the adverse effects of water in the microchannel on the reaction are further amplified. There are two common approaches to solving this problem: (1) adding special chemical reagents to the reaction liquid to inhibit the formation of water or directly react with water to maintain the water content within a reasonable range. Excess chemical reagents often bring about unnecessary side reactions and subsequent separation problems; (2) the reaction liquid is led out of the electrochemical synthesis microreactor, and the water-oil two-phase separation process is completed in an external container without confined space. The reaction liquid is then re-introduced into the microchannel through a delivery pump, which results in a more complicated process, increased equipment investment, and usually causes material back-mixing, resulting in a decrease in electrolysis efficiency and an increase in reaction time and energy consumption per unit product.
[0004] Therefore, how to quickly remove the reaction by-products precipitated in the electrochemical synthesis microreactor, improve the single-pass conversion rate of the reaction solution, and reduce backmixing has become a technical problem that needs to be solved urgently by those skilled in the art. Summary of the invention
[0005] In view of the problems existing in the prior art, the purpose of the present invention is to provide an electrochemical synthesis microreactor and a preparation method and an application method thereof. The electrochemical synthesis microreactor optimizes the structure of the electrochemical synthesis microreactor to solve the problems of difficulty in separating reaction by-products and high cost in the prior art, realizes the timely separation of by-products in the electrochemical reaction, and has low investment cost, simple preparation method and good application prospect.
[0006] To achieve this object, the present invention adopts the following technical solutions:
[0007] In a first aspect, the present invention provides an electrochemical synthesis microreactor, the electrochemical synthesis microreactor comprising an insulating microchannel layer, and an electrode sheet, an insulating gasket and a supporting substrate symmetrically arranged from inside to outside with respect to the insulating microchannel layer;
[0008] The insulating microchannel layer and the support substrate are independently provided with horizontally outwardly protruding and matching support ears on the same side;
[0009] A separation membrane is independently sandwiched between the ear portion of the insulating microchannel layer and the ear portion of each supporting substrate;
[0010] Grooves are independently arranged inside the ear portions of the support substrate, and the grooves, the separation membrane and the ear portions of the insulating microchannel layer form a cavity for temporarily storing the separated reaction by-products.
[0011] In the present invention, the insulating gasket is made of a polymer insulating material and has good electrical insulation, elasticity and weather resistance.
[0012] The following are preferred technical solutions of the present invention, but are not intended to be limitations of the technical solutions provided by the present invention. Through the following technical solutions, the technical objectives and beneficial effects of the present invention can be better achieved and realized.
[0013] As a preferred technical solution of the present invention, the thickness of the insulating microchannel layer is 100-1000μm, for example, 100μm, 200μm, 300μm, 400μm, 500μm, 600μm, 700μm, 800μm, 900μm or 1000μm, but is not limited to the listed values, and other unlisted values within the numerical range are also applicable.
[0014] As a preferred technical solution of the present invention, the insulating microchannel layer is provided with a liquid phase inlet, a front serpentine microchannel, a separation microchannel, a rear serpentine microchannel and a liquid phase outlet which are connected in sequence, and the separation microchannel is located at the branch ear part of the insulating microchannel layer.
[0015] Exemplarily, the liquid phase inlet, the front serpentine microchannel, the separation microchannel, the rear serpentine microchannel and the liquid phase outlet on the insulating microchannel layer are all engraved on the corresponding plate by laser.
[0016] Preferably, the width of the front serpentine microchannel, the separation microchannel and the rear serpentine microchannel are each independently 50-500 μm, for example, 50 μm, 100 μm, 150 μm, 200 μm, 250 μm, 300 μm, 350 μm, 400 μm, 450 μm or 500 μm, etc., but are not limited to the listed values, and other unlisted values within the numerical range are also applicable.
[0017] In the present invention, the overall length of the microchannel is determined according to the residence time required for the reaction, and the widths of various types of microchannels are preferably the same.
[0018] As a preferred technical solution of the present invention, the material of the insulating microchannel layer includes any one of PVC, PTFE, PEEK, PDMS or PMMA.
[0019] As a preferred technical solution of the present invention, the electrode sheet includes one plate-type positive electrode sheet and one plate-type negative electrode sheet.
[0020] In the present invention, the material of the electrode sheet can be selected from titanium, stainless steel or graphite according to the experimental requirements, and a suitable material such as platinum, ruthenium, cadmium or iridium can be plated on the surface of the sheet to achieve the reaction.
[0021] Preferably, each of the electrode sheets is independently provided with a power connection portion protruding horizontally outward.
[0022] As a preferred technical solution of the present invention, the grooves of the ear portions of the support substrate are each independently provided with a support structure for supporting the separation membrane and achieving the sealing effect of the separation microchannel, thereby extending the service life of the separation membrane.
[0023] As a preferred technical solution of the present invention, one side of the groove of the ear portion of the support substrate is independently provided with an air inlet hole, and the other side is independently provided with a liquid discharge hole, preferably on opposite sides.
[0024] In the present invention, the drainage process is achieved by blowing gas into the groove.
[0025] As a preferred technical solution of the present invention, the separation membrane includes a hydrophilic and oleophobic separation membrane.
[0026] In the present invention, the hydrophilic-oleophobic separation membrane is a polymer hydrophilic-oleophobic separation membrane, which has the functions of water passing and oil separating, can allow the water in the reaction liquid to penetrate into the groove of the ear portion of the supporting substrate, and prevent the entry of the oil phase reaction liquid, thereby realizing the dehydration process of the reaction liquid.
[0027] In a second aspect, the present invention provides a method for preparing the electrochemical synthesis microreactor according to the first aspect, the preparation method comprising:
[0028] The insulating microchannel layer, the electrode sheet, the insulating gasket, the supporting substrate and the separation membrane are combined and then extruded through an extrusion device.
[0029] Preferably, the extrusion equipment comprises a plate-frame extrusion equipment.
[0030] In the present invention, the preparation process of the electrochemical synthesis microreactor is simple, and it can be obtained only by extrusion sealing, and is easy to disassemble without the need for screw fixation.
[0031] In the third aspect, the present invention provides an application method of the electrochemical synthesis microreactor described in the first aspect, wherein the reaction raw materials are introduced into the microchannel of the insulating microchannel layer for reaction, the reaction liquid enters the support ear of the insulating microchannel layer along the microchannel, the reaction by-products are separated by the separation membrane and enter the groove of the support ear of the supporting substrate, and the separated reaction liquid continues to flow along the microchannel to complete the electrochemical reaction.
[0032] Preferably, a protective gas is intermittently purged into the groove of the ear portion of the support substrate to discharge the reaction by-products in the groove.
[0033] In a fourth aspect, the present invention provides a method for preparing dimethyl sebacate, the preparation method being carried out using the electrochemical synthesis microreactor as described in the first aspect, the preparation method comprising:
[0034] A mixed solution of monomethyl adipate and methanol is passed into the microchannel of the insulating microchannel layer for reaction. The reaction liquid enters the ear portion of the insulating microchannel layer along the microchannel. The water generated during the reaction is separated by a hydrophilic and oleophobic separation membrane and enters the groove of the ear portion of the supporting substrate. The separated reaction liquid continues to flow along the microchannel to complete the electrochemical reaction.
[0035] Compared with the prior art, the present invention has the following beneficial effects:
[0036] (1) The electrochemical synthesis microreactor of the present invention forms a separation chamber for separating reaction by-products by optimizing the structure of the insulating microchannel layer and the supporting substrate and using a separation membrane, thereby achieving timely separation of reaction by-products and inhibiting the occurrence of side reactions without the need to add additional chemical reagents, thereby reducing the complexity of the system and the energy consumption per unit product; and the electrochemical synthesis microreactor does not require back-mixing operation, thereby improving the production efficiency of the reactor and the yield of the product;
[0037] (2) The electrochemical synthesis microreactor of the present invention also increases the contact area between the reaction solution and the separation membrane by setting up separation membranes on both sides, thereby improving the separation efficiency of reaction by-products;
[0038] (3) The electrochemical synthesis microreactor of the present invention also has a protective gas purge function, which facilitates the timely discharge of reaction by-products and reduces the amount of liquid stagnation in the groove;
[0039] (4) The electrochemical synthesis microreactor of the present invention adopts a plate structure, and the production amplification process can be achieved by stacking multiple microreactors; and there are no fasteners such as screws throughout the body, and the sealing process can be completed by commercially available plate-frame extrusion equipment. When the internal parts need to be replaced, it is convenient to disassemble and assemble, and the operation is convenient. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] Figure 1 It is a schematic diagram of the preparation process of an electrochemical synthesis microreactor provided in a specific embodiment of the present invention.
[0041] Figure 2 It is a schematic structural diagram of an insulating microchannel layer in an electrochemical synthesis microreactor provided in a specific embodiment of the present invention.
[0042] Figure 3 It is a structural schematic diagram of a positive electrode sheet and a negative electrode sheet in an electrochemical synthesis microreactor provided in a specific embodiment of the present invention.
[0043] Figure 4 It is a structural schematic diagram of a supporting substrate in an electrochemical synthesis microreactor provided in a specific embodiment of the present invention.
[0044] Figure 5 It is a structural schematic diagram of an insulating microchannel layer in an electrochemical synthesis microreactor provided in Comparative Example 1 of the present invention.
[0045] Among them, 1-insulating microchannel layer, 11-first ear, 12-liquid phase inlet, 13-front serpentine microchannel, 14-separation microchannel, 15-rear serpentine microchannel, 16-liquid phase outlet, 2-plate positive electrode piece, 3-plate negative electrode piece, e-power connection part, 4-insulating gasket, 5-support substrate, 51-second ear, 52-groove, 53-support structure, 54-air inlet, 55-drainage hole, 6-separation membrane, 7-electrochemical synthesis microreactor. DETAILED DESCRIPTION
[0046] It should be understood that, in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.
[0047] It should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "disposed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.
[0048] In a specific embodiment, the present invention provides an electrochemical synthesis microreactor, the structural schematic diagram of which is as follows Figure 1 As shown, the electrochemical synthesis microreactor 7 includes an insulating microchannel layer 1, and an electrode sheet, an insulating gasket 4 and a supporting substrate 5 which are symmetrically arranged from the inside to the outside of the insulating microchannel layer 1;
[0049] The insulating microchannel layer 1 and the supporting substrate 5 are independently provided with horizontally outwardly protruding and matching ear portions on the same side; the ear portion of the insulating microchannel layer 1 is a first ear portion 11, and the ear portion of the supporting substrate 5 is a second ear portion 51;
[0050] A separation membrane 6 is independently sandwiched between the first ear portion 11 of the insulating microchannel layer 1 and the second ear portion 51 of each of the supporting substrates 5;
[0051] The inner sides of the second ear portions 51 of the support base plate 5 are independently provided with grooves 52 .
[0052] Furthermore, the thickness of the insulating microchannel layer 1 is 100-1000 μm.
[0053] Furthermore, the insulating microchannel layer 1 is provided with a liquid phase inlet 12, a front serpentine microchannel 13, a separation microchannel 14, a rear serpentine microchannel 15 and a liquid phase outlet 16 which are connected in sequence, and the separation microchannel 14 is located at the first branch ear 11 of the insulating microchannel layer 1.
[0054] Furthermore, the widths of the front serpentine microchannel 13, the separation microchannel 14 and the rear serpentine microchannel 15 are independently 50-500 μm.
[0055] Furthermore, the material of the insulating microchannel layer 1 includes any one of PTFE, PEEK, PDMS or PMMA.
[0056] Furthermore, the electrode sheet includes a plate-type positive electrode sheet 2 and a plate-type negative electrode sheet 3 .
[0057] Furthermore, each of the electrode sheets is independently provided with a power connection portion e protruding horizontally outward.
[0058] Furthermore, each groove 52 of the second ear portion 51 of the support substrate 5 is independently provided with a support structure 53 for supporting the separation membrane 6 .
[0059] Furthermore, one side of the groove 52 of the second ear portion 51 of the supporting substrate 5 is independently provided with an air inlet hole 54 , and the other side is independently provided with a liquid discharge hole 55 .
[0060] Furthermore, the separation membrane 6 includes a hydrophilic-oleophobic separation membrane or an oleophilic-hydrophobic separation membrane.
[0061] Based on the electrochemical synthesis microreactor 7 in the specific embodiment, the preparation process includes: stacking the support substrate 5, the insulating gasket 4, the plate-type negative electrode sheet 3, the separation membrane 6, the insulating microchannel layer 1, the plate-type positive electrode sheet 2, the separation membrane 6, the insulating gasket 4 and the support substrate 5 in sequence, and then extruding them through a plate-frame extrusion device. The specific stacking process is as follows: Figure 1 shown.
[0062] The structural schematic diagram of the insulating microchannel layer 1 is as follows: Figure 2 As shown, the schematic diagram of the structure of the plate-type positive electrode sheet 2 and the plate-type negative electrode sheet 3 is as shown Figure 3 As shown, the structural schematic diagram of the supporting substrate 5 is as shown Figure 4 shown.
[0063] Furthermore, the separation membrane 6 used in the following embodiments is a hydrophilic and oleophobic separation membrane, specifically a PVDF membrane modified by copolymerization of 3-aminopropyltriethoxysilane multi-walled carbon nanotubes and dopamine.
[0064] The following are typical but non-limiting embodiments of the present invention:
[0065] Embodiment 1:
[0066] This embodiment provides an electrochemical synthesis microreactor, based on the electrochemical synthesis microreactor 7 in the specific embodiment, wherein:
[0067] The insulating microchannel layer 1 has a thickness of 500 μm, a length of 15 cm, and a width of 10 cm. The total length of the engraved microchannel is about 300 cm.
[0068] The widths of the front serpentine microchannel 13, the separation microchannel 14 and the rear serpentine microchannel 15 are all 200 μm;
[0069] The insulating microchannel layer 1 is made of polymethyl methacrylate (PMMA);
[0070] The electrode sheets are a plate-type positive electrode sheet 2 (made of titanium) and a plate-type negative electrode sheet 3 (made of titanium).
[0071] Application Example 1:
[0072] This application example provides an application method of the electrochemical synthesis microreactor as described in Example 1, wherein the electrochemical synthesis microreactor 7 is used in the electrochemical synthesis of dimethyl sebacate, specifically comprising:
[0073] A methanol solution containing 40 wt % of monomethyl adipate was introduced into the insulating microchannel layer 1 from the liquid phase inlet 12 at a speed of 5.0 mL / min using a precision injection pump, and a voltage of 10 V was applied. The reaction solution entered the separation microchannel 14 through the front serpentine microchannel 13. The byproduct water generated during the reaction passed through the polymer super-hydrophilic and oleophobic separation membrane into the groove 52 of the second ear 51 of the supporting substrate 5. The separated reaction solution entered the rear serpentine microchannel 15 to continue the reaction. During the reaction, nitrogen was purged into the groove 52 for 0.5 min every 5 min to discharge the water in the groove 52. After the entire reaction was run for 3 days, the reaction solution was taken out from the liquid phase outlet 16 for analysis.
[0074] Embodiment 2:
[0075] This embodiment provides an electrochemical synthesis microreactor, based on the electrochemical synthesis microreactor 7 in the specific embodiment, wherein:
[0076] The insulating microchannel layer 1 has a thickness of 100 μm, a length of 15 cm, and a width of 10 cm. The total length of the engraved microchannel is about 300 cm.
[0077] The widths of the front serpentine microchannel 13, the separation microchannel 14 and the rear serpentine microchannel 15 are all 50 μm;
[0078] The insulating microchannel layer 1 is made of PEEK;
[0079] The electrode sheets are a plate-type positive electrode sheet 2 (stainless steel 304L) and a plate-type negative electrode sheet 3 (stainless steel 304L cadmium-plated).
[0080] Embodiment 3:
[0081] This embodiment provides an electrochemical synthesis microreactor, based on the electrochemical synthesis microreactor 7 in the specific embodiment, wherein:
[0082] The insulating microchannel layer 1 has a thickness of 1000 μm, a length of 15 cm, a width of 10 cm, and a total length of the engraved microchannel of about 300 cm;
[0083] The widths of the front serpentine microchannel 13, the separation microchannel 14 and the rear serpentine microchannel 15 are all 500 μm;
[0084] The insulating microchannel layer 1 is made of PTFE;
[0085] The electrode sheets are a plate-type positive electrode sheet 2 (platinum-plated titanium) and a plate-type negative electrode sheet 3 (stainless steel 304L).
[0086] Embodiment 4:
[0087] This embodiment provides an electrochemical synthesis microreactor, based on the electrochemical synthesis microreactor 7 in the specific embodiment, wherein:
[0088] The insulating microchannel layer 1 has a thickness of 800 μm, a length of 15 cm, a width of 10 cm, and a total length of the engraved microchannel of about 300 cm;
[0089] The widths of the front serpentine microchannel 13, the separation microchannel 14 and the rear serpentine microchannel 15 are all 300 μm;
[0090] The insulating microchannel layer 1 is made of PMMA;
[0091] The electrode sheets are a plate-type positive electrode sheet 2 (graphite) and a plate-type negative electrode sheet 3 (graphite).
[0092] Comparative Example 1:
[0093] This comparative example provides an electrochemical synthesis microreactor. The electrochemical synthesis microreactor 7 refers to the electrochemical synthesis microreactor 7 in Example 1, except that: the insulating microchannel layer 1 and the supporting substrate 5 are not provided with ear parts, nor are separation membranes 6. In this comparative example, the specific structural schematic diagram of the insulating microchannel layer 1 is as shown in FIG. Figure 5 shown.
[0094] Comparative Application Example 1:
[0095] This comparative application example provides an application method of the electrochemical synthesis microreactor as described in Comparative Example 1, wherein the electrochemical synthesis microreactor 7 is used in the electrochemical synthesis of dimethyl sebacate, specifically comprising:
[0096] A methanol solution containing 40 wt % of monomethyl adipate was introduced into the insulating microchannel layer 1 from the liquid phase inlet 12 at a rate of 5.0 mL / min using a precision syringe pump, and a voltage of 10 V was applied. After the entire reaction was run for 3 days, the reaction liquid was taken out from the liquid phase outlet 16 for analysis.
[0097] The reaction solutions in Application Example 1 and Comparative Example 1 were analyzed using a high performance liquid chromatography analyzer to measure the water content and the content of the side reaction products in the final reaction solutions. The results are shown in Table 1.
[0098] Table 1
[0099] Water content / wt% Side reaction product content / wt% Application Example 1 0.91 0.23 Comparative application example 1 2.90 0.57
[0100] During the electrochemical synthesis of dimethyl sebacate, there are strict requirements for the water content in the reaction solution, and the water content generally needs to be strictly limited to between 0.1-2wt%. The increase in water content during the reaction will lead to an increase in the content of by-products such as methyl valerate and methyl 6-hydroxycaproate, which are easily attached to the electrode surface, easily leading to inactivation of the electrode surface, decreased conductivity, decreased current efficiency, reduced product yield, and increased energy consumption.
[0101] By comparing Application Example 1 and Comparative Application Example 1, it can be seen that the present invention can timely separate the water generated in the reaction process through the optimized design of the electrochemical synthesis microreactor structure, thereby improving the single-pass conversion rate of the reactor. After the reaction is run for 3 days, the water content is reduced by about 70%, and the content of by-products such as methyl valerate and methyl 6-hydroxyhexanoate is reduced by 50%, indicating that the present electrochemical synthesis microreactor has a good inhibitory effect on suppressing side reactions involving water.
[0102] The present invention illustrates the structure and detailed method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned structure and detailed method, that is, it does not mean that the present invention must rely on the above-mentioned structure and detailed method to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the operation of the present invention, addition of auxiliary operations, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims
1. An electrochemical synthesis microreactor for synthesizing dimethyl sebacate, characterized in that: The electrochemical synthesis microreactor comprises an insulating microchannel layer, and an electrode sheet, an insulating gasket and a supporting substrate which are symmetrically arranged from the inside to the outside of the insulating microchannel layer; The insulating microchannel layer and the support substrate are independently provided with horizontally outwardly protruding and matching support ears on the same side; A separation membrane is independently sandwiched between the ear portion of the insulating microchannel layer and the ear portion of each supporting substrate; The separation membrane comprises a hydrophilic-oleophobic separation membrane or an oleophilic-hydrophobic separation membrane; Grooves are independently arranged inside the ear portions of the support base plate.
2. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The thickness of the insulating microchannel layer is 100-1000 μm.
3. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The insulating microchannel layer is provided with a liquid phase inlet, a front serpentine microchannel, a separation microchannel, a rear serpentine microchannel and a liquid phase outlet which are connected in sequence, and the separation microchannel is located at the branch ear portion of the insulating microchannel layer.
4. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 3, characterized in that: The widths of the front serpentine microchannel, the separation microchannel and the rear serpentine microchannel are each independently 50-500 μm.
5. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The material of the insulating microchannel layer includes any one of PVC, PTFE, PEEK, PDMS or PMMA.
6. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The electrode sheets include a plate-type positive electrode sheet and a plate-type negative electrode sheet.
7. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The electrode sheets are each independently provided with a power connection portion protruding horizontally outward.
8. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: The grooves of the ear portions of the support substrate are each independently provided with a support structure for supporting the separation membrane.
9. The electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to claim 1, characterized in that: One side of the groove of the ear portion of the support substrate is independently provided with an air inlet hole, and the other side is independently provided with a liquid discharge hole.
10. A method for preparing an electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to any one of claims 1 to 9, characterized in that: The preparation method comprises: The insulating microchannel layer, the electrode sheet, the insulating gasket, the supporting substrate and the separation membrane are combined and then extruded through an extrusion device.
11. The preparation method according to claim 10, characterized in that: The extrusion equipment includes a plate-frame extrusion equipment.
12. An application method of the electrochemical synthesis microreactor for synthesizing dimethyl sebacate according to any one of claims 1 to 9, characterized in that: The application method comprises: The reaction raw materials are introduced into the microchannels of the insulating microchannel layer for reaction, and the reaction liquid enters the ear portion of the insulating microchannel layer along the microchannel. The reaction by-products are separated by the separation membrane and enter the groove of the ear portion of the supporting substrate. The separated reaction liquid continues to flow along the microchannel to complete the electrochemical reaction.
13. The application method according to claim 12, characterized in that: The protective gas is intermittently purged into the groove of the support ear portion of the support substrate to discharge the reaction byproducts in the groove.
14. A method for preparing dimethyl sebacate, characterized in that: The preparation method is carried out using an electrochemical synthesis microreactor for synthesizing dimethyl sebacate as described in any one of claims 1 to 9, and the preparation method comprises: A mixed solution of monomethyl adipate and methanol is passed into the microchannel of the insulating microchannel layer for reaction. The reaction liquid enters the ear portion of the insulating microchannel layer along the microchannel. The water generated during the reaction is separated by a hydrophilic and oleophobic separation membrane and enters the groove of the ear portion of the supporting substrate. The separated reaction liquid continues to flow along the microchannel to complete the electrochemical reaction.
Citation Information
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