Electrochemical polymerization reaction device

Abstract

The present invention relates to the technical field of reaction equipment, and discloses an electrochemical polymerization reaction device, including an electrochemical reaction mechanism, which includes a reaction unit and a detection unit. The reaction unit adopts a spiral reactor, and the microchannel wall is used as an electrode to ensure that the material is within the coverage range of the electric field, shorten the mass transfer distance, and improve the mass transfer efficiency. Compared with traditional reactors, this device reduces the difficulty and cost of scale-up production through modular design. The efficient mass transfer and heat transfer in the microchannel make the reaction temperature and process easier to control, reduce the defective rate, and achieve rapid reaction under mild conditions, reducing energy consumption and equipment loss. The device has a wide adaptability to different types of electrochemical polymerization reactions, and significantly improves product quality and market competitiveness. The spiral microchannel combined with the vibration function optimizes the material flow state, prevents local accumulation and enhances the mixing effect, and improves the reaction uniformity and efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of reaction equipment, and in particular to an electrochemical polymerization reaction device. Background Art

[0002] In the field of electrochemical reactions, traditional electrochemical reactors are widely used in various reactions, but there are problems such as low mass transfer efficiency and difficulty in amplification. In terms of mass transfer, the distance between electrodes of traditional electrochemical reactors is large. Taking the intermittent electrochemical reactor commonly used in laboratory organic synthesis as an example, the distance between its electrodes is long, which leads to limited mass transfer rate. The long ion migration distance prolongs the reaction time, and it is easy to cause side reactions due to insufficient concentration of reactants near the electrodes. For example, in the electrosynthesis of organic compounds, long-distance mass transfer makes the reaction efficiency low, and more impurities will be produced, increasing the cost of subsequent separation and purification; when it is necessary to scale up the laboratory-scale reaction to industrial production, simply increasing the size of the reactor will lead to aggravated mass transfer and heat transfer problems, and the use of multiple reactors in parallel makes it difficult to ensure the consistency of reaction conditions in each reactor, resulting in unstable product quality.

[0003] To solve these problems, the prior art has tried a variety of methods. For example, a flow cell equipped with large-area parallel electrodes has been developed. Although the mass transfer distance is shortened to a certain extent, the distance between the electrodes is still in the range of millimeters to centimeters, which cannot effectively control the flow of fluids, and the amplification effect is not ideal. Summary of the invention

[0004] The present invention aims to provide an electrochemical polymerization reaction device to improve the material transfer efficiency of the electropolymerization reaction and reduce the difficulty of scale-up production.

[0005] To achieve the above-mentioned purpose, the present invention adopts the following technical scheme: an electrochemical polymerization reaction device, including an electrochemical reaction mechanism, the electrochemical reaction mechanism includes a reaction unit for performing a polymerization reaction and a detection unit for detecting the reaction condition, the reaction unit includes a reactor for performing an electrochemical polymerization reaction, the reactor includes a microchannel, the microchannel is spiral and can guide the material in the microchannel by vibration.

[0006] The beneficial effects of this solution are as follows: the present application uses a microchannel as a reactor for electrochemical polymerization reaction and utilizes the channel wall of the microchannel as an electrode to ensure that the materials in the microchannel are within the coverage of the electrode electric field, thereby shortening the mass transfer distance and increasing the mass transfer efficiency.

[0007] At the same time, the special reaction principle of the reactor is used to reduce the difficulty of the scale-up process. When a traditional reactor is scaled up, whether it is simply increasing the size or using multiple reactors in parallel, it will face the problem of aggravated mass transfer and heat transfer problems and inconsistent reaction conditions. This device uses the special reaction principle of the reactor to reduce the difficulty of the scale-up process. When scaling up production, the modular design of the reactor makes the entire production system easy to build and expand. Enterprises can achieve scale expansion by simply increasing the number or modules of reactors according to production capacity requirements. There is no need to redesign and transform the structure and layout of the entire equipment on a large scale when expanding the scale, as with traditional reactors, which greatly saves time and labor costs.

[0008] In addition, due to the high mass transfer and heat transfer efficiency in the reactor, the reaction temperature and reaction progress can be better controlled during the scale-up production process. This means that in large-scale production, the product quality can be controlled more accurately and the defective rate caused by fluctuations in reaction conditions can be reduced. Compared with traditional reactors, the device of the present invention consumes less energy during the scale-up process. The efficient mass transfer of the microchannel allows the reaction to proceed quickly under milder conditions. There is no need to promote the reaction by increasing temperature, pressure and other conditions like traditional reactors, thereby reducing energy consumption and equipment loss, further reducing production costs, and improving the market competitiveness of products.

[0009] Moreover, the device has good adaptability to different types of electrochemical polymerization reactions during the amplification process. Whether it is the polymerization reaction of small molecules or the synthesis of complex macromolecules, efficient production can be achieved by adjusting the parameters and reaction conditions of the microchannel. This wide applicability enables the present invention to be effectively applied in multiple fields, such as material science, chemical production, electronic industry, etc., greatly expanding its market application scope, providing strong technical support for the technological upgrading of related industries, and having extremely high market competitiveness and commercial value. In addition, the microchannel is spiral and can guide the materials in the microchannel by vibration, further optimizing the flow state of the materials in the reactor, not only preventing the materials from being locally accumulated, but also strengthening the mixing effect between different materials, thereby further improving the uniformity and efficiency of the reaction, and bringing new technical ideas and development directions to the entire electrochemical polymerization reaction field.

[0010] Furthermore, the microchannel includes a reaction channel and an electrode, and the electrode is fixedly arranged on the inner wall of the reaction channel. By fixing the electrode on the inner wall of the reaction channel, direct connection between the electrodes can be avoided, thereby avoiding the risk of short circuit.

[0011] Furthermore, the reactor further comprises a mounting frame and a feed pump, the microchannel comprises a feed end and a discharge end, both of which are fixed on the mounting frame, and the feed pump is fixed on the mounting frame and communicated with the feed end. By mounting the feed pump on the mounting frame, the vibration of the feed pump during operation can be transmitted to the microchannel, thereby using the vibration of the feed pump during operation to guide the material in the microchannel, further optimizing the flow state of the material in the reactor.

[0012] Furthermore, the reactor further includes a temperature control unit, which includes a shell and a heat transfer medium. The shell is fixed on the mounting frame and wraps the reaction channel, and the heat transfer medium flows between the outer wall of the reaction channel and the inner wall of the shell. The reaction channel is wrapped by the shell, and the heat transfer medium flows between the outer wall of the reaction channel and the inner wall of the shell, so that the heat transfer medium performs immersion heating or cooling on the reaction channel, so as to maximize the heat transfer process in the reaction process and improve the heat transfer efficiency.

[0013] Furthermore, the temperature control unit also includes a thermostat for adjusting the temperature of the heat transfer medium flowing in the shell, and the shell is provided with a first inlet and a second inlet for the heat transfer medium to flow, and the thermostat is connected with the first inlet and the second inlet and can control the temperature of the heat transfer medium. The heat transfer medium flowing in the shell is introduced into the thermostat through the thermostat connected with the first inlet and the second inlet, so that the heat transfer medium always maintains a set temperature, thereby preventing the heat transfer medium in the shell from deviating from the set temperature, thereby maintaining the material in the microchannel to always react at the set temperature, thereby ensuring the smooth progress of the reaction.

[0014] Furthermore, the shell is a cone and includes a first shell, a second shell and a positioning connector. The feed end and the discharge end are fixedly connected to the first shell and the second shell respectively. The first shell and the positioning connector can be detachably fixed to the second shell, and the second shell is fixed to the mounting frame. The split shell design facilitates the installation of the microchannel and subsequent inspection and maintenance work. At the same time, since the shell is conical, the overall reaction channel is also conical, so that the spiral radius of the reaction channel is gradually reduced, thereby increasing the force of the reactants on the inner wall of the reaction channel, making the reaction channel vibrate more violently, and then making the material flow in the reaction channel smoother, thereby improving the mass transfer efficiency of the electropolymerization reaction and reducing the difficulty of scale-up production.

[0015] Furthermore, a second positioning column is fixed at the center of the second shell, and a first inlet and outlet and a first positioning column are provided on the positioning connector. The lower edge of the first inlet and outlet abuts against the upper edge of the first shell and seals the upper edge of the first shell. The free end of the first positioning column is threadedly connected to the free end of the second positioning column. The first positioning column and the second positioning column are both hollow tubular structures provided with a plurality of liquid inlet grooves. The second inlet and outlet are fixedly arranged at the end of the second positioning column and connected to the liquid inlet groove, and the first inlet and outlet are connected to the liquid inlet groove.

[0016] Furthermore, the electrodes include a cathode and an anode, a diaphragm is provided between the cathode and the anode for ion passage, and the diaphragm is fixedly connected to the inner wall of the reaction channel. The design of the diaphragm enhances the safety of the system and prevents short circuit or other safety hazards caused by direct contact between the electrodes.

[0017] Furthermore, the size of the reaction channel is no larger than 200 microns. Such a small-sized channel can better control the reaction conditions, improve the uniformity and efficiency of the reaction, and is particularly suitable for complex small molecule polymerization reactions and macromolecular synthesis.

[0018] In combination with the above technical features, the present application also has the following effects:

[0019] 1. Reduce the difficulty and cost of scale-up production: Compared with traditional reactors, this device reduces the difficulty and cost of scale-up production through modular design. The production capacity can be expanded by simply increasing the number of reactors or modules, without the need for large-scale redesign and transformation of equipment, which greatly saves time and labor costs; 2. Better temperature and reaction process control: The efficient mass transfer and heat transfer in the reactor make the reaction temperature and process easier to control, reduce the defective rate, and achieve rapid reaction under mild conditions, reducing energy consumption and equipment loss. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a connection diagram of an embodiment of the present invention;

[0021] Figure 2 An exploded view of the electrochemical polymerization reaction unit of Example 1 of the present invention;

[0022] Figure 3 This is a schematic diagram of the assembly of the electrochemical polymerization reaction unit housing of Example 1 of the present invention;

[0023] Figure 4 This is a schematic diagram of the internal structure of the electrochemical polymerization reaction unit microchannel of Example 1 of the present invention;

[0024] Figure 5 This is a schematic diagram of the internal structure of the electrochemical polymerization reaction unit microchannel of Example 3 of the present invention;

[0025] Figure 6Schematic diagram of the internal structure of the electrochemical polymerization reaction unit microchannel in Example 4 of the present invention. DETAILED DESCRIPTION

[0026] The following is further described in detail through specific implementation methods:

[0027] The figure marks in the drawings of the specification include: reaction unit 1, first shell 111, discharge port 112, second shell 121, second positioning column 122, feed port 123, first inlet and outlet 131, first positioning column 132, microchannel 14, reaction channel 141, electrode 142, diaphragm 143, thermostat 2, first sensor 31, second sensor 32.

[0028] Example 1

[0029] Embodiment 1 is basically as attached Figure 1-4 As shown, Figure 1-4 An electrochemical polymerization reaction device as shown includes a temperature control unit and a reaction unit 1, such as Figure 1 As shown, the temperature control unit includes a thermostat 2 and a heating medium. The thermostat 2 includes a liquid inlet pipe and a liquid outlet pipe. The heating medium circulates in the thermostat 2 through the liquid inlet pipe and the liquid outlet pipe. The thermostat 2 is equipped with a circulation pump and can maintain the set temperature of the heating medium flowing out of the liquid outlet pipe by heating or cooling.

[0030] The reaction unit 1 includes several reactors, such as Figure 2 As shown, the reactor includes a microchannel 14, a mounting frame, a feed pump and a shell. Figure 4 As shown, the microchannel 14 includes an electrode 142 and a reaction channel 141. The electrode 142 includes a cathode and an anode. The cathode and the anode are fixedly arranged on the inner wall of the reaction channel 141. The reaction channel 141 is a spiral structure including a feed end and a discharge end and an inner diameter not greater than 200 microns, so as to extend the length of the reaction channel 141 per unit area.

[0031] like Figure 2 , Figure 3As shown, the shell includes a first shell 111, a second shell 121, a positioning connector and a plurality of elastic gaskets. The first shell 111 is provided with a discharge port 112, and the second shell 121 is provided with a feed port 123. The first shell 111 and the positioning connector can be detachably fixed to the second shell 121. The second shell 121 is fixed to the mounting frame by bolts. A second positioning column 122 is fixed to the center of the second shell 121. The positioning connector is provided with a first inlet and outlet 131 and a first positioning column 132. The lower edge of the first inlet and outlet 131 abuts against the upper edge of the first shell 111 and is connected to the first inlet and outlet 131. The upper edge of the first shell 111 is sealed by an elastic gasket, the free end of the first positioning column 132 is threadedly connected to the free end of the second positioning column 122, the first positioning column 132 and the second positioning column 122 are both hollow tubular structures with a plurality of liquid inlet grooves, the second inlet and outlet are fixedly arranged at the end of the second positioning column 122 and connected to the liquid inlet groove, the first inlet and outlet 131 are connected to the liquid inlet groove, and the elastic gasket is arranged between the first shell 111 and the second shell 121 and between the upper edge of the first shell 111 and the lower edge of the first inlet and outlet 131, so as to realize the sealing work of the shell through the elastic gasket.

[0032] The first inlet and outlet 131, the second inlet and outlet, the feed port 123 and the discharge port 112 are all provided with sealing connectors, which include sealing components and threaded connectors. The liquid inlet pipe and the liquid outlet pipe are connected to the first inlet and outlet 131 and the second inlet and outlet through the sealing connectors to form a heat transfer cycle. The feed pump is connected to the feed port 123 through the sealing connector to pump the monomer and the solution into the reactor for reaction. After the reaction is completed, the monomer and the solution are discharged from the discharge port 112 for subsequent treatment. The connection methods of the first inlet and outlet 131, the feed port 123 and the discharge port 112 are substantially the same. In this embodiment, a plurality of gaps are provided at the free ends of the feed port 123, the discharge port 112 and the first inlet and outlet 131. Taking the connection of the feed port 123 as an example, when connecting, first, the feed end is passed through the feed port 123, and then, the sealing member is sleeved between the microchannel 14 and the feed port 123. Finally, the threaded connector is threadedly connected to the feed port 123 and the inner wall of the threaded connector is used to press the free end of the feed port 123, so that the free end of the feed port 123 undergoes elastic deformation, thereby pressing the sealing member to complete the sealed connection effect.

[0033] The connection method of the second inlet and outlet is generally the same as that of the sealing connector. The difference is that the second inlet and outlet arranged at the lower end of the second positioning column 122 is a complete tubular structure. When connected, the sealing component is arranged between the threaded connector and the second inlet and outlet. The threaded connector is threadedly connected to the lower end of the second positioning column 122 and compresses the sealing component, causing the sealing component to undergo elastic deformation to complete the sealing connection effect.

[0034] The specific implementation process is as follows:

[0035] When in use, the feed end is sealed and connected to the feed port 123 through a sealing connector, and the discharge end is sealed and connected to the discharge port 112 through a sealing connector. The monomer solution and the solution are pumped into the reactor respectively through two sets of delivery pumps. The intermittent impact force when pumping the monomer solution and the solution is used to periodically impact the inner wall of the microchannel 14, so that the microchannel 14 vibrates periodically, and the vibration generated by the pump itself causes the microchannel 14 to oscillate, thereby promoting the discharge of the solution in the microchannel 14. At the same time, the flow of the heat transfer medium in the shell can also be used to impact the microchannel 14, so that the microchannel 14 vibrates in the shell, thereby guiding the material in the microchannel 14.

[0036] Example 2

[0037] Embodiment 2 is substantially the same as Embodiment 1, except that it further comprises a detection unit and a control unit, such as Figure 1 As shown, the detection unit includes a first sensor 31 and a second sensor 32. The first sensor 31 is arranged at the feed end of the microchannel 14 and can detect the feed pressure of the microchannel 14. The second sensor 32 is arranged at the discharge end of the microchannel 14 and can detect the discharge pressure of the microchannel 14. The control unit includes a controller. The controller is electrically connected to the first sensor 31, the second sensor 32 and the feed pump. When the difference between the feed pressure transmitted by the first sensor 31 and the discharge pressure transmitted by the second sensor 32 received by the controller is greater than a set value, the concentration of the input monomer in the microchannel 14 can be changed by controlling the proportion of the material pumped in by the feed pump, thereby changing the concentration of the polymer in the microchannel 14.

[0038] Example 3

[0039] On the basis of Example 1, Figure 5 As shown, a diaphragm 143 is provided between the cathode and the anode for ion passage, and the diaphragm 143 is fixedly connected to the inner wall of the reaction channel 141 to prevent the positive electrode and the negative electrode from being directly connected. At the same time, by providing the diaphragm 143, the flow rate of the material in the microchannel 14 can be reduced, and the contact time of the material with the electrode 142 can be prolonged, thereby improving the mass transfer efficiency without changing the length of the microchannel 14.

[0040] Example 4

[0041] On the basis of Example 1, Figure 6 As shown, the microchannel 14 is square in shape, and the cathode and the anode are respectively fixed on the inner wall of the microchannel 14 and kept parallel, so as to ensure the uniformity of the electric field inside the microchannel 14 and improve the reaction speed of the electropolymerization reaction.

[0042] The above is only an embodiment of the present invention, and common knowledge such as the known specific technical solutions and / or characteristics in the solution is not described in detail here. It should be pointed out that the technical means for solving the problems in the above-mentioned embodiments of the present invention can be used in combination to solve multiple technical problems at the same time. For those skilled in the art, several modifications and improvements can be made without departing from the technical solution of the present invention, which should also be regarded as the scope of protection of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. An electrochemical polymerization reaction device, characterized in that: The invention comprises a reaction unit for performing polymerization reaction and a detection unit for detecting reaction conditions. The reaction unit comprises a plurality of reactors for performing electrochemical polymerization reaction. The reactor comprises a microchannel. The microchannel is spiral-shaped and can guide materials in the microchannel by vibration. The reactor also comprises a temperature control unit. The temperature control unit comprises a shell and a heat transfer medium. The shell is cone-shaped and comprises a first shell, a second shell and a positioning connection piece. The feed end and the discharge end are respectively fixedly connected to the first shell and the second shell. The first shell and the positioning connection piece can be detachably fixed to the second shell. The second shell is fixed to a mounting frame. The shell is fixed to the mounting frame and wraps the reaction channel. The heat transfer medium flows between the outer wall of the microchannel and the inner wall of the shell. The overall reaction channel is cone-shaped, so that the spiral radius of the reaction channel gradually decreases, thereby increasing the force of the reactants on the inner wall of the reaction channel, making the vibration of the reaction channel more intense.

2. An electrochemical polymerization reaction device according to claim 1, characterized in that: The microchannel comprises a reaction channel and electrodes, and the electrodes are fixedly arranged on the inner wall of the reaction channel.

3. An electrochemical polymerization reaction device according to claim 2, characterized in that: The reactor also includes a mounting frame and a feed pump, the microchannel includes a feed end and a discharge end, both of which are fixed on the mounting frame, and the feed pump is fixed on the mounting frame and communicated with the feed end.

4. An electrochemical polymerization reaction device according to claim 3, characterized in that: The temperature control unit also includes a thermostat for adjusting the temperature of the heat transfer medium flowing in the shell. The shell is provided with a first inlet and a second inlet for the heat transfer medium to flow. The thermostat is connected to the first inlet and the second inlet and can control the temperature of the heat transfer medium.

5. The electrochemical polymerization reaction device according to claim 1, characterized in that: A second positioning column is fixed at the center of the second shell, and a first inlet and outlet and a first positioning column are provided on the positioning connector. The lower edge of the first inlet and outlet abuts against the upper edge of the first shell and seals the upper edge of the first shell. The free end of the first positioning column is threadedly connected with the free end of the second positioning column. The first positioning column and the second positioning column are both hollow tubular structures provided with a plurality of liquid inlet grooves. The second inlet and outlet are fixedly arranged at the end of the second positioning column and connected to the liquid inlet groove, and the first inlet and outlet are connected to the liquid inlet groove.

6. The electrochemical polymerization reaction device according to claim 1, characterized in that: The detection unit includes a first sensor and a second sensor, the first sensor is arranged at the feed end and can detect the pressure at the feed end, the second sensor is arranged at the discharge end and can detect the pressure at the discharge end, and also includes a control unit, the control unit includes a controller, the controller is electrically connected to the first sensor, the second sensor and the feed pump and can control the delivery speed of the feed pump.

7. An electrochemical polymerization reaction device according to claim 6, characterized in that: The electrode comprises a cathode and an anode, a diaphragm is arranged between the cathode and the anode for allowing ions to pass through, and the diaphragm is fixedly connected to the inner wall of the reaction channel.

8. An electrochemical polymerization reaction device according to claim 4, characterized in that: The size of the reaction channel is no larger than 200 microns.

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