A microreactor and a method for manufacturing the same
By designing a special micro-reaction chamber structure with interlaced distribution and specific adhesives and filtration devices in the micro reactor, the problems of micro-reactor channel blockage and insufficient liquid holding volume are solved, and more efficient reactant mixing and heat transfer efficiency is achieved, and self-cleaning function is provided.
Patent Information
- Application Number
- CN202110351134.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-03-31
- Publication Date
- 2025-03-14
- Estimated Expiration
- 2041-03-31
AI Technical Summary
In the case of complex structure and narrow channels, existing micro reactors are prone to blockage of channels and insufficient liquid holding volume, limiting their application range.
A micro reactor was designed, and its reaction channel substrate was equipped with interlaced frog face, ingot and bird-shaped micro-reaction chambers, which added impact columns and arc-shaped baffles, increased channel volume and improved chaos effect, and used specific adhesives and filter devices to prevent and solve channel clogging problems.
By optimizing the structure of the micro reactor, the volume and liquid holding volume of the channel are improved, the possibility of channel blockage is reduced, the mixing effect and heat transfer efficiency of the reactants are enhanced, and the self-cleaning function of the microchannel is realized.
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Figure CN112915941B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical reaction vessels, and in particular relates to a microreactor and a manufacturing method thereof. Background Art
[0002] Traditional chemical equipment has many disadvantages such as bulky, high energy consumption, low efficiency, and serious pollution. With the development of industrial automation and intelligence, as well as the emphasis on green environmental protection, the development of existing chemical production equipment towards automation, integration, and miniaturization is an inevitable trend for the future development of the chemical industry. Microreactors, as integrated and miniaturized chemical reaction equipment, represent an important direction for the development of the chemical industry in the future. Microreactors are chemical reaction devices that limit the site of chemical reactions to millimeters or even micrometers and nanometers. Their basic structure is a large number of micro-pipes, and a large number of bends, folds, obstacles, collisions and other structures are set inside the pipes. This structure greatly increases the impact friction between the reactants and the wall, so that the microreactor has the advantages of large specific surface area, high transfer rate, short contact time, and few by-products. Especially in exothermic reactions, a large amount of heat can be removed in time, thereby ensuring that the reaction temperature is maintained within the set range, minimizing the possibility of accidents. The pipeline structure of the microreactor also has obvious disadvantages, especially the small size of the internal channel, the narrow space, and the complex structure, so that the liquid holding capacity of the reaction channel is only a few milliliters, which can easily cause channel blockage and is difficult to clean. This disadvantage also greatly limits the application of microreactors.
[0003] In short, the bends, folds, obstacles, collisions and other structures in the microreactor pipeline enhance the chaotic effect of the material and improve the mass transfer efficiency. Therefore, designing a more reasonable spatial layout of bends, folds, obstacles, collisions and other structures can not only improve the chaotic effect of the microreactor and improve the mass transfer efficiency, but also increase the volume of the channel, increase the liquid holdup, and reduce channel blockage. Summary of the invention
[0004] The technical problem to be solved by the present invention is to overcome the shortcomings of the existing microreactor and provide a microreactor with reasonable design, good chaos effect, large pipeline volume and avoidance of channel blockage.
[0005] The technical solution adopted to solve the above technical problems is: a microreactor, the microreactor body is a lower heat bath substrate on which a reaction channel substrate is arranged, an upper heat bath substrate is arranged on the reaction channel substrate, a cover plate is arranged on the upper heat bath substrate, the reaction channel substrate is a substrate on which at least one microreaction channel connected end to end is processed, one end of the microreaction channel is an inlet, and the other end is an outlet, each microreaction channel is composed of at least one microreaction chamber connected end to end, the microreaction chambers of two adjacent microreaction channels are staggered, the microreaction chambers are frog-face shaped, the left and right contour lines of the microreaction chambers are symmetrical about the center line, the left contour line is composed of an arc line S1 with the center of the circle pointing outward, an arc line S2 with the center of the circle pointing inward, an arc line S3 with the center of the circle pointing outward, an arc line S4 with the center of the circle pointing inward, a straight line L1, an arc line S5 with the center of the circle pointing inward, a straight line L2, and an arc line S6 with the center of the circle pointing outward are connected in sequence, the straight line L1 is connected with the arc S4 and the arc S5 is connected tangently, straight line L2 is connected tangently to arc S5 and arc S6, arc S1 subtends a central angle of 210°~260°, and the radius of the circle is 0.5~0.8mm, arc S2 subtends a central angle of 100°~120°, and the radius of the circle is 3~3.5mm, arc S3 subtends a central angle of 60°~70°, and the radius of the circle is 0.5~1mm, arc S4 subtends a central angle of 130°~140° , the radius of the circle is 1.5-2.5mm, the central angle of arc S5 is 60°-75°, and the radius of the circle is 2.5-3.5mm, the central angle of arc S6 is 40°-50°, and the radius of the circle is 3-4mm. Two impact columns are arranged at the entrance of the micro-reaction chamber, and the plane where the center lines of the two impact columns are located is perpendicular to the center line of the micro-reaction channel. An arc baffle is arranged in the micro-reaction chamber downstream of the two impact columns.
[0006] As a preferred technical solution, the inner side surface of the arc baffle is a wave-shaped surface formed by three arc surfaces connected in sequence, the middle arc surface is a wave crest, the arc surfaces on both sides are wave troughs, and the outer side surface of the arc baffle is an inner concave surface.
[0007] As a preferred technical solution, the micro-reaction chamber is in the shape of a gold ingot, and the left and right contour lines of the micro-reaction chamber are symmetrical about the center line. The left contour line is composed of an arc C1 with the center inward, a straight line B1, an arc C2 with the center outward, an arc C3 with the center inward, an arc C4 with the center inward, an arc C5 with the center inward, a straight line B2, an arc C6 with the center inward, and an arc C7 with the center outward, wherein the arc C1 has a central angle of 120° to 130° and a circle radius of 2 to 3 mm, the length of the straight line B1 is 1.5 to 2 mm, the angle between the straight line B1 and the vertical direction is 50° to 70°, the central angle between the straight line B2 and the vertical direction is 45° to 55°, the circle radius is 0.5 to 1 mm, and the arc C2 and the straight line are connected in sequence. The arc C3 is tangent to the arc C1, the arc C4 is tangent to the arc C2, the arc C5 is tangent to the arc C3 and the arc C1 is tangent to the arc C1. The arc C3 is tangent to the arc C1 and the arc C2. The arc C4 is tangent to the arc C1 and the arc C2. The arc C5 is tangent to the arc C1 and the arc C2. The arc C6 is tangent to the arc C1 and the arc C2. The arc C6 is tangent to the arc C1 and the arc C2. The arc C6 is tangent to the arc C1 and the arc C2. The arc C7 is tangent to the arc C1 and the arc C2. The arc C7 is tangent to the arc C1 and the arc C2. The arc C1 and the arc C2 are tangent to the arc C1 and the arc C2. The arc C1 and the arc C2 are tangent to the arc C1 and the arc C2. The arc C1 and the arc C2 are tangent to the arc C1 and the arc C2. The arc C1 and the arc C2 are tangent to the arc C1 and the arc C2. The arc C1 and the arc C2 are tangent to the arc C1 and the arc C2.
[0008] As a preferred technical solution, the micro-reaction chamber is a bird-shaped heart and a circle connected as one, the left and right contours of the micro-reaction chamber are symmetrical about the center line, the left contour is composed of an arc A1 with the center of the circle inward, a straight line D1, an arc A2 with the center of the circle outward, an arc A3 with the center of the circle inward, an arc A4 with the center of the circle inward, an arc A5 with the center of the circle inward, an arc A6 with the center of the circle inward, and an arc A7 with the center of the circle outward, which are connected in sequence, the straight line D1 is tangent to the arc A1 and the arc A2, the arc A1 has a central angle of 80° to 100°, and a circle radius of 2 to 3 mm, the length of the straight line D1 is 1.5 to 2 mm, the arc A2 has a central angle of 200° to 300°, and a circle radius of 1 to 1.5 mm The central angle of arc A3 is 30°~60°, and the radius of the circle is 8~9mm, the central angle of arc A4 is 80°~90°, and the radius of the circle is 1.5~2mm, the central angle of arc A5 is 20°~30°, and the radius of the circle is 5~6mm, the central angle of arc A6 is 50°~60°, and the radius of the circle is 1~1.5mm, the central angle of arc A7 is 30°~60°, and the radius of the circle is 3~4mm, an impact column is arranged in the area formed by arc A1 on the left and right sides of the micro reaction chamber, and an arc baffle is arranged in the area formed by arc A2, arc A3, arc A4, arc A5, arc A6, and arc A7 on the left and right sides, and the arc back of the arc baffle faces the impact column.
[0009] As a preferred technical solution, a filtering device is arranged on the microreactor body between the two adjacent groups of microreaction channels. The filtering device is a filter element with two gaskets and a blind hole nut at one end. The upper end of the filter element is a nut, the middle section is a filter cartridge, and the lower end is a threaded section. The filter cartridge wall is provided with evenly distributed filtering holes. When the filter element is installed in the microreactor body, the filter cartridge is located in the microreaction channel of the reaction channel substrate.
[0010] As a preferred technical solution, the pore size of the filter hole is 0.1-1 mm.
[0011] As a preferred technical solution, the upper end of the filter element is a nut, the middle section is a column with an annular notch, and the lower end is a threaded section, and the depth of the notch is 0.1 to 1 mm.
[0012] As a preferred technical solution, the structure of the upper heat bath substrate is the same as that of the lower heat bath substrate. The upper heat bath substrate is a substrate on which an S-shaped heat bath channel is processed, and rectangular support plates are evenly distributed in the heat bath channel.
[0013] The present invention also provides a method for preparing a microreactor, wherein the lower heat bath substrate, the reaction channel substrate, the upper heat bath substrate, and the cover plate are bonded together by an adhesive, and the adhesive consists of 1-1.5% potassium tetrafluoroborate, 1-1.5% magnesium carbonate, 1-1.5% potassium nitrate, 35-40% sodium oxide, 5-10% boron trioxide, 20-25% phosphorus pentoxide, and 25-40% zinc oxide by mass percentage.
[0014] As a preferred technical solution, the inorganic salts of the adhesive are mixed together in proportion and placed in an agate ball grinder, and then 30-40% of the total mass of the adhesive is added to the powder. The powder is ground for 6-10 hours to obtain a fine mixed powder. When used, the powder is added to an aqueous solution containing a suspension stabilizer to prepare a stable suspension. The suspension is then sprayed evenly onto the lower heat bath substrate, the reaction channel substrate, the upper heat bath substrate, and the cover plate using a sprayer, and dried in an oven at 100-120° C. for 1-2 hours. The lower heat bath substrate, the reaction channel substrate, the upper heat bath substrate, and the cover plate are then overlapped in sequence and placed in a muffle furnace at 400-450° C. for 10-30 minutes, and then cooled to room temperature to obtain a microreactor bonded together.
[0015] The beneficial effects of the present invention are as follows:
[0016] 1. Compared with the traditional microreactor of heart-shaped microreactor, the frog-face-shaped microreactor has two additional impact columns and two fold structures, the ingot-shaped microreactor has one additional impact column and two fold structures, and the bird-shaped microreactor has one additional impact column, all of which have better chaos effect. The microreactors of two adjacent microreaction channels are staggered, which reduces the interval space between adjacent microreaction channels, increases the volume of the microreaction channels, and improves the liquid holding capacity of the microreactor.
[0017] 2. The adhesive of the present invention contains a small amount of potassium tetrafluoroborate, magnesium carbonate, potassium nitrate and other high-temperature easily decomposable substances. The adhesive melts at 500°C, and potassium tetrafluoroborate, magnesium carbonate and potassium nitrate will decompose and release gas at this time, thereby separating the substrates bonded together at high temperature. After the micro-reaction channel is blocked, the micro-reactor will be split into the original assembled substrates when heated to a high temperature. After returning to room temperature, the blocked substrate is thoroughly cleaned. After cleaning, the adhesive is applied to the surface of the substrate and heated to 400-450°C. At this time, the adhesive melts, and potassium tetrafluoroborate, magnesium carbonate and potassium nitrate will not decompose. After returning to room temperature, the substrates are bonded together again, thereby realizing the dredging function after the micro-channel is blocked;
[0018] 3. The adhesives of the present invention are all inorganic salts, which have good corrosion resistance. After bonding and forming, they have the same strength as the microreactor sintered at high temperature and can withstand a pressure of at least 0.2Mpa;
[0019] 4. The filtering device of the present invention can prevent the reaction liquid from crystallizing inside the microchannel and blocking the microreaction channel, and can also add a granular catalyst to the microreaction channel with the help of a filter element to realize the catalytic function of the microchannel. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 It is a schematic diagram of the structure of embodiment 1 of the present invention.
[0021] Figure 2 Schematic diagram of the structure of the reaction channel substrate 2 in Example 1.
[0022] Figure 3 It is a schematic diagram of the structure of the micro-reaction chamber a in Example 1.
[0023] Figure 4 Schematic diagram of the structure of the upper heat bath substrate 3 in Example 1.
[0024] Figure 5 It is a schematic structural diagram of the filtering device 5 in Example 1.
[0025] Figure 6 It is a schematic diagram of the structure of the reaction channel substrate 2 in Example 4.
[0026] Figure 7 It is a schematic diagram of the structure of micro-reaction chamber a in Example 4.
[0027] Figure 8 It is a schematic diagram of the structure of the reaction channel substrate 2 in Example 5.
[0028] Fig. 9 It is a schematic diagram of the structure of micro-reaction chamber a in Example 5.
[0029] Fig.10 It is a schematic structural diagram of the filtering device 5 in Example 6. DETAILED DESCRIPTION
[0030] The present invention will be further described in detail below in conjunction with the accompanying drawings and examples, but the present invention is not limited to the following embodiments. Example 1
[0031] exist Figures 1 to 4In the embodiment, the microreactor is composed of a lower heat bath substrate 1, a reaction channel substrate 2, an upper heat bath substrate 3, a cover plate 4, and a filtering device 5. The structure of the microreactor body is that the reaction channel substrate 2 is adhered to the lower heat bath substrate 1 with an adhesive, the upper heat bath substrate 3 is adhered to the reaction channel substrate 2 with an adhesive, and the cover plate 4 is adhered to the upper heat bath substrate 3 with an adhesive. The upper heat bath substrate is a substrate on which a heat channel distributed in an S shape is processed. The structure of the lower heat bath substrate 1 is the same as that of the upper heat bath substrate 3. Rectangular support plates are evenly distributed in the bath heating channel. Heating oil is introduced into the bath heating channel to heat the reaction liquid. The reaction channel substrate is processed with 6 micro-reaction channels connected end to end. One end of the micro-reaction channel is an inlet and the other end is an outlet. Each micro-reaction channel is composed of 12 micro-reaction chambers a connected end to end. The micro-reaction chambers a of two adjacent micro-reaction channels are staggered. The micro-reaction chambers a are frog-face shaped. The left and right contour lines of the micro-reaction chambers a are symmetrical about the center line. The left contour line is composed of an arc S1 with the center of the circle pointing outward, an arc S2 with the center of the circle pointing inward, an arc S3 with the center of the circle pointing outward, and an arc S4 with the center of the circle pointing inward. The arc S4, the straight line L1, the arc S5 with the center inward, the straight line L2, and the arc S6 with the center outward are connected in sequence, the straight line L1 is tangent to the arc S4 and the arc S5, the straight line L2 is tangent to the arc S5 and the arc S6, the arc S1 subtends a central angle of 240° and a circle radius of 0.65 mm, the arc S2 subtends a central angle of 110° and a circle radius of 3.2 mm, the arc S3 subtends a central angle of 65° and a circle radius of 0.7 mm, the arc S4 subtends a central angle of 135° and a circle radius of 2 mm, the arc S5 subtends a central angle of 70° and a circle radius of 0.65 mm, The diameter is 3mm, the central angle of the arc S6 is 45°, and the radius of the circle is 3.5mm. Two impact columns 2-1 are processed at the entrance of the micro-reaction chamber a. The plane where the center lines of the two impact columns 2-1 are located is perpendicular to the flow direction of the liquid. An arc baffle 2-2 is processed in the micro-reaction chamber a downstream of the two impact columns 2-1. The inner side of the arc baffle 2-2 is three arc surfaces connected in sequence to form a wavy surface. The middle arc surface is the crest, and the arc surfaces on both sides are the troughs. The outer side of the arc baffle 2-2 is an inner concave surface. The reaction liquid is introduced into the micro-reaction channel. The reaction liquid flows through the frog face micro-reaction chamber a. Due to the frog The micro-reactor chamber a has a large number of bends, folds, obstacles, collisions and other structures processed inside. The liquid is fully mixed under frequent friction, impact and chaos, and is heated by the tightly fitted upper and lower oil bath channels. Not only is the reactant mixing effect good and there is no amplification effect, but the heat transfer efficiency is also extremely high. The microreactor is particularly suitable for exothermic nitration reactions. A filtering device 5 is installed on the microreactor body between two adjacent groups of micro-reaction channels to prevent the reaction liquid from crystallizing inside the micro-reaction channel and clogging the micro-reaction channel. A granular catalyst can be added to the micro-reaction channel with the help of a filter element to realize the catalytic function of the micro-channel.
[0032] exist Figure 5 In the figure, the filtering device 5 of this embodiment is composed of a filter element 5-1, a gasket 5-2, and a blind hole nut 5-3. The upper end of the filter element 5-1 is a nut, the middle section is a filter cartridge, and the lower end is a threaded section. The filter cartridge wall is processed with evenly distributed filter holes, and the pore size of the filter holes is 0.3 mm, which is used to filter fine solid suspended particles in the reaction liquid. The filter element 5-1 is installed on the microreactor body, and the middle section of the filter cartridge is located in the microreaction channel of the reaction channel substrate. A gasket 5-2 is installed between the nut at the upper end of the filter element 5-1 and the microreactor body, and a blind hole nut 5-3 is installed on the threaded section at the lower end of the filter element 5-1. The blind hole nut 5-3 is used to fix the filter element 5-1 to the microreactor body, and a gasket 5-2 is installed between the blind hole nut 5-3 and the microreactor body. When there are solid suspended particles in the reaction liquid, the solids in the reaction liquid will be throttled at the filter element 5-1. When the filter element 5-1 is blocked, it is only necessary to unscrew the blind hole nut 5-3 to remove the filter element 5-1, and then install it on the microreactor again after unblocking. This prevents the microreaction channel from being blocked and difficult to unblock.
[0033] The adhesive of the present embodiment is composed of 1.2% potassium tetrafluoroborate, 1.2% magnesium carbonate, 1.2% potassium nitrate, 38% sodium oxide, 6.4% boron trioxide, 22% phosphorus pentoxide, and 30% zinc oxide by mass percentage. The above inorganic salts are mixed together in proportion, and then 35% mass fraction of water is added to the powder, and the powder is placed in an agate ball grinder and ground for 8 hours to obtain a fine mixed powder. When used, the powder is added to an aqueous solution containing a small amount of suspension stabilizer to prepare a stable suspension, and then a sprayer is used to evenly spray the suspension onto the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 to be bonded, and dried in an oven at 110°C for 2 hours, and then the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 are overlapped and placed in a muffle furnace at 420°C for 30 minutes, and then cooled to room temperature to obtain a microreactor. Example 2
[0034] In this embodiment, the reaction channel substrate is a substrate on which 6 micro-reaction channels connected end to end are processed, one end of the micro-reaction channel is an inlet, and the other end is an outlet. Each micro-reaction channel is composed of 12 micro-reaction chambers a connected end to end, and the micro-reaction chambers a of two adjacent micro-reaction channels are staggered. The micro-reaction chambers a are in the shape of a frog face, and the left and right contour lines of the micro-reaction chambers a are symmetrical about the center line. The left contour line is composed of an arc S1 with the center of the circle pointing outward, an arc S2 with the center of the circle pointing inward, an arc S3 with the center of the circle pointing outward, an arc S4 with the center of the circle pointing inward, a straight line L1, an arc S5 with the center of the circle pointing inward, a straight line L2, and an arc S6 with the center of the circle pointing outward, which are connected in sequence. The straight line L1 is tangent to the arc S4 and the arc S5, and the straight line L2 is tangent to the arc S5 and The arc S6 is connected tangently, the arc S1 subtends a central angle of 240° and a circle radius of 0.65mm, the arc S2 subtends a central angle of 110° and a circle radius of 3.2mm, the arc S3 subtends a central angle of 65° and a circle radius of 0.7mm, the arc S4 subtends a central angle of 135° and a circle radius of 2mm, the arc S5 subtends a central angle of 70° and a circle radius of 3mm, the arc S6 subtends a central angle of 45° and a circle radius of 3.5mm, two impact columns 2-1 are processed at the entrance of the micro-reaction chamber a, the plane where the center lines of the two impact columns 2-1 are located is perpendicular to the liquid flow direction, and an arc baffle 2-2 is processed in the micro-reaction chamber a downstream of the two impact columns 2-1. Other components and the connection relationship of the components are the same as those in Example 1.
[0035] The adhesive of the present embodiment is composed of 1% potassium tetrafluoroborate, 1.2% magnesium carbonate, 1% potassium nitrate, 35% sodium oxide, 8.8% boron trioxide, 20% phosphorus pentoxide, and 33% zinc oxide by mass percentage. The above inorganic salts are mixed together in proportion, and then 30% water of the total mass of the adhesive is added to the powder, and the powder is placed in an agate ball grinder and ground for 6 hours to obtain a fine mixed powder. When used, the powder is added to an aqueous solution containing a small amount of suspension stabilizer to prepare a stable suspension, and then a sprayer is used to evenly spray the suspension onto the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 to be bonded, and dried in an oven at 100°C for 2 hours, and then the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 are overlapped and placed in a muffle furnace at 400°C for 30 minutes, and then cooled to room temperature to obtain a microreactor. Example 3
[0036] In this embodiment, the reaction channel substrate is a substrate on which 6 micro-reaction channels connected end to end are processed, one end of the micro-reaction channel is an inlet, and the other end is an outlet. Each micro-reaction channel is composed of 12 micro-reaction chambers a connected end to end, and the micro-reaction chambers a of two adjacent micro-reaction channels are staggered. The micro-reaction chambers a are in the shape of a frog face, and the left and right contour lines of the micro-reaction chambers a are symmetrical about the center line. The left contour line is composed of an arc S1 with the center of the circle pointing outward, an arc S2 with the center of the circle pointing inward, an arc S3 with the center of the circle pointing outward, an arc S4 with the center of the circle pointing inward, a straight line L1, an arc S5 with the center of the circle pointing inward, a straight line L2, and an arc S6 with the center of the circle pointing outward, which are connected in sequence. The straight line L1 is tangent to the arc S4 and the arc S5, and the straight line L2 is tangent to the arc S5 and The arc S6 is connected tangently, the arc S1 subtends a central angle of 240° and a circle radius of 0.65mm, the arc S2 subtends a central angle of 110° and a circle radius of 3.2mm, the arc S3 subtends a central angle of 65° and a circle radius of 0.7mm, the arc S4 subtends a central angle of 135° and a circle radius of 2mm, the arc S5 subtends a central angle of 70° and a circle radius of 3mm, the arc S6 subtends a central angle of 45° and a circle radius of 3.5mm, two impact columns 2-1 are processed at the entrance of the micro-reaction chamber a, the plane where the center lines of the two impact columns 2-1 are located is perpendicular to the liquid flow direction, and an arc baffle 2-2 is processed in the micro-reaction chamber a downstream of the two impact columns 2-1. Other components and the connection relationship of the components are the same as those in Example 1.
[0037] The adhesive of the present embodiment is composed of 1.5% potassium tetrafluoroborate, 1.5% magnesium carbonate, 1% potassium nitrate, 40% sodium oxide, 10% boron trioxide, 23% phosphorus pentoxide, and 23% zinc oxide by mass percentage. The above inorganic salts are mixed together in proportion, and then 40% water of the total mass of the adhesive is added to the powder, and the powder is placed in an agate ball grinder and ground for 10 hours to obtain a fine mixed powder. When used, the powder is added to an aqueous solution containing a small amount of suspension stabilizer to prepare a stable suspension, and then a sprayer is used to evenly spray the suspension onto the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 to be bonded, and dried in an oven at 120° C. for 2 hours, and then the lower heat bath substrate 1, the reaction channel substrate 2, the upper heat bath substrate 3, and the cover plate 4 are overlapped and placed in a muffle furnace at 450° C. for 10 minutes, and then cooled to room temperature to obtain a microreactor. Example 4
[0038] In this embodiment, the microreactor with a detachable filter element 5-1 is composed of a lower heat bath substrate 1, a reaction channel substrate 2, an upper heat bath substrate 3, a cover plate 4, and a filtering device 5. The reaction channel substrate 2 is a substrate on which 6 microreaction channels connected end to end are processed. One end of the microreaction channel is an inlet and the other end is an outlet. Each microreaction channel is composed of 12 microreaction chambers a connected end to end. The microreaction chambers a of two adjacent microreaction channels are staggered. Figure 6 , the micro-reaction chamber a is in the shape of a gold ingot, such as Figure 7 The left and right contours of the micro-reaction chamber a are symmetrical about the center line. The left contour is composed of an arc C1 with the center inward, a straight line B1, an arc C2 with the center outward, an arc C3 with the center inward, an arc C4 with the center inward, an arc C5 with the center inward, a straight line B2, an arc C6 with the center inward, and an arc C7 with the center outward, wherein the arc C1 has a central angle of 125° and a circle radius of 2.5 mm, a straight line B1 has a length of 1.8 mm, an angle between the straight line B1 and the vertical direction of 60°, a central angle between the straight line B2 and the vertical direction of 50°, and a circle radius of 0.8 mm, an arc C2 is tangent to the straight line L1, and an arc C3 has a central angle of 0. The arc C4 is 50° and the radius of the circle is 4.5mm, the arc C4 is 95° and the radius of the circle is 2.5mm, the arc C5 is 20° and the radius of the circle is 5.5mm, the length of the straight line B2 is 4.5mm, the straight line L2 is tangent to the arc C5 and the arc C6, the arc C6 is 95° and the radius of the circle is 0.8mm, the arc C7 is 35° and the radius of the circle is 7.5mm, an impact column 2-1 is processed at the entrance of the micro-reaction chamber a, and an arc baffle 2-2 is processed in the micro-reaction chamber a downstream of the impact column 2-1, the arc back of the arc baffle 2-2 faces upstream, and the two ends are folded upstream. Other parts and the connection relationship of the parts are the same as those in Example 1. Example 5
[0039] In this embodiment, the microreactor is composed of a lower heat bath substrate 1, a reaction channel substrate 2, an upper heat bath substrate 3, a cover plate 4, and a filter device 5. The reaction channel substrate 2 is a substrate on which 6 microreaction channels connected end to end are processed. One end of the microreaction channel is an inlet and the other end is an outlet. Each microreaction channel is composed of 12 microreaction chambers a connected end to end. The microreaction chambers a of two adjacent microreaction channels are staggered. Figure 8 The micro-reaction chamber a is a bird-shaped structure that combines a heart shape and a circle. Fig. 9The left and right contours of the micro-reaction chamber a are symmetrical about the center line. The left contour is formed by connecting the arc A1 with the center inward, the straight line D1, the arc A2 with the center outward, the arc A3 with the center inward, the arc A4 with the center inward, the arc A5 with the center inward, the arc A6 with the center inward, and the arc A7 with the center outward in sequence. The straight line D1 is tangent to the arc A1 and the arc A2. The arc A1 has a central angle of 90° and a circle radius of 2.5 mm. The length of the straight line D1 is 1.8 mm. The arc A2 has a central angle of 250° and a circle radius of 1.2 mm. The arc A3 has a central angle of 45°. , the radius of the circle is 8.5mm, the central angle of arc A4 is 85°, the radius of the circle is 1.8mm, the central angle of arc A5 is 25°, the radius of the circle is 5.5mm, the central angle of arc A6 is 55°, the radius of the circle is 1.2mm, the central angle of arc A7 is 45°, the radius of the circle is 3.5mm, and an impact column 2-1 is processed in the area formed by arc A1 on the left and right sides of the micro-reaction chamber a, and an arc baffle is processed in the area formed by arc A2, arc A3, arc A4, arc A5, arc A6, and arc A7 on the left and right sides, and the arc back of the arc baffle faces the impact column 2-1. Other components and the connection relationship of the components are the same as those in Example 1. Example 6
[0040] In the above embodiments 1 to 5, the filter device 5 is composed of a filter element 5-1, a gasket 5-2, and a blind hole nut 5-3. The upper end of the filter element is a nut, the middle section is a column with an annular notch, and the lower end is a threaded section. The depth of the notch is 0.5 mm, or 0.1 mm, or 1 mm. Fig.10 .
Claims
1. A microreactor, characterized in that: The microreactor body is a lower heat bath substrate (1) on which a reaction channel substrate (2) is arranged, an upper heat bath substrate (3) is arranged on the reaction channel substrate (2), and a cover plate (4) is arranged on the upper heat bath substrate (3). The reaction channel substrate is a substrate on which at least one microreaction channel connected end to end is processed, one end of the microreaction channel is an inlet, and the other end is an outlet. Each microreaction channel is composed of at least one microreaction chamber (a) connected end to end. The microreaction chambers (a) of two adjacent microreaction channels are arranged alternately. The microreaction chambers (a) are frog-face shaped. The left and right contour lines of the microreaction chambers (a) are symmetrical about the center line. The left contour line is composed of an arc line S1 with the center of the circle pointing outward, an arc line S2 with the center of the circle pointing inward, an arc line S3 with the center of the circle pointing outward, an arc line S4 with the center of the circle pointing inward, a straight line L1, an arc line S5 with the center of the circle pointing inward, a straight line L2, and an arc line S6 with the center of the circle pointing outward, which are connected in sequence. The straight line L1 is tangent to the arc line S4 and the arc line S5. The straight line L2 is tangent to the arc line S4 and the arc line S5. It is tangent to arc S5 and arc S6. The central angle of arc S1 is 210°~260°, and the radius of the circle is 0.5~0.8mm. The central angle of arc S2 is 100°~120°, and the radius of the circle is 3~3.5mm. The central angle of arc S3 is 60°~70°, and the radius of the circle is 0.5~1mm. The central angle of arc S4 is 130°~140°, and the radius of the circle is 1.5~2.5mm. The center angle of the circle subtended by line S5 is 60° to 75°, and the radius of the circle is 2.5 to 3.5 mm; the center angle of the circle subtended by arc S6 is 40° to 50°, and the radius of the circle is 3 to 4 mm; two impact columns (2-1) are arranged at the entrance of the micro-reaction chamber (a); the plane where the center lines of the two impact columns (2-1) are located is perpendicular to the center line of the micro-reaction channel; and an arc-shaped baffle (2-2) is arranged in the micro-reaction chamber (a) downstream of the two impact columns (2-1); The inner side surface of the arc-shaped baffle (2-2) is composed of three arc-shaped surfaces connected in sequence to form a wave-shaped surface, the middle arc-shaped surface is a wave crest, the arc-shaped surfaces on both sides are wave troughs, and the outer side surface of the arc-shaped baffle (2-2) is an inner concave surface; The structure of the upper heat bath substrate (3) is the same as that of the lower heat bath substrate (1). The upper heat bath substrate (3) is a substrate on which an S-shaped heat bath channel is processed, and rectangular support plates are evenly distributed in the heat bath channel.
2. The microreactor according to claim 1, characterized in that: The micro-reaction chamber (a) is in the shape of a gold ingot, and the left and right contour lines of the micro-reaction chamber (a) are symmetrical about the center line. The left contour line is composed of an arc C1 with the center of the circle pointing inward, a straight line B1, an arc C2 with the center of the circle pointing outward, an arc C3 with the center of the circle pointing inward, an arc C4 with the center of the circle pointing inward, an arc C5 with the center of the circle pointing inward, a straight line B2, an arc C6 with the center of the circle pointing inward, and an arc C7 with the center of the circle pointing outward, which are connected in sequence. The arc C1 has a center angle of 120° to 130° and a circle radius of 2 to 3 mm. The length of the straight line B1 is 1.5 to 2 mm. The angle between the straight line B1 and the vertical direction is 50° to 70°. The center angle between the straight line B2 and the vertical direction is 45° to 55°. The radius of the circle is 0.5 to 1 mm. The arc C2 is tangent to the straight line L1. The center angle between the arc C3 and the vertical direction is 40° to 70°. The arc C4 has a central angle of 90° to 100° and a circle radius of 2 to 3 mm, the arc C5 has a central angle of 15° to 30° and a circle radius of 5 to 6 mm, the length of the straight line B2 is 4 to 5 mm, the straight line L2 is tangent to the arc C5 and the arc C6, the arc C6 has a central angle of 90° to 100° and a circle radius of 0.5 to 1 mm, the arc C7 has a central angle of 30° to 45° and a circle radius of 7 to 8 mm, an impact column (2-1) is arranged at the entrance of the micro-reaction chamber (a), and an arc baffle (2-2) is arranged in the micro-reaction chamber (a) downstream of the impact column (2-1), the arc back of the arc baffle (2-2) faces upstream, and both ends are folded toward the upstream.
3. The microreactor according to claim 1, characterized in that: The micro-reaction chamber (a) is a bird-shaped structure in which a heart shape and a circle are connected as one. The left and right contour lines of the micro-reaction chamber (a) are symmetrical about the center line. The left contour line is composed of an arc A1 with the center of the circle pointing inward, a straight line D1, an arc A2 with the center of the circle pointing outward, an arc A3 with the center of the circle pointing inward, an arc A4 with the center of the circle pointing inward, an arc A5 with the center of the circle pointing inward, an arc A6 with the center of the circle pointing inward, and an arc A7 with the center of the circle pointing outward, which are connected in sequence. The straight line D1 is tangent to the arc A1 and the arc A2. The arc A1 has a center angle of 80° to 100° and a circle radius of 2 to 3 mm. The length of the straight line D1 is 1.5 to 2 mm. The arc A2 has a center angle of 200° to 300° and a circle radius of 1 to 1.5 mm. The arc A3 has a center angle of 30°. The arc A4 is at a central angle of 80° to 90° and a circle with a radius of 1.5 to 2 mm, the arc A5 is at a central angle of 20° to 30° and a circle with a radius of 5 to 6 mm, the arc A6 is at a central angle of 50° to 60° and a circle with a radius of 1 to 1.5 mm, the arc A7 is at a central angle of 30° to 60° and a circle with a radius of 3 to 4 mm, and an impact column (2-1) is arranged in the area formed by the arc A1 on the left and right sides of the micro reaction chamber (a), and an arc baffle (2-2) is arranged in the area formed by the arc A2, arc A3, arc A4, arc A5, arc A6 and arc A7 on the left and right sides, and the back of the arc baffle (2-2) faces the impact column (2-1).
4. The microreactor according to claim 1, characterized in that: A filtering device (5) is provided on the microreactor body between two adjacent groups of microreaction channels. The filtering device (5) is a filter element (5-1) provided with two gaskets (5-2) and a blind hole nut (5-3) at one end. The filter element (5-1) has a nut at the upper end, a filter cartridge in the middle section, and a threaded section at the lower end. The filter cartridge wall is provided with evenly distributed filtering holes. When the filter element (5-1) is installed on the microreactor body, the filter cartridge is located in the microreaction channel of the reaction channel substrate.
5. The microreactor according to claim 4, characterized in that: The pore size of the filter hole is 0.1-1 mm.
6. The microreactor according to claim 4, characterized in that: The filter element (5-1) has a nut at the upper end, a column with an annular notch in the middle, and a threaded section at the lower end, wherein the depth of the notch is 0.1 to 1 mm.
7. The method for making a microreactor according to claim 1, characterized in that: The lower heat bath substrate (1), the reaction channel substrate (2), the upper heat bath substrate (3), and the cover plate (4) are bonded together by an adhesive, wherein the adhesive is composed of 1 to 1.5% potassium tetrafluoroborate, 1 to 1.5% magnesium carbonate, 1 to 1.5% potassium nitrate, 35 to 40% sodium oxide, 5 to 10% boron trioxide, 20 to 25% phosphorus pentoxide, and 25 to 40% zinc oxide by mass percentage.
8. The method for making a microreactor according to claim 7, characterized in that: The inorganic salts of the adhesive are mixed together in proportion and placed in an agate ball grinder, and then 30-40% of the total mass of the adhesive is added to the powder. The powder is ground for 6-10 hours to obtain a fine mixed powder. When used, the powder is added to an aqueous solution containing a suspension stabilizer to prepare a stable suspension. The suspension is then sprayed evenly onto a lower heat bath substrate (1), a reaction channel substrate (2), an upper heat bath substrate (3), and a cover plate (4) using a sprayer, and then dried in an oven at 100-120° C. for 1-2 hours. The lower heat bath substrate (1), the reaction channel substrate (2), the upper heat bath substrate (3), and the cover plate (4) are then overlapped in sequence and placed in a muffle furnace at 400-450° C. for 10-30 minutes, and then cooled to room temperature to obtain a microreactor bonded together.
Citation Information
Patent Citations
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