A microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole
By designing the segmented transfer and segmented pressurized filtration structure of the reagent in the microchannel reactor, the low efficiency and blockage problems in the preparation process of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole are solved, and an efficient and safe reaction process is achieved.
Patent Information
- Application Number
- CN202510804812.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2025-08-15
- Estimated Expiration
- 2045-06-17
AI Technical Summary
In the prior art, the preparation process of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole has problems such as low reaction efficiency, long time and safety hazards, and the microchannel reactor is prone to blockage.
A microchannel reactor is designed to transfer the reaction reagent from the inlet end to the outlet end in segments by setting up the reaction reagent from the inlet end to the outlet end, and pressurize and filter in segments during the transfer process. The driving structure is used to drive the opening and closing of the microchannel reaction member, and the pressure adjustment component is used to realize the segments of the reagent pressurize and filtration, combining the cleaning function of the flexible filter net and the airbag bag to ensure the smooth progress of the reaction.
The reaction efficiency is improved, the micro-reaction flow channel is blocked, the safety and efficiency of the reaction are ensured, and the efficient preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole is achieved.
Smart Images

Figure CN120305910B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of microchannel reactors, in particular to a microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole. Background Art
[0002] The general preparation procedure for 1-methyl-3-trifluoromethyl-5-hydroxypyrazole involves adding 40% methylhydrazine aqueous solution and acetic acid to a reaction flask. Ethyl trifluoroacetoacetate is then added dropwise at a constant temperature. After the reaction is complete, several times the volume of acetic acid is added to cool the reaction, followed by filtration, pulp washing, filtration, and drying of the solid to obtain the product. This reaction is inefficient, time-consuming, and poses safety risks.
[0003] A microchannel reactor is essentially a continuous-flow tubular reactor with channel dimensions typically ranging from micrometers to millimeters. This miniaturized design significantly increases the contact area between reactants and catalysts, while simultaneously reducing mass and heat transfer resistance during the reaction, resulting in safe and efficient reactions. Therefore, the preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole using a microchannel reactor has considerable application value.
[0004] A Chinese patent with authorization announcement number CN117282395B discloses an anti-clogging microchannel reactor, including a microchannel reactor body and a filter cartridge shell. The front end of the filter cartridge shell is fixedly installed with a liquid inlet pipe connected to the well, and the rear end of the filter cartridge shell is fixedly installed with a drain pipe connected to the input end of the microchannel reactor body. A filter plate is fixedly installed in the filter cartridge shell, a filter chip is fixedly installed on the filter plate, a rotating shaft column is rotatably installed on the filter plate, an arc-shaped push flow plate is fixedly installed on the rotating shaft column, a filter core strip is installed at the tail end of the arc-shaped push flow plate, and a water inlet notch is provided at the bottom end of the rotating shaft column, so that the reaction material first undergoes a preliminary reaction or dissolution with the reaction liquid in the filter cartridge shell.
[0005] Blockage of microchannel reactors is a common problem. The existing methods for preventing blockage mainly focus on pretreatment in the early stage, generally filtering the reagents before entering the microreaction channel. However, due to the inherent properties of the finished product during the reaction process, for example, 1-methyl-3-trifluoromethyl-5-hydroxypyrazole itself is a powder, which can easily cause blockage after moving and agglomerating in the microreaction channel, thereby affecting the preparation efficiency and effect. Summary of the Invention
[0006] In response to the problems existing in the background technology, a microchannel reactor for the preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole is proposed. Each reaction reagent is transferred from the water inlet end to the water outlet end in sections. During the transfer process, the reaction reagents are pressurized and filtered in sections, and the preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole is finally completed efficiently.
[0007] The present invention provides a microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole, comprising a reaction barrel, a feed member, a discharge member, a microchannel reaction member, and a pressure regulating assembly. The reaction barrel extends through a housing in the longitudinal direction and is rotatably connected to the housing by a first drive structure. A first feed pipe is provided at one end, and a discharge pipe is provided at the other end. The feed member is located on one side of the housing and connected to the first feed pipe. The discharge member is located on the other side of the housing and connected to the discharge pipe. The microchannel reaction member comprises a plurality of reaction plates forming microreaction flow channels, and the microchannel reaction members are arranged in pairs within the reaction barrel. Each pair of microchannel reaction members is driven by a second drive structure to open and close horizontally and rotate with the reaction barrel. Two adjacent pairs of microchannel reaction members open and close synchronously and in opposite directions. The two outermost groups of microchannel reaction members are respectively connected to the first feed pipe and the discharge pipe. The pressure regulating assembly is fixed between each pair of microchannel reaction members. As the microchannel reaction members on both sides open and close, the air inside the pressure regulating assembly is synchronously squeezed or stretched, thereby pressurizing the circulating reagent in sections.
[0008] Preferably, the space between the outer shell and the reaction cylinder is filled with a heat-insulating agent.
[0009] Preferably, the driving structure 1 is located at both ends of the reaction tube, and includes a gear 1 driven to rotate by a motor 1; the gear 2 is sleeved on the outer circumference of the reaction tube and meshed with the gear 1.
[0010] Preferably, the second driving structure includes an adjusting rod arranged along the length direction of the reaction cylinder and driven to rotate by the driving box; the adjusting rod has corresponding adjusting sections arranged logarithmically corresponding to the microchannel reaction piece; the paired moving blocks are threadedly connected to the two ends of the adjusting sections to achieve opening and closing movement; the mounting frame 1 is clamped on the outside of the microchannel reaction piece and is connected to the moving blocks one by one.
[0011] Preferably, connectors connecting the head end and the tail end of the microreaction channel are respectively provided on both sides of the microchannel reaction piece; the connector at the front end is connected to the feed pipe, the connector at the rear end is connected to the discharge pipe, and the remaining connectors are connected to the pressure regulating assembly; the pressure regulating assembly includes two groups of connecting pipes respectively connected to the connectors on the front and rear microchannel reaction pieces; the opposite ends of the two groups of connecting pipes slide into the pressure regulating cylinder from both ends, and are connected to the piston plates with one-way valves; the one-way valves on the two groups of piston plates control the reagent to enter from one side and exit from the other side; the filter screen is arranged between the two groups of piston plates.
[0012] Preferably, the filter is a flexible filter; a deformable membrane connected to the edge of the flexible filter is provided on the side wall of the pressure regulating cylinder, and a rotatable adjustment ring is also provided on the periphery of the pressure regulating cylinder; the airbag bags are covered one by one on the deformable membrane and filled with gas; the extrusion piece is provided on the adjustment ring, and as the adjustment ring rotates, the airbag bags are squeezed in turn.
[0013] Preferably, extrusion pieces are arranged at intervals on the side walls of the adjustment ring; the end of the adjustment ring is sleeved with gear three, and one side is provided with gear four driven to rotate by motor two; gear three is meshed with gear four and is rotationally connected to the pressure regulating cylinder; the extrusion piece is wheel-shaped and can generate heat when powered.
[0014] Preferably, the feed component includes a mounting frame 2; multiple groups of discharge tanks are arranged in the mounting frame 2, and sampling pumps correspondingly connected to the multiple groups of discharge tanks are arranged on the mounting frame 2; each group of sampling pumps transfers the corresponding reagent to the feed pipe 1 by cooperating with the corresponding feed pipe 2.
[0015] Compared with the prior art, the present invention has the following beneficial technical effects: a reaction cylinder soaked in a heat-insulating agent and rotatable from the origin is provided, so that the temperature of each reaction reagent is maintained and mixed thoroughly during the movement, thereby achieving the purpose of efficient reaction. Microchannel reaction elements are arranged in pairs, and each pair of microchannel reaction elements is driven by a second drive structure to open and close in the horizontal direction, and the opening and closing of two adjacent pairs of microchannel reaction elements are synchronized and opposite, and a pressure regulating assembly is fixed between each pair of microchannel reaction elements. This structure allows the two sets of connecting pipes to drive the two sets of piston plates to separate when the microchannel reaction elements on both sides are separated, stretching the air in the pressure regulating cylinder. When the microchannel reaction elements on both sides are closed, the two sets of connecting pipes drive the two sets of piston plates to close, squeezing the air in the pressure regulating cylinder. The pressure regulating assembly arranged along the flow direction of the reagents squeezes-closes-squeezes-closes in sequence, so that the reagents in the adjacent microchannel reaction elements alternately enter and exit, and the reagents are pressurized in sections, on the one hand reducing the blockage of the micro-reaction flow channel, and on the other hand accelerating mixing and reaction. Simultaneously, the pressure regulating cylinder rotates, driving the extrusion element to squeeze the airbag. The deformable membrane deforms under the pressure of the gas, driving the filter to deform, thereby achieving both cleaning and localized pressurization. Finally, the reaction reagents are transferred from the water inlet to the outlet in stages, undergoing staged pressurization and filtration during the transfer process, ultimately completing the efficient preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 Schematic diagram of the structure of the microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole in the present invention;
[0017] Figure 2 is a cross-sectional view of the housing of the present invention;
[0018] Figure 3 is a cross-sectional view of the reaction tube in the present invention;
[0019] Figure 4 for Figure 2 Enlarged view of point A in the middle;
[0020] Figure 5 Schematic diagram of the structure of the driving structure 2 and the microchannel reaction element;
[0021] Figure 6 It is a structural diagram of a microchannel reaction component and a pressure regulating assembly;
[0022] Figure 7 It is a structural diagram of the pressure regulating component;
[0023] Figure 8 It is a schematic diagram of the local structure of the pressure regulating component;
[0024] Figure 9 It is a partial cross-sectional view of the pressure regulating assembly;
[0025] Figure 10 It is a structural schematic diagram of the feeding part in the present invention.
[0026] Reference numerals: 1, feed member; 101, mounting frame 2; 102, discharge tank; 103, feed pipe 2; 104, sample pump; 2, housing; 3, discharge member; 4, reaction cylinder; 401, feed pipe 1; 402, discharge pipe; 403, drive structure 1; 40301, motor 1; 40302, gear 1; 40303, gear 2; 5, microchannel reaction member; 501, connector; 6, pressure regulating group Parts; 601, connecting pipe; 602, pressure regulating cylinder; 603, piston plate; 604, filter screen; 605, deformable membrane; 606, airbag bag; 607, adjusting ring; 608, extrusion part; 609, gear three; 610, gear four; 611, motor two; 7, drive structure two; 701, adjusting rod; 702, drive box; 703, moving block; 704, mounting bracket one; 705, fixing rod. DETAILED DESCRIPTION
[0027] Example 1, as Figure 1-Figure 3As shown, the present invention proposes a microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole, comprising a reaction barrel 4, a feed member 1, a discharge member 3, a microchannel reaction member 5, and a pressure regulating assembly 6. The reaction barrel 4 passes through the housing 2 along the length direction and is driven by a driving structure 1 403 to be rotatably connected to the housing 2. A feed pipe 1 401 is provided at one end, and a discharge pipe 402 is provided at the other end. The feed member 1 is located on one side of the housing 2 and is connected to the feed pipe 1 401. The discharge member 3 is located on the other side of the housing 2 and is connected to the discharge pipe 402. The microchannel reaction member 5 is composed of a plurality of reaction plates forming a micro-reaction flow channel, and the microchannel reaction members 5 are arranged in pairs in the reaction barrel 4. Each pair of microchannel reaction members 5 is driven by a driving structure 2 7 to rotate in the horizontal direction. On the one hand, it opens and closes, and on the other hand, it rotates with the reaction cylinder 4; the two adjacent pairs of microchannel reaction parts 5 open and close synchronously and in opposite directions; the two outermost groups of microchannel reaction parts 5 are respectively connected to the feed pipe 401 and the discharge pipe 402; the pressure regulating component 6 is fixed between each pair of microchannel reaction parts 5. As the microchannel reaction parts 5 on both sides open and close, the air inside the pressure regulating component 6 is synchronously squeezed or stretched, and the circulating reagents are pressurized in sections. On the one hand, the pressurization of the reagents can accelerate their mixing and promote the reaction, and on the other hand, it can dredge the microreaction flow channel.
[0028] It should be further explained that the space between the outer shell 2 and the reaction tube 4 is filled with a heat-insulating agent; the temperature-controlling agent can be oil. The temperature range required for the preparation of 1-methyl-3-trifluoromethyl-5-hydroxypyrazole is around 40°C. The reaction temperature is controlled by heating the oil to promote the smooth completion of the reaction.
[0029] like Figure 4 As shown, drive structure 1 403 is located at each end of reaction barrel 4 and includes gear 1 40302, which is driven by motor 1 40301. Gear 2 40303 is sleeved on the outer periphery of reaction barrel 4 and meshes with gear 1 40302. By driving drive structure 1 403 to rotate reaction barrel 4 about its origin, microchannel reaction element 5 is synchronously rotated. This rotation facilitates mixing of reaction reagents and maintains temperature stability.
[0030] like Figure 5 As shown, the driving structure 2 7 includes an adjusting rod 701 arranged along the length direction of the reaction cylinder 4 and driven to rotate by a driving box 702; the adjusting rod 701 has corresponding adjusting sections arranged logarithmically corresponding to the microchannel reaction element 5; the paired moving blocks 703 realize opening and closing movement by respectively threadedly connecting the two ends of the adjusting sections; the mounting frame 1 704 is clamped on the outside of the microchannel reaction element 5 and is connected to the moving blocks 703 one by one.
[0031] It should be further explained that opposite threads are provided at both ends of each adjustment section, and the moving blocks 703 at both ends are driven to move open and close through the threaded connection.
[0032] It should be further explained that after the fixing rod 705 passes through the microchannel reaction piece 5 from the periphery, the end portion passes through the mounting frame 1 704 and is further tightened by a nut, thereby further locking the microchannel reaction piece 5, reducing its leakage and facilitating the adjustment of its movement.
[0033] It should be further explained that the mounting frame 704 is a U-shaped structure.
[0034] By driving the second structure 7, the horizontal opening and closing movement of each pair of microchannel reaction elements 5 can be realized, and the opening and closing of two adjacent pairs of microchannel reaction elements 5 are synchronized but in opposite directions. In other words, a cycle of squeezing-pulling-squeezing-pulling the air on the inner wall of the pressure regulating component 6 is formed, so that the reagent flow is continuous and the segmented pressurization is efficient.
[0035] like Figure 6 As shown, connectors 501 connecting the head end and the tail end of the micro-reaction flow channel are respectively provided on both sides of the microchannel reaction element 5; the frontmost connector 501 is connected to the feed pipe 401, the rearmost connector 501 is connected to the discharge pipe 402, and the remaining connectors 501 are connected to the pressure regulating component 6.
[0036] like Figure 7-Figure 9 As shown, the pressure regulating assembly 6 includes two sets of connecting tubes 601 respectively connected to the joints 501 on the front and rear microchannel reaction elements 5; the opposite ends of the two sets of connecting tubes 601 slide into the pressure regulating cylinder 602 from both ends and are connected to the piston plate 603 with a one-way valve.
[0037] It should be further explained that the one-way valves on the two sets of piston plates 603 control the reagent to enter from one side and exit from the other side; the filter screen 604 is arranged between the two sets of piston plates 603.
[0038] As the front pair of microchannel reaction elements 5 move together, the rear pair of microchannel reaction elements 5 simultaneously move apart. The two sets of connecting tubes 601 on the pressure regulating assembly 6 between the front pair of microchannel reaction elements 5 drive the two sets of piston plates 603 together, squeezing the air within the pressure regulating cylinder 602. The reagent is rapidly filtered and transferred to the rear pair of microchannel reaction elements 5. Simultaneously, the two sets of connecting tubes 601 on the pressure regulating assembly 6 between the rear pair of microchannel reaction elements 5 drive the two sets of piston plates 603 apart, stretching the air within the pressure regulating cylinder 602. The reagent originally in the rear pair of microchannel reaction elements 5 flows into the pressure regulating cylinder 602. This alternating flow of reagents transfers the reagents from the water inlet to the water outlet. During this transfer process, the reagents are pressurized and filtered in stages. This not only maintains a dynamic flow rate of the reagents, reduces clogging in the microreaction channels, but also promotes the mixing reaction. It also promptly filters impurities and agglomerated reagents generated during the reaction, further reducing the occurrence of clogging in the microreaction channels.
[0039] It should be further explained that the filter screen 604 is a flexible filter screen for the dispersed 1-methyl-3-trifluoromethyl-5-hydroxypyrazole powder to pass through; a circle of deformable membrane 605 connected to the edge of the flexible filter screen is provided on the side wall of the pressure regulating cylinder 602, and a circle of rotatable adjustment ring 607 is also provided on the periphery of the pressure regulating cylinder 602; the airbag bags 606 are covered one by one on the deformable membrane 605 and filled with gas; the extrusion piece 608 is provided on the adjustment ring 607, and as the adjustment ring 607 rotates, the airbag bags 606 are squeezed in turn.
[0040] To clean the filter 604, rotating the pressure regulating cylinder 602 drives the extrusion element 608 to rotate synchronously, squeezing the airbags 606 in turn. The deformable membrane 605 deforms under the pressure of the gas, driving the deformation of the filter 604 and thus cleaning it. Furthermore, the cleaning process squeezes the reagent inside, achieving localized pressurization, dispersing agglomerated products and intercepting large debris, thereby improving the cleaning effect.
[0041] It should be further explained that extrusion pieces 608 are arranged at intervals on the side walls of the adjustment ring 607; the end of the adjustment ring 607 is sleeved with gear three 609, and one side is provided with gear four 610 driven to rotate by motor two 611; gear three 609 is engaged with gear four 610 and is rotatably connected to the pressure regulating cylinder 602; the extrusion piece 608 is wheel-shaped and can generate heat when powered.
[0042] Gears 3 609 and 4 610 work together to drive the adjustment ring 607 to rotate. The extrusion member 608 moves synchronously with the adjustment ring 607. During this movement, the airbag 606 repeatedly deforms and recovers, producing a cleaning and pressurizing effect. Simultaneously, the extrusion member 608 heats the air inside the airbag 606, causing it to expand and further enhance the squeezing effect.
[0043] like Figure 10 As shown, the feed unit 1 includes a second mounting frame 101; multiple groups of discharge tanks 102 are arranged within the second mounting frame 101, and sampling pumps 104 are provided on the second mounting frame 101, each connected to each of the multiple groups of discharge tanks 102. Each sampling pump 104 cooperates with a corresponding second feeding tube 103 to transfer the corresponding reagent to the first feeding tube 401. By setting up independent sampling, premature reaction of the reagent is avoided while ensuring the accuracy of the sampling.
[0044] It should be further explained that the discharge tank 102 is provided with three groups, which are used to place methylhydrazine aqueous reagent (40%), acetic acid and ethyl trifluoroacetoacetate respectively.
[0045] Example 2: This example is based on a microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole in Example 1, and proposes a method for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole. The steps are as follows:
[0046] S1, the sampling pump 104 respectively adds methylhydrazine aqueous reagent (40%) and acetic acid and ethyl trifluoroacetoacetate into the reaction cylinder 4 in proportion;
[0047] S2. The driving structure 403 drives the reaction cylinder 4 to rotate at its origin, thereby driving the microchannel reaction element 5 to rotate synchronously, thereby achieving the purpose of mixing the reaction reagents.
[0048] S3. The reagents pass through the paired microchannel reaction elements 5 in sequence; the driving structure 2 7 drives each pair of microchannel reaction elements 5 to open and close horizontally, and the adjacent pairs of microchannel reaction elements 5 open and close synchronously but in opposite directions; as the front pair of microchannel reaction elements 5 moves together, the rear pair of microchannel reaction elements 5 moves apart synchronously. The two sets of connecting tubes 601 on the pressure regulating assembly 6 between the front pair of microchannel reaction elements 5 drive the two sets of piston plates 603 to move together, squeezing the air in the pressure regulating cylinder 602. The reagents are quickly filtered and transferred to the rear pair of microchannel reaction elements 5; at the same time, the two sets of connecting tubes 601 on the pressure regulating assembly 6 between the rear pair of microchannel reaction elements 5 drive the two sets of piston plates 603 to move apart, stretching the air in the pressure regulating cylinder 602. The reagents originally in the rear pair of microchannel reaction elements 5 flow into the pressure regulating cylinder 602.
[0049] S4: The filter 604 intercepts large debris and agglomerated products. By rotating the pressure regulating cylinder 602, the extrusion member 608 is driven to rotate synchronously, thereby squeezing the airbags 606 in sequence. The extrusion member 608 heats the air inside the airbags 606, causing them to expand in volume. The deformable membrane 605 deforms under the pressure of the gas, driving the filter 604 to deform, thereby achieving the purpose of cleaning and locally pressurizing the airbags to disperse the products.
[0050] S5. By alternately feeding and discharging reagents, the reagents are transferred from the water inlet to the water outlet in sections. During the transfer process, the reagents are pressurized and filtered in sections to complete the corresponding chemical reaction. At the same time, in order to ensure the reaction effect, the oil is heated and the reaction temperature is controlled to be maintained at around 40°C.
[0051] S6. The prepared 1-methyl-3-trifluoromethyl-5-hydroxypyrazole enters the discharge part 3.
[0052] The embodiments of the present invention are described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Various changes can be made within the scope of knowledge possessed by those skilled in the art without departing from the spirit of the present invention.
Claims
1. A microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole, characterized in that: include: A reaction cylinder (4), the reaction cylinder (4) passes through the shell (2) along the length direction and is driven by a driving structure (403) to be rotatably connected to the shell (2), with a feed pipe (401) provided at one end and a discharge pipe (402) provided at the other end; A feed piece (1), the feed piece (1) is located on one side of the housing (2) and is connected to a feed pipe (401); A discharge member (3), the discharge member (3) is located on the other side of the housing (2) and is connected to the discharge pipe (402); A microchannel reaction member (5), wherein the microchannel reaction member (5) is composed of a plurality of reaction plates forming a microreaction flow channel, and the microchannel reaction members (5) are arranged in pairs in the reaction barrel (4), and each pair of microchannel reaction members (5) is driven by a second driving structure (7) to open and close in the horizontal direction on the one hand, and rotates with the reaction barrel (4) on the other hand; two adjacent pairs of microchannel reaction members (5) open and close synchronously and in opposite directions; the two outermost groups of microchannel reaction members (5) are respectively connected to a first feed pipe (401) and a discharge pipe (402); And a pressure regulating assembly (6), the pressure regulating assembly (6) is fixed between each pair of microchannel reaction parts (5), and as the microchannel reaction parts (5) on both sides open and close, the air inside the pressure regulating assembly (6) is synchronously squeezed or stretched, thereby pressurizing the circulating reagent in sections.
2. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 1, characterized in that: The space between the outer shell (2) and the reaction cylinder (4) is filled with a heat-insulating agent.
3. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 1, characterized in that: The driving structure 1 (403) is respectively located at both ends of the reaction tube (4), and includes a gear 1 (40302) driven to rotate by the motor 1 (40301); the gear 2 (40303) is sleeved on the outer periphery of the reaction tube (4) and meshes with the gear 1 (40302).
4. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 1, characterized in that: The second driving structure (7) includes an adjusting rod (701) arranged along the length direction of the reaction cylinder (4) and driven to rotate by a driving box (702); the adjusting rod (701) has corresponding adjusting sections arranged in a logarithm corresponding to the microchannel reaction element (5); the paired moving blocks (703) are respectively threadedly connected to the two ends of the adjusting sections to achieve opening and closing movement; the first mounting frame (704) is clamped on the outside of the microchannel reaction element (5) and is connected to the moving blocks (703) in a one-to-one correspondence.
5. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 1, characterized in that: Connectors (501) are provided on both sides of the microchannel reaction element (5) for connecting the head end and the tail end of the microreaction flow channel; the frontmost connector (501) is connected to the feed pipe (401), the rearmost connector (501) is connected to the discharge pipe (402), and the remaining connectors (501) are connected to the pressure regulating assembly (6); The pressure regulating assembly (6) includes two sets of connecting pipes (601) connected to the upper joints (501) of the front and rear microchannel reaction parts (5) respectively; the opposite ends of the two sets of connecting pipes (601) slide into the pressure regulating cylinder (602) from both ends and are connected to the piston plate (603) with a one-way valve; The one-way valves on the two sets of piston plates (603) control the reagent to enter from one side and exit from the other side; The filter screen (604) is arranged between the two sets of piston plates (603).
6. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 5, characterized in that: The filter screen (604) is a flexible filter screen; a deformable membrane (605) is provided on the side wall of the pressure regulating cylinder (602) and is connected to the edge of the flexible filter screen; a rotatable adjustment ring (607) is also provided on the periphery of the pressure regulating cylinder (602); The airbag bags (606) are covered on the deformable membrane (605) in a one-to-one correspondence and are filled with gas; The extrusion member (608) is arranged on the adjustment ring (607) and sequentially squeezes the airbag bags (606) as the adjustment ring (607) rotates.
7. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 6, characterized in that: Extrusion members (608) are spaced apart on the side wall of the adjusting ring (607); the end of the adjusting ring (607) is sleeved with gear three (609), and one side is provided with gear four (610) driven to rotate by motor two (611); gear three (609) is meshedly connected to gear four (610) and is rotationally connected to the pressure regulating cylinder (602); The extrusion piece (608) is wheel-shaped and can generate heat when powered.
8. The microchannel reactor for preparing 1-methyl-3-trifluoromethyl-5-hydroxypyrazole according to claim 1, characterized in that: The feed component (1) includes a second mounting frame (101); a plurality of discharge tanks (102) are arranged in the second mounting frame (101); and a sampling pump (104) connected to the plurality of discharge tanks (102) in a one-to-one correspondence is arranged on the second mounting frame (101); each sampling pump (104) transfers the corresponding reagent to the first feeding pipe (401) by cooperating with the corresponding second feeding pipe (103).
Citation Information
Patent Citations
A kind of anti-clogging microchannel reactor
CN117282395B
Microchannel reactor, device and method for preparing 5-fluorocytosine
CN107670603A
Micro-channel reactor for synthesizing nitrochlorobenzene
CN114432983A