Multi-channel microjet impinging mixer
The multi-channel microjets impact mixer achieves uniform mixing of formamide and hydrazine hydrate through spiral heating and impact mechanism, solving the problems of thermal runaway, side reactions and low efficiency in the synthesis of triazole, and improving product purity and production efficiency.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-30
- Publication Date
- 2026-04-03
AI Technical Summary
Existing triazole synthesis processes suffer from the risk of thermal runaway, side reactions caused by excessively high concentrations of hydrazine hydrate in localized areas, unsuitable reaction temperatures, and low production efficiency.
A multi-channel micro-jet impact mixer is used to preheat formamide through a spiral heating tube. The impact mechanism enables formamide and hydrazine hydrate to be instantaneously impacted and mixed without interruption or concentration fluctuation in the mixing chamber, achieving uniform contact throughout the process, suppressing the generation of by-products, and realizing continuous production through a continuous feeding and collection mechanism.
It improves the safety and purity of triazole synthesis, reduces the difficulty and cost of separation and purification, meets the optimal reaction temperature requirements, and improves production efficiency.
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Figure CN121775796A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of triazole synthesis technology, and particularly to a multichannel microjet impingement mixer. Background Technology
[0002] 1,2,4-1H-triazole is a key intermediate in the pharmaceutical, pesticide and dye fields, and its synthesis mainly depends on the cyclization reaction of formamide and hydrazine hydrate.
[0003] Traditional processes commonly employ a batch synthesis mode in a reactor. For example, Chinese Patent No. CN219024311U discloses a high-efficiency triazole synthesis system. This system includes a triazole synthesis reactor equipped with a hydrazine hydrate inlet and a formamide inlet, each connected to a separate inlet pipe. Multiple control valves are installed on both the hydrazine hydrate and formamide inlets. An outlet is located at the bottom of the reactor. The reactor is also connected to a packed tower, with a first condenser at the top. The first condenser is connected to the inner cavity of the packed tower and contains a temperature monitoring device. The outlet of the first condenser is connected to a reactant recycling device. During synthesis, an intermittent dropping method is used, transferring formamide into the triazole synthesis reactor and then uniformly adding hydrazine hydrate.
[0004] However, the above-mentioned synthesis method based on a synthesis reactor has the following drawbacks: First, the synthesis process requires storing a large amount of formamide and hydrazine hydrate mixture under high-temperature conditions. The large material holding capacity makes it highly susceptible to thermal runaway due to heat accumulation, resulting in insufficient safety. Second, in the intermittent dropping method, the initial addition of hydrazine hydrate results in a high concentration of formamide in the synthesis reactor. However, as the amount of hydrazine hydrate added increases, the formamide concentration in the reactor continuously decreases, preventing uniform contact between hydrazine hydrate and formamide throughout the process. This leads to excessively high concentrations of hydrazine hydrate in localized areas, which can easily trigger a hydrazine hydrate self-condensation side reaction (referred to as a hydrazine-hydrazine side reaction), generating 4-amino-1,2,4-triazole impurities. This not only reduces the purity of the main product but also increases the difficulty of subsequent separation and purification. Third, the optimal reaction temperature for triazole synthesis is 170-180℃; otherwise, the generation of 4-amino-1,2,4-triazole impurities increases. The reaction between formamide and hydrazine hydrate is exothermic. However, as the reaction proceeds, the heat of reaction is insufficient to expel the generated water from the synthesis vessel. An external heat source is needed to provide a large amount of heat to maintain the synthesis temperature of triazole. The current method is to reduce the dropping rate of hydrazine hydrate and heat the materials inside the reactor. In reality, the reaction temperature can only be achieved at 150-165 °C, which is not the optimal reaction temperature. The 4-amino-1,2,4-triazole has high impurity levels, and although the produced triazole undergoes subsequent crystallization purification, it is still difficult to meet pharmaceutical requirements in a single reaction. Furthermore, the reaction time for 1 ton of hydrazine hydrate is approximately 15-20 hours, which is inefficient. Summary of the Invention
[0005] The present invention provides a multi-channel micro-jet impingement mixer to solve at least one of the technical problems mentioned in the background art.
[0006] To address the aforementioned technical problems, this invention discloses a multi-channel micro-jet impact mixer, comprising: a mixing cylinder and a collecting cylinder, the upper end of the collecting cylinder being connected to the lower end of the mixing cylinder; a heating jacket being disposed outside the mixing cylinder; a spiral heating tube being disposed inside the heating jacket; a formamide inlet pipe being connected to the lower end of the spiral heating tube; an impact mechanism being disposed inside the mixing cylinder; the impact mechanism including a partition plate being fixedly disposed inside the mixing cylinder; a hydrazine hydrate diverter being rotatably disposed at the center of the upper surface of the partition plate; the upper end of the hydrazine hydrate diverter being rotatably and sealingly connected to the top wall of the mixing cylinder; a mixing cavity being formed between the outer wall of the hydrazine hydrate diverter and the inner wall of the mixing cylinder; and several through holes being disposed through the partition plate, the upper ends of which being connected to the mixing cavity. The mixing cylinder has several first channels evenly arranged on its side wall. An annular liquid inlet chamber is provided on the inner wall of the upper end of the mixing cylinder. Several second channels are provided at the lower end of the annular liquid inlet chamber. A formamide distribution pipe is provided at the lower end of the second channel. The formamide distribution pipe is located in the mixing chamber. Several atomizing nozzles are connected to the side wall of the formamide distribution pipe. A first delivery pump and a second delivery pump are provided at the upper end of the mixing cylinder. The input end of the first delivery pump is connected to the hydrazine hydrate inlet pipe. The output end of the first delivery pump is connected to the upper end of the hydrazine hydrate distribution cylinder through the liquid inlet hole. The input end of the second delivery pump is connected to the upper end of the spiral heating pipe through the delivery pipe. The output end of the second delivery pump is connected to the annular liquid inlet chamber through the delivery channel.
[0007] Preferably, the heating jacket includes a heat-conducting jacket and two heat-insulating rings. The heat-conducting jacket is fitted onto the outer wall of the mixing cylinder. The outer wall of the heat-conducting jacket is provided with a first mounting groove adapted to the spiral heating tube. The two heat-insulating rings are assembled on the outside of the heat-conducting jacket. The heat-insulating rings are semi-circular ring structures. The inner wall of the heat-insulating rings is provided with a second mounting groove adapted to the spiral heating tube. Connecting ears are provided at the front and rear ends of the heat-insulating rings respectively. The front and rear ends of the two heat-insulating rings are connected through the connecting ears.
[0008] Preferably, a third mounting groove is provided on the side of the first mounting groove near the mixing cylinder. The third mounting groove is spiral-shaped, and a heating strip is provided inside the third mounting groove. The heating strip is connected to the outer wall of the spiral heating tube.
[0009] Preferably, an impact block is fixedly installed at the center of the bottom wall of the hydrazine hydrate distributor. The impact block is located directly below the liquid inlet, and the impact block is hemispherical with its arc surface facing the liquid inlet.
[0010] Preferably, the bottom wall of the hydrazine hydrate diverter is provided with several arc-shaped blades, which are arranged in a ring array about the central axis of the hydrazine hydrate diverter.
[0011] Preferably, several second channels are arranged in a ring array about the center of the annular liquid inlet chamber, the formamide diversion tube is vertically set, the atomizing nozzles are equally spaced along the axial direction of the formamide diversion tube, and the spray direction of the atomizing nozzles is tangent to the outer wall of the formamide diversion tube.
[0012] Preferably, a collection hood is provided below the partition, and the lower end of the through hole is connected to the inside of the collection hood, which is funnel-shaped.
[0013] Preferably, a mixing mechanism is provided at the lower end of the collection hood. The mixing mechanism includes a third delivery pump. The input end of the third delivery pump is connected to the lower end of the collection hood. An overflow cylinder is provided below the third delivery pump. The overflow cylinder is cylindrical and horizontally positioned. The outside of the overflow cylinder is fixedly connected to the inner wall of the mixing cylinder through a fixing plate. A three-way pipe is provided at the output end of the third delivery pump. The three-way pipe includes an input pipe and two output pipes. The three-way pipe is connected to the output end of the third delivery pump through the input pipe. The two output pipes of the three-way pipe are respectively connected to the upper part of the overflow cylinder. The two output pipes are horizontally positioned and the liquid outlet direction of the two output pipes is on the same horizontal plane. Two rotating shafts are symmetrically arranged inside the overflow cylinder. The front and rear ends of the rotating shafts are rotatably connected to the inner walls of the front and rear sides of the overflow cylinder, respectively. Several stirring blades are provided on the outer wall of the rotating shafts. Two overflow holes are provided on the side wall of the overflow cylinder. The overflow holes are located at the lower part of the overflow cylinder. A drain pipe is provided at the bottom of the overflow cylinder. A first valve is provided on the drain pipe.
[0014] Preferably, a gas outlet pipe is provided on the side wall of the collection cylinder, one end of which extends into the collection hood and communicates with the upper end of the collection hood, and the other end of which extends to the outside of the collection cylinder and is equipped with an air pump.
[0015] Preferably, the collecting cylinder is funnel-shaped, with a guide pipe at the lower end of the collecting cylinder and a second valve at the lower end of the guide pipe.
[0016] The technical solution of this invention has the following advantages: This invention provides a multi-channel microjets impact mixer, relating to the field of triazole synthesis technology, comprising: a mixing cylinder and a collecting cylinder; a heating jacket is provided outside the mixing cylinder; a spiral heating tube is provided inside the heating jacket; the lower end of the spiral heating tube is connected to a formamide inlet pipe; an impact mechanism is provided inside the mixing cylinder; the impact mechanism includes a partition plate, which is fixedly installed inside the mixing cylinder; a hydrazine hydrate distribution cylinder is rotatably installed at the center of the upper surface of the partition plate; the upper end of the hydrazine hydrate distribution cylinder is rotatably and sealingly connected to the top wall of the mixing cylinder; a mixing cavity is formed between the outer wall of the hydrazine hydrate distribution cylinder and the inner wall of the mixing cylinder; several first channels are uniformly arranged on the side wall of the hydrazine hydrate distribution cylinder; an annular inlet cavity is provided on the upper inner wall of the mixing cylinder; and several second channels are provided at the lower end of the annular inlet cavity. In this invention, by setting the impact mechanism, formamide and hydrazine hydrate can be instantaneously impacted and mixed without interruption or concentration fluctuation in the mixing cavity of the mixing cylinder, thereby achieving uniform contact throughout the entire process of formamide and hydrazine hydrate synthesis, suppressing the generation of by-products, increasing the concentration of the main product, and reducing the difficulty and cost of subsequent separation and purification.
[0017] Other features and advantages of the invention will be set forth in the description which follows, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention may be realized and obtained by means of the means particularly pointed out in the written description and the accompanying drawings.
[0018] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description
[0019] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings: Figure 1 This is a schematic diagram of the internal structure of the multi-channel microjet impact mixer of the present invention; Figure 2 This is a top view of the heating sleeve in this invention; Figure 3 This is a top view of the partition in this invention; Figure 4 For the present invention Figure 1 Enlarged view of the structure at point A in the middle; Figure 5 For the present invention Figure 1 Enlarged view of the structure at point B in the middle.
[0020] In the diagram: 1. Mixing cylinder; 2. Collecting cylinder; 3. Spiral heating tube; 4. Formamide inlet pipe; 5. Baffle; 6. Hydrazine hydrate diverter; 61. Arc-shaped blade; 7. Mixing chamber; 8. Through hole; 9. First channel; 10. Annular inlet chamber; 11. Second channel; 12. Formamide diverter; 13. Atomizing nozzle; 14. First delivery pump; 15. Second delivery pump; 16. Hydrazine hydrate inlet pipe; 17. Inlet hole ; 18. Conveying pipe; 19. Conveying channel; 20. Heat-conducting sleeve; 21. Insulation ring; 22. Connecting ear; 23. Third mounting slot; 24. Heating strip; 25. Impact block; 26. Collection cover; 27. Third conveying pump; 28. Overflow cylinder; 29. Fixing plate; 30. T-shaped pipe; 31. Rotating shaft; 32. Stirring blade; 33. Overflow hole; 34. Drain pipe; 35. Gas outlet pipe; 36. Guide pipe. Detailed Implementation
[0021] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.
[0022] Furthermore, in this invention, the use of terms such as "first" and "second" is for descriptive purposes only and does not specifically refer to any order or sequence, nor is it intended to limit the invention. They are merely used to distinguish components or operations described using the same technical terms and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the technical solutions and features of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. If a combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.
[0023] Example 1: This embodiment of the invention provides a multi-channel microjets impact mixer, such as... Figures 1-5 As shown, the system includes: a mixing cylinder 1 and a collecting cylinder 2. The upper end of the collecting cylinder 2 is connected to the lower end of the mixing cylinder 1. A heating jacket is installed outside the mixing cylinder 1, and a spiral heating tube 3 is installed inside the heating jacket. The lower end of the spiral heating tube 3 is connected to a formamide inlet pipe 4. An impact mechanism is installed inside the mixing cylinder 1. The impact mechanism includes a partition plate 5, which is fixedly installed inside the mixing cylinder 1. A hydrazine hydrate diverter 6 is rotatably installed at the center of the upper surface of the partition plate 5. The upper end of the hydrazine hydrate diverter 6 is rotatably and sealingly connected to the top wall of the mixing cylinder 1. A mixing cavity 7 is formed between the outer wall of the hydrazine hydrate diverter 6 and the inner wall of the mixing cylinder 1. Several through holes 8 are provided through the partition plate 5, and the upper ends of the through holes 8 are connected to the mixing cavity 7. Several first channels 9 are evenly provided on the side wall of the hydrazine hydrate diverter 6. An annular liquid inlet chamber 10 is provided on the inner wall of the upper end of the mixing cylinder 1. Several second channels 11 are provided at the lower end of the annular liquid inlet chamber 10. A formamide diversion pipe 12 is provided at the lower end of the second channel 11. The formamide diversion pipe 12 is located in the mixing chamber 7. Several atomizing nozzles 13 are connected to the side wall of the formamide diversion pipe 12. A first delivery pump 14 and a second delivery pump 15 are provided at the upper end of the mixing cylinder 1. The input end of the first delivery pump 14 is connected to the hydrazine hydrate inlet pipe 16. The output end of the first delivery pump 14 is connected to the upper end of the hydrazine hydrate diversion cylinder 6 through the liquid inlet hole 17. The input end of the second delivery pump 15 is connected to the upper end of the spiral heating pipe 3 through the delivery pipe 18. The output end of the second delivery pump 15 is connected to the annular liquid inlet chamber 10 through the delivery channel 19.
[0024] The working principle and beneficial effects of the above technical solution are as follows: The mixing cylinder 1, collecting cylinder 2, and spiral heating tube 3 can be made of Hastelloy alloy (preferably Hastelloy C-276 / C-22), which can withstand high temperatures of not less than 200℃, thus adapting to high-temperature reaction conditions. The formamide inlet pipe 4 is connected to a first container outside the mixer, which stores room-temperature formamide liquid. The hydrazine hydrate inlet pipe 16 is connected to a second container outside the mixer, which stores room-temperature hydrazine hydrate liquid. When the mixer is working, the second delivery pump 15 introduces formamide into the spiral heating tube 3 inside the heating jacket through the formamide inlet pipe 4. The spiral heating tube 3 is provided with a spiral flow channel, which allows the formamide to flow spirally upward along the spiral flow channel and gradually heat up to 160℃-180℃ during the flow. Then, it quickly enters the annular inlet chamber 10 at the upper end of the mixing cylinder 1 through the delivery channel 19. When the annular inlet chamber 10 is filled with formamide, the formamide in the annular inlet chamber 10 is diverted through the second channel 11. The formamide is directed to the formamide distribution pipe 12, where it is atomized by the atomizing nozzle 13 on the side wall and evenly sprayed into the mixing chamber 7. Simultaneously, the first delivery pump 14 is activated, pressurizing the hydrazine hydrate at room temperature and delivering it to the hydrazine hydrate distribution cylinder 6 through the inlet port 17. The molar ratio of formamide to hydrazine hydrate is controlled within the range of 4:1 to 6:1. Both the second delivery pump 15 and the first delivery pump 14 are high-temperature and high-pressure metering pumps, injecting formamide and hydrazine hydrate into the mixing cylinder at a pressure of 1.2-1.5 MPa. 1. Initial high pressure is formed within the mixing chamber 7. Hydrazine hydrate diffuses after impacting the bottom wall of the hydrazine hydrate distributor 6, and then is uniformly ejected through several first channels 9 on the side wall of the hydrazine hydrate distributor 6. The ejected hydrazine hydrate and atomized formamide instantaneously converge within the annular mixing chamber 7, allowing the formamide and hydrazine hydrate to be uniformly mixed within milliseconds, simultaneously initiating a cyclization reaction to generate 1H-1,2,4-triazole, water, and ammonia. The reaction equation is: C2H5NO + NH2NH 2·H2O→C2H3N3+2H2O+NH3; The product after the mixed reaction flows rapidly through the through-hole 8 on the partition 5 to the area below the partition 5, and finally flows into the collection cylinder 2, so that the product will not remain in the mixing chamber 7 for a long time, realizing continuous product collection; In this embodiment, the formamide is continuously preheated by the spiral heating tube 3, which eliminates the need to store a large amount of formamide and hydrazine hydrate mixture at high temperature, avoids the risk of thermal runaway caused by the accumulation of high temperature materials, and improves safety performance. In addition, by setting an impact mechanism, the formamide passes through the atomizing nozzle 1 3. The formation of micro-droplets increases the contact area between formamide and hydrazine hydrate. The hydrazine hydrate, through the uniformly distributed first channel 9, achieves a uniform micro-jet flow. This micro-jet flow of hydrazine hydrate reacts with formamide, allowing for seamless and instantaneous collision mixing of formamide and hydrazine hydrate within the mixing chamber 7 of the mixing cylinder 1. This solves the problem of formamide concentration fluctuations, thereby achieving uniform contact throughout the entire synthesis process of formamide and hydrazine hydrate. This effectively suppresses hydrazine-hydrazine side reactions, significantly reduces the formation of 4-amino-1,2,4-triazole impurities, and promotes the production of the main product 1,2... The purity of 4-1H-triazole is significantly improved, reducing the difficulty and cost of subsequent separation and purification. Optimally, the heating temperature for formamide is 170℃. Since the reaction between formamide and hydrazine hydrate is exothermic, the microfluidic reaction—where a microfluidic jet of hydrazine hydrate achieves instantaneous molecular-level contact with atomized formamide—leads to a rapid increase in the cyclization rate and a highly concentrated exothermic effect. Without the need for additional external heating, the reaction temperature naturally rises to the optimal range of 170-180℃, not only meeting the optimal reaction temperature requirements for triazole synthesis but also maximizing the inhibition of 4-1H-triazole. AT impurities are generated, and since formamide only needs to be preheated to 170℃ (before reaching the decomposition temperature), the stability of the raw materials and the purity of the main product are ensured. The first delivery pump 14 realizes the continuous feeding of hydrazine hydrate, and the second delivery pump 15 realizes the continuous feeding of formamide, thereby continuously carrying out the cyclization reaction. The mixing chamber 7 and the collecting cylinder 2 are seamlessly connected, so that the reaction products can be continuously discharged through the collecting cylinder 2, forming a continuous production process without the need for intermittent operation. This solves the problem of low efficiency of traditional intermittent production in reactors and is more suitable for the needs of large-scale industrial synthesis.
[0025] Example 2: Based on Example 1 above, as follows Figure 1 , Figure 2 As shown, the heating jacket includes a heat-conducting jacket 20 and two heat-insulating rings 21. The heat-conducting jacket 20 is fitted onto the outer wall of the mixing cylinder 1. The outer wall of the heat-conducting jacket 20 is provided with a first mounting groove that is compatible with the spiral heating tube 3. The two heat-insulating rings 21 are assembled on the outside of the heat-conducting jacket 20. The heat-insulating rings 21 are semi-circular rings. The inner wall of the heat-insulating rings 21 is provided with a second mounting groove that is compatible with the spiral heating tube 3. Connecting ears 22 are provided at the front and rear ends of the heat-insulating rings 21 respectively. The front and rear ends of the two heat-insulating rings 21 are connected through the connecting ears 22. A third mounting groove 23 is provided on the side of the first mounting groove near the mixing cylinder 1. The third mounting groove 23 is spiral in shape, and a heating strip 24 is provided inside the third mounting groove 23. The heating strip 24 is connected to the outer wall of the spiral heating tube 3.
[0026] The working principle and beneficial effects of the above technical solution are as follows: During installation, the heat-conducting sleeve 20 is first fixedly installed on the outer wall of the mixing cylinder 1, then the heating strip 24 is installed on the outer wall of the spiral heating tube 3. Next, the spiral heating tube 3 is installed in the first mounting groove of the heat-conducting sleeve 20, and the heating strip 24 is located in the third mounting groove 23. Finally, the two heat-insulating rings 21 are joined together and wrapped inside the heat-conducting sleeve 20. The second mounting groove on the inner wall of the heat-insulating ring 21 is precisely matched with the spiral heating tube 3. The connecting ears 22 at both ends of the heat-insulating ring 21 are fixed by bolts to ensure good sealing after joining. When the mixer is working, the heating strip 24 is activated. The heating strip 24 can transfer heat to the spiral heating tube 3. When formamide flows in the spiral heating tube 3, it can be heated to 160℃-18℃. At 0℃, the formamide is preheated. At the same time, the heat-conducting sleeve 20 is tightly fitted on the outer wall of the mixing cylinder 1. The heat-conducting sleeve 20 is made of a high thermal conductivity material. The heating strip 24 is in contact with the heat-conducting sleeve 20, and the heat-conducting sleeve 20 can synchronously conduct the heat generated by the heating strip 24 to the mixing cylinder 1, thereby maintaining the reaction temperature of 160℃-180℃ in the mixing cylinder 1. This avoids the decrease in reaction efficiency or the increase of by-products caused by temperature fluctuations in the mixing chamber 7. The heat generated by the heating strip 24 can be evenly transferred to the spiral heating tube 3 and the mixing cylinder 1, so that the mixing cylinder 1 does not need additional heating equipment, reducing the preparation cost. Two heat-insulating rings 21 are set on the outside of the heat-conducting sleeve 20. The heat-insulating rings 21 are made of high temperature resistant heat-insulating material, which can reduce heat loss and improve energy utilization.
[0027] Example 3: Based on Example 1 or 2, such as Figure 1 , Figure 3 As shown, an impact block 25 is fixedly installed at the center of the bottom wall of the hydrazine hydrate diverter 6. The impact block 25 is located directly below the liquid inlet 17. The impact block 25 is hemispherical, and the arc surface of the impact block 25 faces the liquid inlet 17. The bottom wall of the hydrazine hydrate diverter 6 is provided with several arc-shaped blades 61, which are arranged in a ring array about the central axis of the hydrazine hydrate diverter 6.
[0028] The working principle and beneficial effects of the above technical solution are as follows: After being pressurized by the first delivery pump 14, the hydrazine hydrate is sprayed downward through the inlet hole 17. The sprayed hydrazine hydrate directly impacts the impact block 25 at the center of the bottom wall of the hydrazine hydrate distribution cylinder 6. Through the hemispherical arc surface of the impact block 25, the axial direct injection is transformed into radial uniform diffusion, ensuring that the hydrazine hydrate can be evenly distributed to several first channels 9 on the side wall of the hydrazine hydrate distribution cylinder 6. During the diffusion process, the hydrazine hydrate can impact the arc-shaped blades 61, thereby converting part of the delivery pressure of the hydrazine hydrate into the rotational power of the hydrazine hydrate distribution cylinder 6. Through the impact of the hydrazine hydrate on the arc-shaped blades 61, the hydrazine hydrate distribution cylinder 6 is driven to rotate stably around the central axis. Several arc-shaped blades 61 are arranged in a ring array to ensure that the hydrazine hydrate distribution cylinder 6 is subjected to balanced force, avoids eccentric swaying during rotation, and maintains the uniformity of the radial jet. Finally, the hydrazine hydrate is ejected into the mixing chamber 7 through the first channel 9. Under the action of the rotation of the hydrazine hydrate distribution cylinder 6, a uniform radial rotating jet is formed, which is then mixed with the atomized spray. The atomized formamide droplets from the head 13 precisely converge within the mixing chamber 7. Utilizing the dispersing effect of the atomizing nozzle 13, the rotational effect of the hydrazine hydrate distribution tube 6, and the impact force of the hydrazine hydrate jet, formamide and hydrazine hydrate converge and form a high-intensity turbulent field within the mixing chamber 7. This ensures more thorough impact contact between the hydrazine hydrate and the atomized formamide droplets, further shortening the mixing time and achieving precise molecular-level mixing. The hemispherical impact block 25, guided by its arc surface, achieves uniform circumferential distribution of hydrazine hydrate, preventing localized concentrations. Combined with the annular array of arc-shaped blades 61, the flow deviation of hydrazine hydrate in each first channel 9 is ≤1%, preventing the potential for excessively high local concentrations of hydrazine hydrate from the source. This further suppresses hydrazine-hydrazine side reactions and improves the purity of the main product. Both the impact block 25 and the arc-shaped blades 61 are integrally molded from Hastelloy, sharing the same material as the hydrazine hydrate distribution tube 6. This ensures resistance to high temperature and pressure conditions, eliminating the risk of deformation, corrosion, or detachment. The rotational power originates from the hydrazine hydrate's own delivery pressure, requiring no additional energy consumption.
[0029] Example 4: Based on any one of Examples 1-3, such as Figure 1 , Figure 3 , Figure 4 As shown, several second channels 11 are arranged in a ring array about the center of the annular liquid inlet chamber 10, the formamide diversion tube 12 is vertically arranged, and the atomizing nozzles 13 are arranged at equal intervals along the axial direction of the formamide diversion tube 12. The spray direction of the atomizing nozzles 13 is tangent to the outer wall of the formamide diversion tube 12.
[0030] The working principle and beneficial effects of the above technical solution are as follows: The preheated formamide in the annular inlet chamber 10 is uniformly distributed circumferentially through several second channels 11 arranged in a ring array. Each second channel 11 corresponds to a vertically arranged formamide distribution pipe 12. Atomizing nozzles 13 are arranged at equal intervals along the axial direction of the formamide distribution pipe 12, forming a multi-layered atomization area. Combined with the uniform circumferential distribution of the formamide distribution pipe 12, the atomized formamide droplets achieve full circumferential coverage and axial distribution within the mixing chamber 7. Layered liquid distribution reduces atomization blind zones and ensures that formamide droplets can contact different positions within the mixing chamber 7. The spray direction of the atomizing nozzle 13 is tangential to the outer wall of the formamide distribution pipe 12, causing the sprayed formamide droplets to generate rotational kinetic energy along the tangential direction of the distribution pipe, thereby forming a ring-shaped rotating flow field within the mixing chamber 7. When the hydrazine hydrate distribution pipe 6 rotates counterclockwise, the formamide droplets rotate clockwise within the mixing chamber 7. Formamide and hydrazine hydrate form an anti-rotational counter-current within the mixing chamber 7, enhancing the hydrazine hydrate's reaction. The impact of formamide and the strong shearing force of the reverse rotation further break the atomized formamide droplets and hydrazine hydrate jet into smaller fluid units, improving mixing efficiency and uniformity. At the same time, it avoids excessively high local concentrations of hydrazine hydrate, further suppressing hydrazine-hydrazine side reactions. The rotating flow field drives rapid convection of the fluid in the mixing chamber 7, enhancing the heat exchange between the formamide droplets and the high-temperature environment of the mixing chamber 7, keeping the temperature in the mixing chamber 7 within a stable range, thereby ensuring a stable cyclization reaction rate. The layered flow field design of the formamide atomizing nozzle 13 enables uniform mixing of formamide and hydrazine hydrate, with more synchronous and concentrated heat release, effectively supplementing the heat of reaction and reducing the supplementary load of external heat sources. This allows all material molecules to participate in the cyclization reaction at the optimal temperature, avoiding reaction lag and low temperature caused by uneven mixing of local materials. At the same time, the improved reaction synchronization can significantly accelerate the cyclization reaction rate. The reaction time for 1 ton of hydrazine hydrate can be shortened to 8-10 hours, increasing production efficiency by more than 50% compared to existing processes.
[0031] Example 5: Based on any one of Examples 1-4, such as Figure 1 , Figure 5 As shown, a collection cover 26 is provided below the partition 5, and the lower end of the through hole 8 is connected to the inside of the collection cover 26. The collection cover 26 is funnel-shaped. A mixing mechanism is provided at the lower end of the collection hood 26. The mixing mechanism includes a third delivery pump 27, which can be a high-temperature and high-pressure metering pump. The input end of the third delivery pump 27 is connected to the lower end of the collection hood 26. An overflow cylinder 28 is provided below the third delivery pump 27. The overflow cylinder 28 is cylindrical and horizontally positioned. The outside of the overflow cylinder 28 is fixedly connected to the inner wall of the mixing cylinder 1 through a fixing plate 29. A three-way pipe 30 is provided at the output end of the third delivery pump 27. The three-way pipe 30 includes one input pipe and two output pipes. The three-way pipe 30 is connected to the third delivery pump 27 through the input pipe. The pump 27 is connected to the output end. The two output pipes of the three-way pipe 30 are connected to the upper part of the overflow cylinder 28. The two output pipes are horizontally set and the liquid outlet direction of the two output pipes is on the same horizontal plane. Two rotating shafts 31 are symmetrically arranged inside the overflow cylinder 28. The front and rear ends of the rotating shafts 31 are rotatably connected to the inner walls of the front and rear sides of the overflow cylinder 28, respectively. Several stirring blades 32 are arranged on the outer wall of the rotating shafts 31. Two overflow holes 33 are arranged on the side wall of the overflow cylinder 28. The overflow holes 33 are located at the lower part of the overflow cylinder 28. A drain pipe 34 is arranged at the bottom of the overflow cylinder 28. A first valve is arranged on the drain pipe 34.
[0032] The working principle and beneficial effects of the above technical solution are as follows: The gas-liquid mixture (liquid triazole, water, unreacted materials, and ammonia) after a mixing reaction in the mixing chamber 7 can flow rapidly into the funnel-shaped collection hood 26 below through the through hole 8 on the partition 5. The funnel structure of the collection hood 26 utilizes gravity to achieve natural aggregation of liquid products, preventing liquid products from stagnating below the partition 5. At the same time, residual ammonia can be folded back upward along the inner wall of the collection hood 26 to achieve gas-liquid separation. The third delivery pump 27 can draw the liquid products collected in the collection hood 26 to the input pipe of the three-way pipe 30, and then divert them to two output pipes. The liquid products are injected simultaneously from both sides of the overflow cylinder 28. Since the output pipe is horizontally set, the liquid products can form a horizontal convection flow field after flowing into the overflow cylinder 28. The two liquid products collide and flow downward, driving the stirring blades 32 to rotate in the overflow cylinder 28. The stirring blades 32 apply shear force and stirring force to the injected liquid products to achieve uniform mixing of formamide and hydrazine hydrate. The mixing process eliminates localized proportioning deviations. Simultaneously, the two overflow holes 33 on the sidewall of the overflow cylinder 28 stabilize the liquid level at a set height. Excess liquid product overflows through the overflow holes 33. The height of the overflow holes 33 is lower than the height of the rotating shaft 31 but higher than the height of the stirring blades 32 when they are at their lowest position. This prevents insufficient mixing due to excessively high liquid levels or idling due to excessively low liquid levels. The purity of the liquid product after being stirred by the stirring blades 32 is further improved. The horizontal convection flow field of the two output pipes, combined with the shearing effect of the stirring blades 32, makes the flow field inside the overflow cylinder 28 more regular, thus maintaining a stable mixing effect. A drain pipe 34 is installed at the bottom of the overflow cylinder 28. The drain pipe 34 is conical in shape, with its upper end adapted to the bottom of the overflow cylinder 28. The stirred liquid product can be continuously discharged through the drain pipe 34. The first valve can precisely control the discharge rate according to the feed requirements of the subsequent distillation column, ensuring a continuous and stable production process without intermittent operation.
[0033] Example 6: Based on Example 5, such as Figure 1 As shown, a gas outlet pipe 35 is provided on the side wall of the collection cylinder 2. One end of the gas outlet pipe 35 extends into the collection cover 26 and communicates with the upper end of the collection cover 26. The other end of the gas outlet pipe 35 extends to the outside of the collection cylinder 2 and is equipped with an air pump.
[0034] The working principle and beneficial effects of the above technical solution are as follows: Since the density of ammonia is much smaller than that of liquid products, ammonia will quickly and naturally rise to the gas accumulation area at the top of the collection hood 26. One end of the gas outlet pipe 35 extends precisely to this area and is connected. After the gas pump is started, the gas outlet pipe 35 can quickly extract the ammonia at the top of the collection hood 26, preventing the ammonia from diffusing to the bottom of the collection hood 26.
[0035] Example 7: Based on any one of Examples 1-6, such as Figure 1As shown, the collecting cylinder 2 is funnel-shaped, and a guide pipe 36 is provided at the lower end of the collecting cylinder 2. A second valve is provided at the lower end of the guide pipe 36.
[0036] The working principle and beneficial effects of the above technical solution are as follows: the high-purity liquid product (1,2,4-triazole, water, and trace amounts of unreacted materials) after the mixing reaction can continuously flow into the funnel-shaped collection cylinder 2, thereby collecting in the collection cylinder 2. When the second valve is opened, the collected liquid product can flow to the subsequent distillation column equipment through the guide pipe 36. By adjusting the opening degree of the second valve, the discharge rate of the product can be controlled, so that the discharge flow rate is precisely matched with the feed requirements of the subsequent distillation column and other equipment, thus meeting the needs of continuous production.
[0037] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.
[0038] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0039] Although embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. They can be applied to various fields suitable for the present invention. Other modifications can be easily made by those skilled in the art. Therefore, without departing from the general concept defined by the claims and their equivalents, the present invention is not limited to the specific details and illustrations shown and described herein.
Claims
1. A multi-channel micro-jet impact mixer, characterized in that, include: A mixing cylinder (1) and a collecting cylinder (2) are provided. The upper end of the collecting cylinder (2) is connected to the lower end of the mixing cylinder (1). A heating jacket is provided outside the mixing cylinder (1). A spiral heating tube (3) is provided inside the heating jacket. A formamide inlet pipe (4) is connected to the lower end of the spiral heating tube (3). An impact mechanism is provided inside the mixing cylinder (1). The impact mechanism includes a partition plate (5). The partition plate (5) is fixedly installed inside the mixing cylinder (1). A hydrazine hydrate diverter (6) is rotatably installed at the center of the upper surface of the partition plate (5). The upper end of the hydrazine hydrate diverter (6) is sealed and rotatably connected to the top wall of the mixing cylinder (1). A mixing cavity (7) is formed between the outer wall of the hydrazine hydrate diverter (6) and the inner wall of the mixing cylinder (1). Several through holes (8) are provided through the partition plate (5). The upper end of the through holes (8) is connected to the mixing cavity (7). Several first channels (9) are evenly provided on the side wall of the hydrazine hydrate diverter (6). An annular liquid inlet chamber (10) is provided on the inner wall of the upper end of the cylinder (1). Several second channels (11) are provided at the lower end of the annular liquid inlet chamber (10). A formamide diversion pipe (12) is provided at the lower end of the second channel (11). The formamide diversion pipe (12) is located in the mixing chamber (7). Several atomizing nozzles (13) are connected to the side wall of the formamide diversion pipe (12). A first delivery pump (14) and a second delivery pump (15) are provided at the upper end of the mixing cylinder (1). The input end of the first delivery pump (14) is connected to the hydrazine hydrate inlet pipe (16). The output end of the first delivery pump (14) is connected to the upper end of the hydrazine hydrate diversion cylinder (6) through the liquid inlet hole (17). The input end of the second delivery pump (15) is connected to the upper end of the spiral heating pipe (3) through the delivery pipe (18). The output end of the second delivery pump (15) is connected to the annular liquid inlet chamber (10) through the delivery channel (19).
2. The multi-channel microjets impact mixer according to claim 1, characterized in that, The heating jacket includes a heat-conducting jacket (20) and two heat-insulating rings (21). The heat-conducting jacket (20) is fitted on the outer wall of the mixing cylinder (1). The outer wall of the heat-conducting jacket (20) is provided with a first mounting groove that is compatible with the spiral heating tube (3). The two heat-insulating rings (21) are assembled on the outside of the heat-conducting jacket (20). The heat-insulating rings (21) are semi-circular ring structures. The inner wall of the heat-insulating rings (21) is provided with a second mounting groove that is compatible with the spiral heating tube (3). Connecting ears (22) are provided at the front and rear ends of the heat-insulating rings (21). The front and rear ends of the two heat-insulating rings (21) are connected by connecting ears (22).
3. The multi-channel microjets impact mixer according to claim 2, characterized in that, The first mounting groove is provided with a third mounting groove (23) on the side near the mixing cylinder (1). The third mounting groove (23) is spiral in shape. A heating strip (24) is provided inside the third mounting groove (23). The heating strip (24) is connected to the outer wall of the spiral heating tube (3).
4. The multi-channel microjets impact mixer according to claim 1, characterized in that, An impact block (25) is fixedly installed at the center of the bottom wall of the hydrazine hydrate diverter (6). The impact block (25) is located directly below the liquid inlet (17). The impact block (25) is hemispherical and the arc surface of the impact block (25) faces the liquid inlet (17).
5. The multi-channel microjets impact mixer according to claim 4, characterized in that, The bottom wall of the hydrazine hydrate diverter (6) is provided with several arc-shaped blades (61), and the several arc-shaped blades (61) are arranged in a ring array about the central axis of the hydrazine hydrate diverter (6).
6. The multi-channel microjets impact mixer according to claim 1, characterized in that, Several second channels (11) are arranged in a ring array about the center of the annular liquid inlet chamber (10). The formamide diversion tube (12) is set vertically. The atomizing nozzles (13) are set at equal intervals along the axial direction of the formamide diversion tube (12). The spray direction of the atomizing nozzles (13) is tangent to the outer wall of the formamide diversion tube (12).
7. The multi-channel microjets impact mixer according to claim 1, characterized in that, A collection cover (26) is installed below the partition (5), and the lower end of the through hole (8) is connected to the inside of the collection cover (26). The collection cover (26) is funnel-shaped.
8. The multi-channel microjets impact mixer according to claim 7, characterized in that, A mixing mechanism is provided at the lower end of the collection hood (26). The mixing mechanism includes a third conveying pump (27). The input end of the third conveying pump (27) is connected to the lower end of the collection hood (26). An overflow cylinder (28) is provided below the third conveying pump (27). The overflow cylinder (28) is cylindrical and horizontally positioned. The outside of the overflow cylinder (28) is fixedly connected to the inner wall of the mixing cylinder (1) through a fixing plate (29). A three-way pipe (30) is provided at the output end of the third conveying pump (27). The three-way pipe (30) includes an input pipe and two output pipes. The three-way pipe (30) is connected to the output end of the third conveying pump (27) through the input pipe. The two output pipes of the three-way pipe (30) are connected to the upper part of the overflow cylinder (28). The two output pipes are set horizontally and the liquid outlet direction of the two output pipes is on the same horizontal plane. Two rotating shafts (31) are symmetrically arranged inside the overflow cylinder (28). The front and rear ends of the rotating shafts (31) are rotatably connected to the inner walls of the front and rear sides of the overflow cylinder (28). Several stirring blades (32) are arranged on the outer wall of the rotating shafts (31). Two overflow holes (33) are arranged on the side wall of the overflow cylinder (28). The overflow holes (33) are located at the lower part of the overflow cylinder (28). A drain pipe (34) is arranged at the bottom of the overflow cylinder (28). A first valve is arranged on the drain pipe (34).
9. The multi-channel microjets impact mixer according to claim 7, characterized in that, A gas outlet pipe (35) is provided on the side wall of the collection cylinder (2). One end of the gas outlet pipe (35) extends into the collection hood (26) and is connected to the upper end of the collection hood (26). The other end of the gas outlet pipe (35) extends to the outside of the collection cylinder (2) and is equipped with an air pump.
10. The multi-channel microjets impact mixer according to claim 1, characterized in that, The collecting cylinder (2) is funnel-shaped, and a guide pipe (36) is provided at the lower end of the collecting cylinder (2). A second valve is provided at the lower end of the guide pipe (36).
Citation Information
Patent Citations
Triazole synthesis system with high reaction efficiency
CN219024311U