A microreactor apparatus and method for preparing di-tert-butyl peroxide

Abstract

The application relates to the field of di-tert-butyl peroxide preparation, and particularly discloses a micro-reaction equipment and method for preparing di-tert-butyl peroxide, which comprises a body provided with a reaction channel, the body is stacked by multiple groups of plates, the multiple groups of plates are sequentially a first layer plate, a second layer plate, a third layer plate and a fourth layer plate from top to bottom, the reaction channel is formed between the second layer plate and the third layer plate, the reaction channel is provided with a feeding port and a discharging port on the two sides respectively, and the feeding port and the discharging port are respectively arranged at the two ends of the third layer plate; the reaction channel is respectively provided with a mixing area and a reaction area close to the feeding port and the discharging port, the reaction area is provided with a heat conduction block, the heat conduction block is integrally arranged with the second layer plate, and the heat conduction block extends into the reaction channel. The application forms a passing area through the metal heat conduction block and the reaction channel, combines the internal S-shaped cooling cavity and the external radiator linkage, realizes accurate temperature control of the reaction area, avoids the risk of over-temperature, and guarantees that the reaction is safely and stably carried out.

Description

Technical Field

[0001] This invention relates to the field of di-tert-butyl peroxide preparation technology, and more particularly to a microreaction apparatus and method for preparing di-tert-butyl peroxide. Background Technology

[0002] The synthesis of di-tert-butyl peroxide (DTBP) uses tert-butanol (TBA) as a raw material, hydrogen peroxide (H2O2) as an oxidant, and concentrated sulfuric acid (H2SO2) as a catalyst. It is achieved through a two-step reaction: First, tert-butanol reacts with hydrogen peroxide under sulfuric acid catalysis to generate tert-butyl hydrogen peroxide (TBHP) (an intermediate product); Second, TBHP further reacts with tert-butanol to generate the target product, di-tert-butyl peroxide (DTBP). Traditional batch processes have low selectivity (approximately 85%), mainly due to excessively high temperatures and long residence times leading to increased side reactions (such as the decomposition of TBHP into tert-butanol and water). The microreactor effectively suppresses side reactions through segmented temperature control (10-25℃ for the first microchannel reactor and 45-65℃ for the second microchannel reactor) and short residence time (0.5-3 minutes): Step 1 (generation of tert-butyl hydroperoxide (TBHP): Low temperature (10-25℃) avoids excessive decomposition of hydrogen peroxide, increasing TBHP yield; Step 2 (reaction of TBHP with tert-butanol to generate DTBP): Medium temperature (45-65℃) accelerates the reaction rate while preventing DTBP decomposition; ultimately achieving a tert-butanol conversion rate >99%, DTBP selectivity >97.9%, and yield >94.8% (purity >94%), far exceeding traditional processes (conversion rate <90%, selectivity <85%).

[0003] Existing technologies have also made relevant improvements to microreactor devices. For example, prior art publication number CN211725714U discloses a high-throughput microreactor device for preparing di-tert-butyl peroxide. This device includes a feeding device, a microreactor, and a post-processing device. The feeding device is connected to the microreactor, and the microreactor is connected to the post-processing device. In the microreactor and post-processing devices, tert-butanol reacts with hydrogen peroxide to generate the reaction product. This device can be scaled up to different ratios according to production needs, without scale-up effect, and has a large throughput. The process of preparing di-tert-butyl peroxide using microreactors has advantages such as high material utilization, high reaction efficiency, short reaction time, low production cost, and safety and reliability.

[0004] Since the secondary reaction between the tert-butyl hydrogen peroxide solution generated in the first reaction and tert-butanol is a medium-temperature reaction (45-65℃), while the first step of generating tert-butyl hydrogen peroxide is a low-temperature reaction (10-25℃), it is crucial to use a coolant to control the temperature of the reaction zone. However, existing microreactors use a cooling plate through which a coolant is introduced to exchange heat with the solution in the reaction channel. This method has a limited contact area between the reaction zone and the cooling plate, resulting in limited heat exchange efficiency. The heat accumulation effect after a long reaction period leads to excessively high local temperatures, which is detrimental to subsequent solution reactions.

[0005] In summary, there is still room for improvement in the current technology for temperature control within the reaction channel. Summary of the Invention

[0006] The purpose of this section is to outline some aspects of embodiments of the present invention and to briefly describe some preferred embodiments. Simplifications or omissions may be made in this section, as well as in the abstract and title of this application, to avoid obscuring the purpose of these documents; however, such simplifications or omissions should not be construed as limiting the scope of the invention.

[0007] This invention provides a microreactor and method for preparing di-tert-butyl peroxide, which solves the problem of difficult temperature control in existing technologies. The specific solution is as follows: On one hand, the present invention provides a microreactor for preparing di-tert-butyl peroxide, comprising a body with a reaction channel, the body being composed of multiple stacked plates, the multiple plates being, from top to bottom, a first plate, a second plate, a third plate, and a fourth plate, a reaction channel being formed between the second and third plates, the reaction channel having an inlet and a outlet on both sides, the inlet and outlet being respectively located at both ends of the third plate; the reaction channel having a mixing zone and a reaction zone near the inlet and outlet, respectively, a heat-conducting block being provided in the reaction zone, the heat-conducting block being integrally formed with the second plate, the heat-conducting block extending into the reaction channel, the outer wall of the heat-conducting block forming a passage area with the reaction channel, allowing the reacted liquid to be discharged from the outlet.

[0008] Preferably, the heat-conducting block roughly covers the top-view projection surface of the reaction zone and occupies a certain volume of the reaction zone. The heat-conducting block and the second layer plate are made of metal, so that the liquid in the reaction channel can exchange heat with the outside air through the heat-conducting block and the second layer plate. By forming a passage area with the metal heat-conducting block and the reaction channel, combined with the internal S-shaped cooling cavity and the external heat sink, the temperature of the reaction zone can be precisely controlled, avoiding the risk of overheating and ensuring the safe and stable progress of the reaction.

[0009] Preferably, the heat-conducting block has a cooling chamber inside, and an injection chamber and an exhaust chamber are respectively opened at both ends of the cooling chamber. The injection chamber and the exhaust chamber are respectively opened at both ends of the second layer plate and penetrate to the outer wall of the second layer plate. The injection chamber and the exhaust chamber are respectively connected to the coolant injection pipe and the coolant exhaust pipe, so that the heat of the heat-conducting block is carried away by the coolant.

[0010] Preferably, the cooling cavity is S-shaped, and the S-shaped cooling cavity roughly covers the top projection surface of the heat-conducting block, and at least a portion of the cooling cavity overlaps with the thickness range of the reaction channel.

[0011] Preferably, the first and second plates have interconnected catalyst inlets on one side, the top of the catalyst inlet is connected to the catalyst tube, and the bottom of the catalyst inlet leads to the reaction channel.

[0012] Preferably, a dispersion block is installed inside the catalyst inlet, and the dispersion block has several dispersion holes. The dispersion holes disperse the liquid catalyst into fine water droplets, which mix with the reactants in the reaction channel.

[0013] Preferably, there is at least one mixer between the catalyst inlet and the discharge port. The mixer consists of a rotating shaft and several rotating blades. The middle of the reaction channel has a receiving area that matches the mixer. When the mixed solution passes through the rotating blades, the several rotating blades can fully mix the mixed solution before it flows into the reaction zone.

[0014] Preferably, a temperature sensor is installed below the reaction channel, and slots matching the temperature sensor are opened on the third and fourth layers. The top of the slot is closed to the reaction channel on the third layer. By embedding the temperature sensor in the slot to monitor the temperature of the mixing zone and the reaction zone, and combining multi-point data feedback, the coolant flow rate is dynamically adjusted to achieve fine process control.

[0015] Preferably, the mixing area has a narrowing region on the side closest to the receiving area.

[0016] On the other hand, the present invention also provides a micro-reaction method for preparing di-tert-butyl peroxide, comprising the following steps: S1. Provide a micro-reaction device, which includes a body composed of multiple stacked plates, wherein a reaction channel is formed between the second and third plates, the end of the reaction channel near the feed inlet is a mixing zone, and the end near the discharge outlet is a reaction zone. A heat-conducting block integrally formed with the second plate is provided in the reaction zone, the heat-conducting block extends into the reaction channel, and its outer wall and the inner wall of the reaction channel form a flow channel for the reaction liquid to pass through. S2. Inject tert-butanol, hydrogen peroxide and concentrated sulfuric acid into the mixing zone of the reaction channel and mix them in the mixing zone. S3. The mixed material enters the reaction zone and flows and reacts in the channel between the outer wall of the heat-conducting block and the inner wall of the reaction channel. At the same time, the temperature of the reaction zone is controlled by the heat-conducting block to maintain the target reaction conditions. S4. Tert-butanol reacts with hydrogen peroxide under sulfuric acid catalysis to produce tert-butyl hydrogen peroxide; S5. The tert-butyl hydrogen peroxide solution after the reaction is completed is discharged through the discharge port and then enters another microreactor with the same structure to react further with tert-butanol to generate the target product di-tert-butyl peroxide.

[0017] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects: 1. This invention forms a passage area by connecting a metal heat-conducting block with the reaction channel, and combines the internal S-shaped cooling cavity with the external heat sink to achieve precise temperature control of the reaction zone, avoid the risk of overheating, and ensure the safe and stable progress of the reaction.

[0018] 2. The present invention refines the catalyst into a mist through the splitting chamber, dispersion chamber and dispersion holes, and rapidly integrates it with the reaction liquid in the mixing zone; the rotating blades of the mixer further agitate the fluid, thereby improving the reaction conversion rate.

[0019] 3. The present invention guides the fluid to flow in the center and accelerates the turbulence by the synergistic effect of the arc-shaped structure of the guide block and the narrowing area, thereby reducing local accumulation and ensuring smooth channel flow and mixing efficiency.

[0020] 4. The present invention fixes the first, second, third and fourth layers of the plate with bolts and sealant, and integrates the heat-conducting block with the second layer of the plate, which takes into account both structural strength and ease of disassembly and assembly, and extends the service life of the equipment.

[0021] 5. This invention monitors the temperature of the mixing and reaction zones by embedding a temperature sensor in a slot, and dynamically adjusts the coolant flow rate by combining multi-point data feedback, thereby achieving refined process control.

[0022] 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 structures particularly pointed out in the written description and the accompanying drawings. Attached Figure Description

[0023] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. Wherein: Figure 1This is a perspective view of the entire invention; Figure 2 This is a perspective view of the upper part of the present invention; Figure 3 This is a perspective view of the bottom of the present invention; Figure 4 This is a schematic diagram of the second and third layers of the present invention; Figure 5 This is a partial cross-sectional view of the second and third layers of the present invention; Figure 6 This is a perspective view of the reaction channel and heat-conducting block of the present invention; Figure 7 This is a cross-sectional view of the present invention; Figure 8 This is a top view of the third layer plate of the present invention; Figure 9 This is a side sectional view of the first and second layers of the present invention; Figure 10 This is a perspective view of the first, second, and third layers of the present invention; Figure 11 This is a perspective view of the dispersion block of the present invention; Figure 12 This is a schematic diagram of the installation of the mixer of the present invention.

[0024] The accompanying figure is labeled as follows: 1. First layer plate; 2. Second layer plate; 3. Third layer plate; 4. Fourth layer plate; 5. Reaction channel; 6. Feed inlet; 7. Discharge outlet; 8. Mixing zone; 9. Reaction zone; 10. Heat-conducting block; 11. Passing area; 12. Cooling chamber; 13. Injection chamber; 14. Discharge chamber; 15. Coolant injection pipe; 16. Coolant discharge pipe; 17. Guide block; 18. Catalyst inlet; 19. Catalyst tube; 20. Diverting chamber; 21. Diverting block; 22. Dispersion chamber; 23. Dispersion block; 24. Dispersion hole; 25. Mixer; 26. Rotating shaft; 27. Rotating plate; 28. Receiving area; 29. ​​Narrowing area; 30. Temperature sensor; 31. Slot. Detailed Implementation

[0025] Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form part of the present invention and, together with the embodiments of the present invention, serve to illustrate the principles of the present invention.

[0026] Example 1: As Figure 1 , Figure 2 , Figure 3As shown, this embodiment provides a microreactor for preparing di-tert-butyl peroxide, including a body with a reaction channel. The body is composed of multiple stacked plates, which are arranged from top to bottom as a first plate 1, a second plate 2, a third plate 3, and a fourth plate 4. The first plate 1, the second plate 2, the third plate 3, and the fourth plate 4 are fixed together by several bolts, and sealant is filled between adjacent plates.

[0027] like Figure 4 , Figure 5 As shown, a reaction channel 5 is formed between the second plate 2 and the third plate 3. The reaction channel 5 has an inlet 6 and a outlet 7 on both sides, which are respectively located at the two ends of the third plate 3. The end of the reaction channel 5 closest to the inlet 6 and the outlet 7 is the mixing zone 8 (section a) and the reaction zone 9 (section b). A heat-conducting block 10 is provided in the reaction zone 9. The heat-conducting block 10 is integrally formed with the second plate 2 and extends into the reaction channel 5. A passage area 11 is formed between the outer wall of the heat-conducting block 10 and the reaction channel 5. The passage area 11 allows the liquid that has completed the reaction to be discharged from the outlet 7.

[0028] As one possible implementation, such as Figure 5 As shown, the heat-conducting block 10 roughly covers the top view projection surface of the reaction zone 9 and occupies a certain volume of the reaction zone 9. The heat-conducting block 10 and the second plate 2 are made of metal, so that the liquid in the reaction channel 5 can exchange heat with the outside air through the heat-conducting block 10 and the second plate 2, thereby improving the heat conduction efficiency of the solution in the reaction zone 9 and avoiding exceeding the critical temperature of the reaction.

[0029] As one possible implementation, such as Figure 1 , Figure 6 , Figure 7 As shown, the heat-conducting block 10 has a cooling chamber 12 inside. The two ends of the cooling chamber 12 are respectively provided with an injection chamber 13 and an exhaust chamber 14. The injection chamber 13 and the exhaust chamber 14 are respectively opened at both ends of the second layer plate 2 and penetrate to the outer wall of the second layer plate 2. The injection chamber 13 and the exhaust chamber 14 are respectively connected to the coolant injection pipe 15 and the coolant exhaust pipe 16. The heat of the heat-conducting block 10 is carried out by the coolant. The coolant injection pipe 15 and the coolant exhaust pipe 16 are connected to the external radiator, which can cool the coolant.

[0030] It should be noted that the working principle of the radiator is as follows: the coolant in the coolant discharge pipe 16 is discharged, and the circulating coolant is cooled by the compressor or semiconductor cooler in the heat dissipation container. Then, the coolant is injected into the cooling chamber 12 from the injection chamber 13 through the coolant injection pipe 15.

[0031] As one possible implementation, such as Figure 8As shown, the cooling cavity 12 is S-shaped, and the S-shaped cooling cavity 12 roughly covers the top projection surface of the heat-conducting block 10. At least a portion of the cooling cavity 12 overlaps with the thickness range of the reaction channel 5.

[0032] like Figure 4 , Figure 5 As shown, a guide block 17 is provided at one end of the second plate 2 near the feed inlet 6. The width of the guide block 17 matches the width of the reaction channel 5. The guide block 17 and the inner wall of the feed inlet 6 have an arc-shaped area with the same curvature, which can guide the injected reaction liquid to the middle of the reaction channel 5 and prevent the reaction liquid from accumulating there.

[0033] As one possible implementation, such as Figure 1 , Figure 9 , Figure 10 As shown, catalyst inlets 18 are interconnected on one side of the first plate 1 and the second plate 2. The top of the catalyst inlet 18 is connected to the catalyst tube 19, and the lower part of the catalyst inlet 18 leads to the reaction channel 5. After the catalyst is injected into the catalyst inlet 18 from the catalyst tube 19, it enters the reaction channel 5 and mixes with the reactants, thereby causing the reactants to undergo a chemical reaction.

[0034] As one possible implementation, such as Figure 9 As shown, the catalyst inlet 18 includes a flow divider 20, which is opened on the first plate 1. A flow divider block 21 is fixedly connected to the middle of the flow divider 20. The bottom of the flow divider 20 is connected to the bottom of the first plate 1. Two dispersion chambers 22 are opened on the second plate 2 at the corresponding positions of the flow divider 20. The two dispersion chambers 22 avoid the injection chamber 13 and are connected to the flow divider 20.

[0035] As one possible implementation, such as Figure 9 , Figure 11 As shown, a dispersion block 23 is installed on the top of the dispersion chamber 22. Several dispersion holes 24 are opened on the dispersion block 23. The dispersion holes 24 disperse the liquid catalyst into fine water droplets and mix them with the reactants in the reaction channel 5.

[0036] As one possible implementation, such as Figure 4 , Figure 12 As shown, there is at least one mixer 25 between the catalyst inlet 18 and the discharge port. The mixer 25 consists of a rotating shaft 26 and several rotating blades 27. The middle part of the reaction channel 5 has a receiving area 28 that matches the mixer 25. When the mixed solution passes through the rotating blades 27, the several rotating blades 27 can fully mix the mixed solution and then flow into the reaction zone 9.

[0037] It should be noted that the aforementioned rotating shaft 26 is located off-center in the reaction channel 5, so that after the solution collides with the rotating plate 27, the rotating plate 27 and the rotating shaft 26 can rotate in the same direction.

[0038] It should also be noted that, in order to ensure that the rotating shaft 26 is properly fixed, rotating holes (not shown in the figure) are provided at corresponding positions of the first layer plate 1 and the second layer plate 2. Thus, when the first layer plate 1, the second layer plate 2 and the third layer plate 3 need to be installed, the rotating shaft can be inserted into the rotating hole to position the mixer 25.

[0039] As one possible implementation, such as Figure 4 As shown, the mixing zone 8 has a narrowing region 29 on the side near the containment zone. The narrowing region 29 allows the flow rate of the solution to be reacted to be increased and the solution to be disturbed, thereby fully mixing with the catalyst.

[0040] As one possible implementation, such as Figure 7 As shown, a temperature sensor 30 is installed below the reaction channel 5, and slots 31 matching the temperature sensor 30 are provided on the third plate 3 and the fourth plate 4, so that the temperature of the solution in the reaction channel 5 can be directly monitored through the temperature sensor 30.

[0041] As one possible embodiment, in the above scheme, the top of the slot 31 and the reaction channel 5 on the third layer plate 3 are enclosed; the surface temperature of the third layer plate 3 is measured by the temperature sensor 30 to infer the solution temperature in the reaction channel 5, and at least two temperature sensors 30 are distributed in the mixing zone 8 and the reaction zone 9 of the reaction channel 5 to monitor the temperature at different locations of the reaction channel 5, so as to facilitate precise control of the temperature of the coolant.

[0042] Example 2: This example differs from Example 1 in that it provides a micro-reaction method for preparing di-tert-butyl peroxide, comprising the following steps: S1. Fluid Input and Premixing: Directional Flow Guidance and Flow Pattern Optimization S1.1 The raw material liquid (such as a mixture of tert-butanol and hydrogen peroxide) is injected into the reaction channel 5 through the inlet 6 at both ends of the third layer plate 3. The channel is formed by the parallel stacking of the second layer plate 2 and the third layer plate 3, and the interior is a rectangular or quasi-rectangular flow channel. The guide block 17 is fixed to the end of the second layer plate 2 near the inlet 6. Its width matches the reaction channel 5, and both the guide block 17 and the inner wall of the inlet 6 are designed with the same arc. When the raw material liquid is injected at high speed, the arc structure will "constrict" the fluid and guide it to the middle of the channel, avoiding adhesion and accumulation along the wall (especially the "side wall effect" that is prone to occur at low flow rates).

[0043] S1.2 After the fluid enters the mixing zone 8, it first flows through the narrowing zone 29: According to Bernoulli's principle, the flow velocity increases significantly due to the reduction of the cross-sectional area, and at the same time, the flow state changes from laminar flow to turbulent flow, generating strong turbulence; this process not only breaks the initial stratification of the raw material liquid, but also breaks the large droplets into small droplets through shear force, laying the foundation for subsequent catalytic reaction and mixing.

[0044] S2. Catalytic reaction initiation: Multi-stage dispersion and precise dosing: The catalyst (such as concentrated sulfuric acid) is delivered to the catalyst inlet 18 through the catalyst tube 19. This inlet is located on the same side of the first plate 1 and the second plate 2, ensuring vertical downward injection into the mixing zone 8 of the reaction channel 5. The interior of the inlet has a hierarchical dispersion structure. First-stage diversion: The catalyst first enters the diversion chamber 20 on the first plate 1. The diversion block 21 fixed in the middle of the chamber "splits" the fluid into two equal branches to avoid single-point concentrated addition that would lead to excessively high local concentration. Second-stage dispersion: Two branches flow into two symmetrically opened dispersion chambers 22 on the second layer plate 2 (to avoid the coolant injection chamber 13) to prevent interference with the cooling system. A dispersion block 23 is installed on the top of the chamber, and dispersion holes 24 with a diameter of 0.5-2mm are evenly distributed on the block.

[0045] S3, Enhanced Mixing and Reaction: Mechanical Disturbance and Mass Transfer Enhancement: The pre-mixed catalyst flows into the containment area 28 in the middle of the reaction channel 5, where a mixer 25 is built. The mixer consists of a rotating shaft 26 and multiple tilted rotating plates 27. The rotating shaft 26 is positioned by rotating holes (not shown) on the first plate 1 and the second plate 2, and its axis is offset from the center line of the channel (about 1 / 3 of the channel width). When the mixture flows through the rotating plates 27, the asymmetric pressure difference generated by the fluid impacting the plates forms a unidirectional torque (similar to water turbine drive), which drives the rotating shaft 26 and the rotating plates 27 to rotate at a low speed.

[0046] The rotating plate 27 causes the fluid to be repeatedly "cut" and "folded" as it passes through: on the one hand, it breaks up the incompletely reacted agglomerates (such as catalyst particle aggregates), and on the other hand, it shortens the molecular diffusion distance through forced convection, ensuring that the reactants (tert-butanol, hydrogen peroxide) are in full contact with the active sites of the catalyst, thereby improving the reaction conversion rate; the mixed solution finally enters the reaction zone 9.

[0047] S4. Temperature-controlled reaction and product discharge: High-efficiency heat exchange and closed-loop cooling: Reaction zone 9 is the core region of the exothermic reaction. The synthesis of di-tert-butyl peroxide is significantly exothermic, and its temperature must be strictly controlled below the critical value (to avoid side reactions or decomposition). Temperature control relies on the coordinated action of the heat-conducting block 10 and the cooling system. Heat-conducting block design: The heat-conducting block 10 is integrally formed with the second layer plate 2. The top view projection covers most of the area of ​​the reaction zone 9. The distance between the outer wall and the inner wall of the reaction channel 5 forms the passage area 11. When the reaction liquid flows through the passage area 11, it comes into direct contact with the outer wall of the heat-conducting block 10. The reaction heat is quickly conducted to the interior through the metal block (high thermal conductivity ≥100W / (m·K)). Cooling chamber 12 structure: An S-shaped cooling chamber 12 is opened inside the heat-conducting block 10. The chamber extends horizontally along the heat-conducting block 10, covering most of the top-view projection surface of the heat-conducting block, and overlaps with the thickness of the reaction channel 5 (to ensure maximum heat exchange area); coolant (such as water or ethylene glycol aqueous solution) is pumped in from the injection chamber 13 at one end of the second layer plate 2, flows through the S-shaped cavity, absorbs heat from the heat-conducting block, and then enters the external radiator (including compressor or semiconductor refrigerator) from the discharge chamber 14 at the other end through the coolant discharge pipe 16. After cooling down, it flows back to the injection chamber 13 through the coolant injection pipe 15 to form closed-loop cooling; Product discharge: The di-tert-butyl peroxide solution that has completed the reaction continues to flow through zone 11 and eventually collects at the discharge port 7 at the other end of the third plate 3, and is discharged to the subsequent separation and purification unit.

[0048] S5. Real-time monitoring and control: Multi-point temperature measurement and dynamic feedback: To ensure that the temperature is controllable throughout the reaction, a temperature sensor 30 is embedded in the slot 31 between the third layer plate 3 and the fourth layer plate 4, thereby monitoring the temperature of the solution inside the reaction channel 5 in real time.

[0049] In summary, this invention achieves precise temperature control in the reaction zone 9 by forming a passage area 11 with the metal heat-conducting block 10 and the reaction channel 5, combined with the internal S-shaped cooling cavity 12 and the external heat sink, thus avoiding the risk of overheating and ensuring the safe and stable progress of the reaction. The catalyst is atomized into a mist through the flow distribution cavity 20, dispersion cavity 22, and dispersion holes 24, allowing it to rapidly fuse with the reaction liquid in the mixing zone 8. The rotating blades 27 of the mixer 25 further agitate the fluid, improving the reaction conversion rate. The arc-shaped structure of the guide block 17, in conjunction with the narrowing area 29, guides the fluid to flow centrally and accelerates turbulence, reducing local accumulation and ensuring unobstructed channels and mixing efficiency. The first layer plate 1, the second layer plate 2, the third layer plate 3, and the fourth layer plate 4 are fixed with bolts and sealant, and the heat-conducting block 10 and the second layer plate 2 are integrally formed, balancing structural strength and ease of disassembly and assembly, extending equipment lifespan. By embedding the temperature sensor 30 into the slot 31 to monitor the temperature of the mixing zone 8 and the reaction zone 9, and combining multi-point data feedback, the coolant flow rate is dynamically adjusted, achieving refined process control.

[0050] It should be noted that the preparation process of di-tert-butyl peroxide in the above method consists of two steps: tert-Butanol reacts with hydrogen peroxide under sulfuric acid catalysis to produce tert-butyl hydrogen peroxide; The tert-butyl hydrogen peroxide solution after the reaction is completed is discharged through discharge port 7 and then enters another microreactor with the same structure to react further with tert-butanol to generate the target product di-tert-butyl peroxide.

[0051] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0052] The parallelism defined in this application is not limited to absolute parallelism. This definition of parallelism can be understood as basic parallelism, allowing for situations where the parallelism is not absolute due to factors such as assembly tolerances, design tolerances, and structural flatness. Small angular range errors are allowed, such as assembly error within 10 degrees, which can all be understood as a parallel relationship.

[0053] The perpendicularity defined in this application is not limited to an absolute perpendicular intersection (with an included angle of 90 degrees). It allows for non-absolute perpendicular intersections caused by factors such as assembly tolerances, design tolerances, and structural flatness. It allows for errors within a small angular range, such as an assembly error range of 80 to 100 degrees, which can all be understood as a perpendicular relationship.

[0054] The term "multiple" in this article refers to two or more. The term "and / or" in this article is merely a description of the relationship between related objects, indicating that there can be three relationships. For example, A and / or B can represent three cases: A exists alone, A and B exist simultaneously, and B exists alone.

[0055] The terms "first," "second," "third," "fourth," etc. (if present) in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that embodiments of the present application described herein can be implemented, for example, in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

[0056] The devices or elements referred to in the embodiments of this application or implied herein must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the embodiments of this application. In the description of the embodiments of this application, "a plurality of" means two or more, unless otherwise precisely specified.

[0057] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A microreactor for preparing di-tert-butyl peroxide, comprising a body with a reaction channel, characterized in that: The machine body is composed of multiple stacked plates, which are arranged from top to bottom as a first plate, a second plate, a third plate, and a fourth plate. A reaction channel is formed between the second and third plates. The reaction channel has an inlet and a outlet on each side, which are located at the two ends of the third plate. The mixing zone and the reaction zone are located near the inlet and outlet of the reaction channel, respectively. A heat-conducting block is installed in the reaction zone. The heat-conducting block is integrally set with the second plate and extends into the reaction channel. The outer wall of the heat-conducting block forms a passage area with the reaction channel, allowing the reacted liquid to be discharged from the outlet.

2. The microreactor for preparing di-tert-butyl peroxide as described in claim 1, characterized in that: The heat-conducting block covers the top-view projection surface of the reaction zone. The heat-conducting block and the second layer plate are made of metal, allowing the liquid in the reaction channel to exchange heat with the outside air through the heat-conducting block and the second layer plate.

3. The microreactor for preparing di-tert-butyl peroxide as described in claim 1, characterized in that: The heat-conducting block has a cooling chamber inside. The two ends of the cooling chamber are respectively opened into an injection chamber and an exhaust chamber. The injection chamber and the exhaust chamber are respectively opened into the two ends of the second layer plate and penetrate to the outer wall of the second layer plate. The injection chamber and the exhaust chamber are respectively connected to the coolant injection pipe and the coolant exhaust pipe, so that the heat of the heat-conducting block is carried away by the coolant.

4. The microreactor for preparing di-tert-butyl peroxide as described in claim 1, characterized in that: The cooling cavity is S-shaped, and the S-shaped cooling cavity covers the top projection surface of the heat-conducting block. At least a portion of the cooling cavity overlaps with the thickness range of the reaction channel.

5. The microreactor for preparing di-tert-butyl peroxide as described in claim 1, characterized in that: The first and second plates have interconnected catalyst inlets on one side, which are connected to the catalyst tube at the top and lead to the reaction channel at the bottom.

6. The microreactor for preparing di-tert-butyl peroxide as described in claim 5, characterized in that: The catalyst inlet is equipped with a dispersion block with several dispersion holes. The dispersion holes disperse the liquid catalyst into fine water droplets, which mix with the reactants in the reaction channel.

7. The microreactor for preparing di-tert-butyl peroxide as described in claim 6, characterized in that: There is at least one mixer between the catalyst inlet and the discharge outlet. The mixer consists of a rotating shaft and several rotating blades. The middle of the reaction channel has a receiving area that matches the mixer. When the mixed solution passes through the rotating blades, the several rotating blades can fully mix the mixed solution before it flows into the reaction zone.

8. The microreactor for preparing di-tert-butyl peroxide as described in claim 1, characterized in that: A temperature sensor is installed below the reaction channel. Slots matching the temperature sensor are provided on the third and fourth layers. The top of the slots is closed to the reaction channel on the third layer.

9. The microreactor for preparing di-tert-butyl peroxide as described in claim 7, characterized in that: The first and second plates have interconnected catalyst inlets on one side. The top of the catalyst inlet is connected to the catalyst tube, and the bottom of the catalyst inlet leads to the reaction channel. The catalyst inlet includes a flow divider chamber, which is located on the first plate. A flow divider block is fixedly connected to the middle of the flow divider chamber, and the bottom of the flow divider chamber is connected to the bottom of the first plate. The second plate has two dispersion chambers at corresponding positions to the flow divider chamber. The two dispersion chambers avoid the injection chamber and are connected to the flow divider chamber. A dispersion block is installed on the top of the dispersion chamber, and several dispersion holes are formed on the dispersion block.

10. A microreaction method for preparing di-tert-butyl peroxide, using the microreaction apparatus for preparing di-tert-butyl peroxide as described in any one of claims 1-9, characterized in that, Includes the following steps: S1. Provide a micro-reaction device, which includes a body composed of multiple stacked plates, wherein a reaction channel is formed between the second and third plates, the end of the reaction channel near the feed inlet is a mixing zone, and the end near the discharge outlet is a reaction zone. A heat-conducting block integrally formed with the second plate is provided in the reaction zone, the heat-conducting block extends into the reaction channel, and its outer wall and the inner wall of the reaction channel form a flow channel for the reaction liquid to pass through. S2. Inject tert-butanol, hydrogen peroxide and concentrated sulfuric acid into the mixing zone of the reaction channel and mix them in the mixing zone. S3. The mixed material enters the reaction zone and flows and reacts in the channel between the outer wall of the heat-conducting block and the inner wall of the reaction channel. At the same time, the temperature of the reaction zone is controlled by the heat-conducting block to maintain the target reaction conditions. S4. Tert-butanol reacts with hydrogen peroxide under sulfuric acid catalysis to produce tert-butyl hydrogen peroxide; S5. The tert-butyl hydrogen peroxide solution after the reaction is completed is discharged through the discharge port and then enters another microreactor with the same structure to react further with tert-butanol to generate the target product di-tert-butyl peroxide.

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