Method for preparing butanol by using continuous flow heat exchange microreactor

Abstract

The invention discloses a method for preparing butanol by a continuous flow heat exchange microreactor, which comprises the following steps: S1, hydroformylation reaction: introducing a raw material mixture into a first parallel feed pipe, carrying out chemical reaction on the mixture in a first carbonyl reactor, and discharging the reacted product through a discharge pipe I; s2, hydrogenation reaction: enabling the product discharged from the discharge pipe I to enter a second carbonyl reactor for chemical reaction, and discharging the reacted product into a discharge pipe II; s3, temperature control: enabling a product discharged from a discharge pipe II to enter a cooler to be cooled, shunting the product to a shunting pipe I and a shunting pipe II, and respectively performing heat exchange on a first carbonyl reactor and a second carbonyl reactor through a heat exchanger I and a heat exchanger II; and S4, data monitoring: fitting the currently required heat exchange amount according to recorded data in the reaction process of S1 and S2, and further controlling the adjusting mechanism and the heat exchange mechanism to perform synchronous temperature control on the hydroformylation reaction and hydrogenation reaction processes.

Description

Technical Field

[0001] This invention relates to the field of butanol preparation technology, specifically to a method for preparing butanol using a continuous flow heat exchange microreactor. Background Technology

[0002] Butanol is an important organic chemical raw material, widely used in solvents, plasticizers, coatings, fragrances and other fields. The carbonyl synthesis method is the main method for preparing butanol in industry, which is completed in two steps: hydroformylation and hydrogenation.

[0003] A search revealed Chinese patent CN115178168B, which solves the problem of poor gas-liquid mixing effect in existing gas-liquid mixers and improves the uniformity and throughput of gas-liquid mixing. The solution includes a shell, a second fixing plate fixedly arranged in the shell from top to bottom, several mixing modules, a first fixing plate, and a gas distribution plate.

[0004] For example, Chinese patent CN118788271B discloses a method to set up a pressurization zone in the channel of a continuous flow microchannel reactor and use a micro diaphragm pump to intermittently apply pressure in the pressurization zone, thereby pressurizing the fluid in the channel of the continuous flow microchannel reactor and increasing the fluid flow rate in the channel of the continuous flow microchannel reactor.

[0005] As mentioned above, using the microreactor described in Scheme 2 combined with the gas-liquid mixer in Scheme 1 to prepare butanol can effectively improve its production efficiency and quality. However, in the preparation of butanol, both the hydroformylation and hydrogenation reactions are exothermic. Therefore, effective temperature control is required during the reaction to avoid overheating, which could lead to an increase in side reactions or catalyst deactivation. In the existing technology, reactor coils are usually used for cooling. However, the reaction liquid in the coil is limited, resulting in a limited amount of liquid participating in the cooling process. This can easily lead to insufficient cooling, meaning that the temperature adjustment margin of the reactor coil is small, resulting in low energy utilization and difficulty in accurately controlling the temperature. Summary of the Invention

[0006] The purpose of this invention is to provide a method for preparing butanol using a continuous flow heat exchange microreactor, which has the advantages of temperature regulation and synchronous control, and solves the problems mentioned in the background art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing butanol using a continuous flow heat exchange microreactor, comprising the following steps: S1, hydroformylation reaction; S2, hydrogenation reaction; S3, temperature control; S4, data monitoring.

[0008] S1, hydroformylation reaction: A mixture of propylene, carbon monoxide and hydrogen is fed into the first parallel feed pipe. The mixture is mixed and emulsified when it passes through the first micro mixer, and a circulation loop is formed inside the first carbonyl reactor to carry out a chemical reaction. The product after the reaction is discharged through the discharge pipe.

[0009] S2, Hydrogenation reaction: The product discharged from the discharge pipe 1 is pumped into the feed pipe through the circulation pump 1, and then enters the second carbonyl reactor. When passing through the second micro mixer, it is mixed and emulsified again. Then, a circulation loop is formed inside the second carbonyl reactor to carry out a chemical reaction. The product after the reaction is discharged into the discharge pipe 2.

[0010] S3. Temperature control: The product discharged from the discharge pipe 2 enters the cooler for cooling. After being cooled to the set temperature, the product enters the circulation pump 2 and is pumped to the cooling pipe. Subsequently, the product is split into the split pipe 1 and the split pipe 2, and heat exchangers 1 and 2 are used to exchange heat with the first carbonyl reactor and the second carbonyl reactor respectively, thus completing the temperature control of the reaction process of the first carbonyl reactor and the second carbonyl reactor. The product after heat exchange is discharged into the collection box through the discharge pipe. After separation in the collection box, butanol is obtained.

[0011] S4. Data Monitoring: During the reaction processes of S1 and S2, the reaction temperatures of the first carbonyl reactor and the second carbonyl reactor are monitored in real time by the control module. Based on the recorded data, the required heat exchange amount is fitted, and then the operation of the regulating mechanism is controlled. The regulating mechanism controls the flow ratio of the heat exchange mechanism according to the analysis results, and performs synchronous temperature control on the hydroformylation reaction and the hydrogenation reaction.

[0012] Preferably, the device includes a first carbonyl reactor, a heat exchange mechanism, an adjustment mechanism, and a control module. A first parallel feed pipe is provided through the first carbonyl reactor. A first micro mixer is provided inside the first carbonyl reactor, and two outlets at the bottom of the first parallel feed pipe are connected to the first micro mixer. A discharge pipe is provided through the bottom of the first carbonyl reactor. The other end of the discharge pipe is connected to a circulation pump, and the other end of the circulation pump is connected to a feed guide pipe.

[0013] Preferably, the other end of the feed pipe is connected to a second parallel feed pipe, and a second carbonyl reactor is disposed through the outer contour of the second parallel feed pipe. The two outlets at the bottom of the second parallel feed pipe are connected to the same second micro mixer, which is disposed inside the second carbonyl reactor. The bottom end of the second carbonyl reactor is connected to a second discharge pipe, the other end of which is connected to a cooler, and the other end of which is connected to a second circulation pump.

[0014] Preferably, the heat exchange mechanism includes a cooling pipe for completing the cooling product conveying process. The cooling pipe is connected to the other end of the second circulating pump. The other end of the cooling pipe is connected to a first branch pipe and a second branch pipe. The other end of the first branch pipe is connected to a first heat exchanger, which surrounds the outside of the first carbonyl reactor. The other end of the second branch pipe is connected to a second heat exchanger, which surrounds the outside of the second carbonyl reactor. The other ends of the first and second heat exchangers are connected to a discharge pipe. A discharge port is provided in the middle section of the discharge pipe, and a collection frame is placed below the discharge port.

[0015] Preferably, the regulating mechanism includes a needle valve one for controlling the flow ratio of the heat exchange mechanism. The needle valve one is disposed on the outer contour of the diverter pipe one. A valve one penetrates through the top end of the needle valve one, and the bottom end of the valve one extends into the interior of the needle valve one and controls the opening degree of the needle valve one. A positioning plate is sleeved on the outer contour of the valve one. A drive wheel is connected through and limited to the other end of the positioning plate. A motor is fixedly connected to the top end of the drive wheel. The drive wheel meshes with the valve one and is connected for transmission. A lever is fixedly connected to one side of the positioning plate.

[0016] Preferably, the adjusting mechanism further includes a needle valve two disposed on the outer contour of the second diverter pipe, the top end of the needle valve two having a valve two extending through it, the valve two being intermittently meshing and connected to the drive wheel, and the bottom end of the valve two extending into the interior of the needle valve two and controlling the opening degree of the needle valve two.

[0017] Preferably, the control module includes temperature sensors mounted on heat exchanger one and heat exchanger two to monitor the reaction temperatures of the first and second carbonyl reactors, and a transmission structure that controls the deflection of the positioning plate and lever to engage the drive wheel with valve two. The temperature monitoring steps for the first and second carbonyl reactors are as follows:

[0018] S41. Change value recording: Before the preparation process begins, record the initial temperature of the first carbonyl reactor and the second carbonyl reactor. After the preparation process begins, record the temperature of the first carbonyl reactor and the second carbonyl reactor again and mark the part that exceeds the set temperature as ΔT.

[0019] S42. Data analysis: Using the recorded ΔT, combined with the heat balance calculation formula: Q=m*c p *ΔT+Q1, calculate the excess reaction heat Q of the first carbonyl reactor and the second carbonyl reactor respectively, where:

[0020] m: The mass of the reaction system, calculated based on the amount of raw materials added.

[0021] c p The specific heat capacity of the reaction system is calculated based on the type and proportion of the raw materials.

[0022] ΔT: Temperature change of the reaction system, obtained by monitoring the control module.

[0023] Q1: The environmental heat loss of the reaction system was determined experimentally.

[0024] Preferably, the specific steps for the regulating mechanism to control the flow ratio of the heat exchange mechanism based on the analysis results are as follows:

[0025] S43. Result Calculation: Calculate the valve opening of the heat exchange mechanism at this time using the excess reaction heat Q obtained in S42 and the flow rate formula. The specific calculation formula is as follows: in:

[0026] c v Flow coefficient, representing the flow capacity of a valve when it is fully open;

[0027] ΔP: Pressure difference across the valve, measured according to the actual scenario;

[0028] SG: Specific gravity of the cooling fluid, measured based on the actual product;

[0029] c p1 The specific heat capacity of the cooling fluid is calculated based on the type and proportion of the actual products.

[0030] x: Opening degree of needle valve one and needle valve two;

[0031] S44. Control and Regulation: Based on the valve opening calculated in S43, the flow ratio of the heat exchange mechanism is controlled accordingly. By adjusting the flow ratio, the heat exchange between heat exchanger one and heat exchanger two is controlled, thereby completing the synchronous temperature control process of the first carbonyl reactor and the second carbonyl reactor.

[0032] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0033] 1. This invention achieves temperature control of the reaction process by setting up a heat exchange mechanism to replace the reactor coil. The temperature control process has a large margin for adjustment and a large amount of temperature adjustment, thus effectively achieving precise temperature control.

[0034] 2. By setting up an adjustment mechanism, the present invention achieves synchronous temperature control of reaction process one and reaction process two by controlling the flow ratio of the heat exchange mechanism, which simplifies the operation process and further improves the integration of the device.

[0035] 3. This invention achieves automatic temperature control by setting up a control module, monitoring and analyzing the current data throughout the reaction process, and automatically controlling the adjustment mechanism and heat exchange mechanism based on the current feedback data. Attached Figure Description

[0036] Figure 1This is a schematic diagram of the main structure of the present invention;

[0037] Figure 2 This is a partial sectional view of the main structure of the present invention;

[0038] Figure 3 This is a schematic diagram of the interior of the carbonyl reactor of the present invention;

[0039] Figure 4 This is a schematic diagram of the connection relationship in reaction process one of the present invention;

[0040] Figure 5 This is a schematic diagram showing the connection relationship between the heat exchange mechanism and the regulating mechanism of the present invention;

[0041] Figure 6 This is a schematic diagram of the adjustment mechanism of the present invention;

[0042] Figure 7 This is a diagram of the reaction process of the present invention;

[0043] Figure 8 This is a flowchart illustrating the overall workflow of the present invention.

[0044] In the diagram: 1. First carbonyl reactor; 11. First parallel feed pipe; 12. First micro mixer; 13. Discharge pipe one; 14. Circulation pump one; 15. Feed guide pipe; 2. Second carbonyl reactor; 21. Second parallel feed pipe; 22. Second micro mixer; 23. Discharge pipe two; 24. Cooler; 25. Circulation pump two; 3. Cooling pipe; 31. Diverter pipe one; 32. Diverter pipe two; 33. Heat exchanger one; 34. Heat exchanger two; 35. Discharge pipe; 36. Collection frame; 4. Needle valve one; 41. Valve one; 42. Positioning plate; 43. Lever; 44. Drive wheel; 45. Motor; 46. Needle valve two; 47. Valve two. Detailed Implementation

[0045] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0046] Example 1:

[0047] Please see Figures 1 to 8 The present invention provides a technical solution: a method for preparing butanol using a continuous flow heat exchange microreactor, comprising the following steps: S1, hydroformylation reaction; S2, hydrogenation reaction; S3, temperature control; S4, data monitoring.

[0048] S1, hydroformylation reaction: A mixture of propylene, carbon monoxide and hydrogen is fed into the first parallel feed pipe 11. When the mixture passes through the first micro mixer 12, it undergoes mixing and emulsification, and forms a circulation loop inside the first carbonyl reactor 1 to carry out a chemical reaction. The product after the reaction is discharged through the discharge pipe 13.

[0049] S2, Hydrogenation reaction: The product discharged from the discharge pipe 13 is pumped into the feed pipe 15 through the circulation pump 14, and then enters the second carbonyl reactor 2. When passing through the second micro mixer 22, it is mixed and emulsified again. Then, a circulation loop is formed inside the second carbonyl reactor 2 to carry out a chemical reaction. The product after the reaction is discharged into the discharge pipe 23.

[0050] S3. Temperature control: The product discharged from the discharge pipe 23 enters the cooler 24 for cooling. After being cooled to the set temperature, the product enters the circulation pump 25 and is pumped to the cooling pipe 3. Subsequently, the product is split into the split pipe 31 and the split pipe 32, and heat exchangers 33 and 34 are used to exchange heat with the first carbonyl reactor 1 and the second carbonyl reactor 2 respectively, thus completing the temperature control of the reaction process of the first carbonyl reactor 1 and the second carbonyl reactor 2. The product after heat exchange is discharged into the collection frame 36 through the discharge pipe 35. After separation in the collection frame 36, butanol is obtained.

[0051] S4. Data Monitoring: During the reaction processes of S1 and S2, the reaction temperatures of the first carbonyl reactor 1 and the second carbonyl reactor 2 are monitored in real time by the control module. Based on the recorded data, the required heat exchange amount is fitted, and then the operation of the regulating mechanism is controlled. The regulating mechanism controls the flow ratio of the heat exchange mechanism according to the analysis results, and performs synchronous temperature control on the hydroformylation reaction and the hydrogenation reaction.

[0052] In this scheme, the reactor coil is replaced by a heat exchange mechanism, a regulating mechanism, and a control module to achieve precise temperature control. The cooled product is used to exchange heat with the reaction process, avoiding the problem of insufficient cooling caused by the limited liquid volume in the coil. At the same time, this temperature control method is not limited by the pump feed rate, the temperature control speed is easy to operate, and it is not likely to cause the limitation of slow temperature rise in the second carbonyl reactor 2. On the other hand, precise temperature control can increase the gas-liquid contact area in the reaction process, increase the phase interface area and mass transfer rate, improve the material conversion rate and the reactor processing capacity, and reduce the coalescence of bubbles in the mixture. The equipment is integrated, reducing investment costs.

[0053] Example 2:

[0054] The device includes a first carbonyl reactor 1, a heat exchange mechanism, an adjustment mechanism, and a control module. A first parallel feed pipe 11 is provided through the first carbonyl reactor 1. A first micro mixer 12 is provided inside the first carbonyl reactor 1, and the two outlets at the bottom of the first parallel feed pipe 11 are connected to the first micro mixer 12. A discharge pipe 13 is provided through the bottom of the first carbonyl reactor 1. The other end of the discharge pipe 13 is connected to a circulation pump 14, and the other end of the circulation pump 14 is connected to a feed guide pipe 15.

[0055] The other end of the feed pipe 15 is connected to a second parallel feed pipe 21. A second carbonyl reactor 2 is installed through the outer contour of the second parallel feed pipe 21. The two outlets at the bottom of the second parallel feed pipe 21 are connected to the same second micro mixer 22. The second micro mixer 22 is located inside the second carbonyl reactor 2. The bottom end of the second carbonyl reactor 2 is connected to a discharge pipe 23. The other end of the discharge pipe 23 is connected to a cooler 24. The other end of the cooler 24 is connected to a circulation pump 25.

[0056] A mixture of propylene, carbon monoxide, and hydrogen is fed into the first parallel feed pipe 11. A premixing chamber is provided inside the first micromixer 12. After entering the first micromixer 12, the raw material mixture undergoes mixing and emulsification through micro-interface technology and is further refined before being injected into the first carbonyl reactor 1 to begin the reaction. The main reaction equation inside the first carbonyl reactor 1 is:

[0057] C3H6 + CO + H2 → C4H8O (Butyraldehyde)

[0058] This reaction is exothermic, so the temperature of the first carbonyl reactor 1 will gradually increase during the reaction. The reaction conditions are 80-150℃. When the temperature of the first carbonyl reactor 1 exceeds the threshold, overheating will occur, leading to side reactions or catalyst deactivation, which in turn will reduce the preparation efficiency and quality.

[0059] Furthermore, the reaction product, mainly butyraldehyde, is discharged into the discharge pipe 13 and pumped by the circulation pump 14 into the feed pipe 15 and the second parallel feed pipe 21. The second micro-mixer 22 has a premixing chamber inside. After the material enters the second micro-mixer 22, it is mixed and emulsified again through micro-interface technology. Subsequently, it reacts further inside the second carbonyl reactor 2. At this time, the main reaction equation inside the second carbonyl reactor 2 is:

[0060] C4H8O + H2 → C4H 10 O(butanol)

[0061] This reaction process is also exothermic, so the temperature of the second carbonyl reactor 2 increases synchronously. When the temperature of the second carbonyl reactor 2 exceeds the reaction condition temperature by 100-150℃, overheating will also occur, leading to side reactions or catalyst deactivation. Therefore, it is necessary to cool down both reaction processes to control their reaction temperature.

[0062] The product after complete reaction is mainly butanol, mixed with some unreacted raw materials and catalyst. This mixture is injected into cooler 24 through discharge pipe 23. Cooler 24 cools the mixture to a set temperature and serves as a cooling fluid for cooling the first carbonyl reactor 1 and the second carbonyl reactor 2. Then, the mixture is pumped to the heat exchange mechanism by circulating pump 25.

[0063] Example 3:

[0064] The heat exchange mechanism includes a cooling pipe 3 for completing the cooling product conveying process. The cooling pipe 3 is connected to the other end of the second circulating pump 25. The other end of the cooling pipe 3 is connected to a first branch pipe 31 and a second branch pipe 32. The other end of the first branch pipe 31 is connected to a first heat exchanger 33, which surrounds the outside of the first carbonyl reactor 1. The other end of the second branch pipe 32 is connected to a second heat exchanger 34, which surrounds the outside of the second carbonyl reactor 2. The other ends of the first heat exchanger 33 and the second heat exchanger 34 are connected to a discharge pipe 35. A discharge port is provided in the middle section of the discharge pipe 35, and a collection frame 36 is placed below the discharge port.

[0065] The regulating mechanism includes a needle valve 4 for controlling the flow ratio of the heat exchange mechanism. The needle valve 4 is disposed on the outer contour of the diversion pipe 31. A valve 41 passes through the top of the needle valve 4, and the bottom of the valve 41 extends into the needle valve 4 and controls the opening of the needle valve 4. A positioning plate 42 is sleeved on the outer contour of the valve 41. The other end of the positioning plate 42 is penetrated and connected to a drive wheel 44 for rotatable limitation. A motor 45 is fixedly connected to the top of the drive wheel 44. The drive wheel 44 meshes with the valve 41 and is connected for transmission. A lever 43 is fixedly connected to one side of the positioning plate 42.

[0066] The regulating mechanism also includes a needle valve 46 disposed on the outer contour of the second diversion pipe 32. A valve 47 passes through the top of the needle valve 46. The valve 47 is intermittently meshed with the drive wheel 44. The bottom end of the valve 47 extends into the interior of the needle valve 46 and controls the opening degree of the needle valve 46.

[0067] The mixed cooling fluid pumped to the cooling pipe 3 is split through the first split pipe 31 and the second split pipe 32, and then undergoes heat exchange with the first carbonyl reactor 1 and the second carbonyl reactor 2 inside the first heat exchanger 33 and the second heat exchanger 34, thereby realizing the temperature control function of the first carbonyl reactor 1 and the second carbonyl reactor 2. The cooling fluid after heat exchange is discharged into the collection frame 36 through the discharge pipe 35, and the preparation of butanol is completed under the separation operation.

[0068] It should be noted that when the cooling fluid is split through the first split pipe 31 and the second split pipe 32, the initial flow rate in the first split pipe 31 and the second split pipe 32 is the same. That is, at this time, the heat exchange capacity of the first heat exchanger 33 and the second heat exchanger 34 is the same. However, the reaction conditions inside the first carbonyl reactor 1 and the second carbonyl reactor 2 are different. Therefore, it is necessary to control the flow rate in the first split pipe 31 and the second split pipe 32 to achieve synchronous temperature control of the first carbonyl reactor 1 and the second carbonyl reactor 2 by the first heat exchanger 33 and the second heat exchanger 34.

[0069] The function of controlling the flow rate inside the first diversion pipe 31 and the second diversion pipe 32 is achieved through an adjustment mechanism. When the drive wheel 44 engages with the second valve 47, the drive motor 45 drives the drive wheel 44 to rotate. The drive wheel 44 further drives the first valve 41 and the second valve 47 to rotate synchronously. At this time, the rotation of the first valve 41 causes the opening of the first needle valve 4 to gradually decrease, which in turn causes the first needle valve 4 to gradually cut off the flow of fluid inside the first diversion pipe 31, and the flow rate inside the first diversion pipe 31 decreases synchronously. Similarly, the rotation of the second valve 47 causes the opening of the second needle valve 46 to decrease. The second needle valve 46 cuts off the flow of fluid inside the second diversion pipe 32, causing the flow rate inside the second diversion pipe 32 to decrease. That is, with the rotation of the drive wheel 44, the opening of the first needle valve 4 and the second needle valve 46 gradually decreases, and the flow rate inside the first diversion pipe 31 and the second diversion pipe 32 decreases synchronously.

[0070] When the drive wheel 44 is not engaged with valve 47, valve 47 can rotate independently, meaning the flow rate of the diversion pipe 32 can be adjusted independently. Since the reaction conditions in the first carbonyl reactor 1 and the second carbonyl reactor 2 are different (the internal temperature of the second carbonyl reactor 2 is higher than that of the first carbonyl reactor 1), it is necessary to control the heat exchange rate of heat exchanger 34 to be less than that of heat exchanger 33. This is achieved by adjusting the diversion pipe 32 independently so that its initial flow rate is less than that of diversion pipe 31. Subsequently, the lever 43 and the positioning plate 42 are deflected to engage the drive wheel 44 and valve 47. During the rotation of the drive wheel 44, the rotation speeds of valve 47 and valve 41 are the same, meaning the flow rates of the flow in the first and second branch pipes 31 and 32 are the same. At this time, the flow ratio between the first and second branch pipes 31 and 32 mainly depends on the difference in their initial flow rates. This ensures that the heat exchange of the second heat exchanger 34 is less than that of the first heat exchanger 33 during the synchronous temperature control of the first carbonyl reactor 1 and the second carbonyl reactor 2, thereby ensuring that the temperature of the second carbonyl reactor 2 is higher than that of the first carbonyl reactor 1 to meet the different reaction conditions between the first carbonyl reactor 1 and the second carbonyl reactor 2.

[0071] It should be noted that the switching of motor 45 and the deflection of lever 43 and drive wheel 44 during the above adjustment process are all achieved through the control module. The adjustment process is simple and can effectively improve the automation and integration of the device in the scheme, thereby improving the production efficiency and quality of butanol.

[0072] On the other hand, during the reaction process of the first carbonyl reactor 1 and the second carbonyl reactor 2, as the reaction time increases, the reaction rate decreases due to the gradual decrease in the concentration of reactants inside the first carbonyl reactor 1 and the second carbonyl reactor 2. At this time, the temperature rise trend of the first carbonyl reactor 1 and the second carbonyl reactor 2 decreases synchronously, that is, the required heat exchange amount of the first carbonyl reactor 1 and the second carbonyl reactor 2 decreases synchronously. Therefore, the required heat exchange amount of the first carbonyl reactor 1 and the second carbonyl reactor 2 is calculated based on the data monitored in real time by the control module. The dynamic control adjustment mechanism and the heat exchange mechanism are used to limit the flow of the first branch pipe 31 and the second branch pipe 32, thereby realizing the dynamic adjustment of the temperature control of the reaction process.

[0073] Example 4:

[0074] The control module includes temperature sensors installed on heat exchanger 33 and heat exchanger 34 to monitor the reaction temperatures of the first carbonyl reactor 1 and the second carbonyl reactor 2, as well as a transmission structure that controls the deflection of the positioning plate 42 and the lever 43 to engage the drive wheel 44 with the valve 47. The temperature monitoring steps for the first carbonyl reactor 1 and the second carbonyl reactor 2 are as follows:

[0075] S41. Change value recording: Before the preparation process begins, record the initial temperature of the first carbonyl reactor 1 and the second carbonyl reactor 2. After the preparation process begins, record the temperature of the first carbonyl reactor 1 and the second carbonyl reactor 2 again and mark the part that exceeds the set temperature as ΔT.

[0076] S42. Data analysis: Using the recorded ΔT, combined with the heat balance calculation formula: Q=m*c p *ΔT+Q1, calculate the excess reaction heat Q of the first carbonyl reactor 1 and the second carbonyl reactor 2 respectively, where:

[0077] m: The mass of the reaction system, calculated based on the amount of raw materials added.

[0078] c p The specific heat capacity of the reaction system is calculated based on the type and proportion of the raw materials.

[0079] ΔT: Temperature change of the reaction system, obtained by monitoring the control module.

[0080] Q1: The environmental heat loss of the reaction system was determined experimentally.

[0081] The specific steps for the regulating mechanism to control the flow ratio of the heat exchanger based on the analysis results are as follows:

[0082] S43. Result Calculation: Calculate the valve opening of the heat exchange mechanism at this time using the excess reaction heat Q obtained in S42 and the flow rate formula. The specific calculation formula is as follows: in:

[0083] c v Flow coefficient, representing the flow capacity of a valve when it is fully open;

[0084] ΔP: Pressure difference across the valve, measured according to the actual scenario;

[0085] SG: Specific gravity of the cooling fluid, measured based on the actual product;

[0086] c p1 The specific heat capacity of the cooling fluid is calculated based on the type and proportion of the actual products.

[0087] x: The opening degree of needle valve 4 and needle valve 46;

[0088] S44. Control and Regulation: Based on the valve opening calculated in S43, the flow ratio of the heat exchange mechanism is controlled accordingly. By adjusting the flow ratio, the heat exchange capacity of heat exchanger 1 33 and heat exchanger 2 34 is controlled, thereby completing the synchronous temperature control process of the first carbonyl reactor 1 and the second carbonyl reactor 2.

[0089] In this scheme, the microchannel structure of the first micromixer 12 and the second micromixer 22 provides an extremely high specific surface area, which can quickly transfer heat and mass, significantly improving reaction efficiency; at the same time, the amount of reactants required is small and the reaction conditions are optimized, reducing the waste of raw materials and energy; the reactants continuously enter the first micromixer 12 and the second micromixer 22, and the products continuously flow out, which is suitable for large-scale industrial production.

[0090] The excess heat of reaction of the first carbonyl reactor 1 and the second carbonyl reactor 2 is calculated, which is the amount of heat exchange required for the first carbonyl reactor 1 and the second carbonyl reactor 2 to drop from their current temperature to the set temperature. According to the heat balance equation, the amount of heat exchange required for the temperature of the first carbonyl reactor 1 and the second carbonyl reactor 2 to drop is equal to the amount of heat exchange required for the cooling fluid to rise. The amount of heat exchange of the cooling fluid in heat exchanger 1 33 and heat exchanger 2 34 is limited by the flow rate in the split pipe 1 31 and split pipe 2 32. Therefore, by adjusting the opening of needle valve 1 4 and needle valve 2 46, the flow rate in split pipe 1 31 and split pipe 2 32 can be effectively limited, thereby controlling the amount of heat exchange of the cooling fluid in heat exchanger 1 33 and heat exchanger 2 34, and achieving precise temperature control of the first carbonyl reactor 1 and the second carbonyl reactor 2.

[0091] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing butanol using a continuous flow heat exchange microreactor, characterized in that: Includes the following steps: S1, hydroformylation reaction; S2, hydrogenation reaction; S3, temperature control; S4, data monitoring.

2. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 1, characterized in that: The S1 hydroformylation reaction includes passing a mixture of propylene, carbon monoxide and hydrogen into the first parallel feed pipe (11). When the mixture passes through the first micro mixer (12), it undergoes mixing and emulsification and forms a circulation loop inside the first carbonyl reactor (1) to carry out a chemical reaction. The product after the reaction is discharged through the discharge pipe (13). The S2 hydrogenation reaction involves the product discharged from the discharge pipe one (13) being pumped into the feed pipe (15) by the circulation pump one (14), and then entering the second carbonyl reactor (2) where it is mixed and emulsified again when passing through the second micro mixer (22). Subsequently, a circulation loop is formed inside the second carbonyl reactor (2) where a chemical reaction occurs, and the product after the reaction is discharged into the discharge pipe two (23). The temperature control in S3 includes the product discharged from the discharge pipe 2 (23) entering the cooler (24) for cooling. After being cooled to the set temperature, the product enters the circulation pump 2 (25) and is pumped to the cooling pipe (3). Subsequently, the product is diverted to the diversion pipe 1 (31) and the diversion pipe 2 (32), and heat exchange is performed on the first carbonyl reactor (1) and the second carbonyl reactor (2) through the heat exchanger 1 (33) and the heat exchanger 2 (34) respectively, thus completing the temperature control of the reaction process of the first carbonyl reactor (1) and the second carbonyl reactor (2). After heat exchange, the product is discharged into the collection frame (36) through the discharge pipe (35). After separation in the collection frame (36), butanol is obtained. The S4 data monitoring includes real-time monitoring of the reaction temperatures of the first carbonyl reactor (1) and the second carbonyl reactor (2) through the control module during the reaction processes of S1 and S2, fitting the required heat exchange amount based on the recorded data, and then controlling the operation of the regulating mechanism. The regulating mechanism controls the flow ratio of the heat exchange mechanism based on the analysis results, and performs synchronous temperature control on the hydroformylation reaction and the hydrogenation reaction.

3. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 2, characterized in that: The device includes a first carbonyl reactor (1), a heat exchange mechanism, an adjustment mechanism, and a control module. A first parallel feed pipe (11) is provided through the first carbonyl reactor (1). A first micro mixer (12) is provided inside the first carbonyl reactor (1), and the two output ports at the bottom of the first parallel feed pipe (11) are connected to the first micro mixer (12). A discharge pipe (13) is provided through the bottom of the first carbonyl reactor (1). The other end of the discharge pipe (13) is connected to a circulation pump (14), and the other end of the circulation pump (14) is connected to a feed pipe (15).

4. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 3, characterized in that: The other end of the feed pipe (15) is connected to a second parallel feed pipe (21). A second carbonyl reactor (2) is installed through the outer contour of the second parallel feed pipe (21). The two outlets at the bottom of the second parallel feed pipe (21) are connected to the same second micro mixer (22). The second micro mixer (22) is located inside the second carbonyl reactor (2). The bottom end of the second carbonyl reactor (2) is connected to a discharge pipe (23). The other end of the discharge pipe (23) is connected to a cooler (24). The other end of the cooler (24) is connected to a circulating pump (25).

5. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 3, characterized in that: The heat exchange mechanism includes a cooling pipe (3) for completing the cooling product conveying process. The cooling pipe (3) is connected to the other end of the circulating pump (25). The other end of the cooling pipe (3) is connected to a first branch pipe (31) and a second branch pipe (32). The other end of the first branch pipe (31) is connected to a first heat exchanger (33), which surrounds the outside of the first carbonyl reactor (1). The other end of the second branch pipe (32) is connected to a second heat exchanger (34), which surrounds the outside of the second carbonyl reactor (2). The other ends of the first heat exchanger (33) and the second heat exchanger (34) are connected to a discharge pipe (35). The middle section of the discharge pipe (35) is provided with a discharge port, and a collection frame (36) is placed below the discharge port.

6. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 3, characterized in that: The regulating mechanism includes a needle valve (4) for controlling the flow ratio of the heat exchange mechanism. The needle valve (4) is set on the outer contour of the diversion pipe (31). A valve (41) passes through the top of the needle valve (4). The bottom of the valve (41) extends into the interior of the needle valve (4) and controls the opening degree of the needle valve (4). A positioning plate (42) is sleeved on the outer contour of the valve (41). The other end of the positioning plate (42) is penetrated and connected to a drive wheel (44) for limited rotation. A motor (45) is fixedly connected to the top of the drive wheel (44). The drive wheel (44) meshes with the valve (41) and is connected for transmission. A lever (43) is fixedly connected to one side of the positioning plate (42).

7. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 3, characterized in that: The regulating mechanism also includes a needle valve 2 (46) disposed on the outer contour of the diverter pipe 2 (32). A valve 2 (47) passes through the top of the needle valve 2 (46). The valve 2 (47) is intermittently meshed with the drive wheel (44). The bottom end of the valve 2 (47) extends into the interior of the needle valve 2 (46) and controls the opening degree of the needle valve 2 (46).

8. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 3, characterized in that: The control module includes temperature sensors installed on heat exchanger one (33) and heat exchanger two (34) to monitor the reaction temperatures of the first carbonyl reactor (1) and the second carbonyl reactor (2), as well as a transmission structure that controls the deflection of the positioning plate (42) and the lever (43) to complete the engagement of the drive wheel (44) with the valve two (47). The temperature monitoring steps for the first carbonyl reactor (1) and the second carbonyl reactor (2) are as follows: S41. Change value recording: Before the preparation process begins, record the initial temperature of the first carbonyl reactor (1) and the second carbonyl reactor (2). After the preparation process begins, record the temperature of the first carbonyl reactor (1) and the second carbonyl reactor (2) again and mark the part that exceeds the set temperature. ; S42. Data analysis, utilizing records ， Using the formula for calculating thermal equilibrium: The excess heat of reaction for the first carbonyl reactor (1) and the second carbonyl reactor (2) was calculated respectively. Q ,in: The mass of the reaction system is calculated based on the amount of raw materials added. The specific heat capacity of the reaction system is calculated based on the type and proportion of the raw materials. The temperature change of the reaction system is monitored and obtained by the control module. The environmental heat loss of the reaction system was determined experimentally.

9. The method for preparing butanol using a continuous flow heat exchange microreactor according to claim 1, characterized in that: The specific steps for the regulating mechanism to control the flow ratio of the heat exchanger based on the analysis results are as follows: S43. Result Calculation: Calculate the excess heat of reaction obtained in S42. Q The valve opening of the heat exchange mechanism at this time is calculated using the flow rate formula. The specific calculation formula is as follows: ;in: Flow coefficient, representing the flow capacity of a valve when it is fully open; The pressure difference across the valve is measured based on the actual scenario. The specific gravity of the cooling fluid is determined based on the actual product. The specific heat capacity of the cooling fluid is calculated based on the type and proportion of the actual products. The opening degree of needle valve one (4) and needle valve two (46); S44. Control and Regulation: Based on the valve opening calculated in S43, the flow ratio of the heat exchange mechanism is controlled accordingly. By adjusting the flow ratio, the heat exchange amount of heat exchanger one (33) and heat exchanger two (34) is controlled, thus completing the synchronous temperature control process of the first carbonyl reactor (1) and the second carbonyl reactor (2).

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