Continuous hydrogenation reaction system
By designing a continuous hydrogenation reaction system, the problems of overpressure and low mass transfer efficiency in batch reactors and easy clogging in fixed-bed reactors were solved, achieving efficient catalyst pretreatment and stable operation of the production process, and improving product yield and purity.
Patent Information
- Application Number
- CN202423263626.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-12-09
- Estimated Expiration
- 2034-12-27
AI Technical Summary
Existing batch reactors have the risks of overpressure, low mass transfer efficiency, and heavy metal residues, while fixed-bed reactors are prone to clogging and have strict requirements on catalyst particle size, leading to unstable production and catalyst waste.
A continuous hydrogenation reaction system was designed, including a feeding module, an inlet module, a reaction module, a separation module, and a collection module. It adopts a fixed-bed reactor parallel and series pipeline design to achieve individual pretreatment of the catalyst and short-circuiting in case of blockage, thus ensuring continuous production.
It improves catalyst activation and product yield, reduces the risk of clogging, ensures the stability and efficiency of the production process, and reduces catalyst waste.
Smart Images
Figure CN223641805U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to a continuous hydrogenation reaction system. Background Technology
[0002] In recent years, hydrogenation reactions have been increasingly used in the preparation of pharmaceutical intermediates, and can be classified into hydrogenation, deprotection, and reduction reactions according to substrate type. Currently, hydrogenation reactions are usually carried out in batch reactors and fixed-bed reactors.
[0003] There are a series of unavoidable risks in carrying out hydrogenation reactions in a batch reactor: (1) For some deprotection reactions that produce gas, there is a risk of overpressure when using a batch reactor; (2) The general hydrogenation reaction is a gas-solid-liquid three-phase reaction, and the mass transfer efficiency of the batch reactor is low, the reaction time is long, and there is a risk of side reactions; (3) After obtaining the product solution using a batch reactor, the catalyst still needs to be filtered and separated, and there is a risk of heavy metal residues; while the fixed bed reactor can solve the above-mentioned drawbacks of the batch reactor.
[0004] However, at the same time, fixed-bed reactors also have some specific problems: (1) Fixed-bed reactors have certain requirements for the particle size of catalysts. Fine-particle catalysts will cause the fixed bed pressure drop to be high; (2) When using some catalysts with insufficient mechanical strength or easy to shed carbon powder, it may cause the fixed bed to be blocked, affecting subsequent normal use. Utility Model Content
[0005] This invention addresses the problem of catalyst and its debris clogging fixed-bed reactors in actual production by providing a continuous hydrogenation reaction system. The continuous hydrogenation reaction system provided by this invention can fully pretreat the catalyst, thereby effectively improving product yield and purity. It also avoids the risk of catalyst and its debris clogging the fixed-bed reactor and can safely and efficiently ensure the normal operation of the production process in the event of clogging.
[0006] The present invention solves the above-mentioned technical problems through the following technical solutions.
[0007] This utility model provides a continuous hydrogenation reaction system, which includes a feeding module, an inlet module, a reaction module, a separation module, and a collection module; wherein,
[0008] The feeding module includes a liquid raw material storage tank and a solvent storage tank;
[0009] The air intake module includes a gas storage tank;
[0010] The reaction module includes N fixed-bed reactors, where N is a positive integer greater than or equal to 2. Each fixed-bed reactor is equipped with an inlet, an outlet, and a gas-liquid disperser. The outlet of one fixed-bed reactor is connected to the inlet of the next fixed-bed reactor. The inlet of each fixed-bed reactor is also connected to the gas outlet of the gas storage tank, the discharge outlet of the liquid raw material storage tank, and the discharge outlet of the solvent storage tank via feed pipelines. The feed pipelines are divided into a main feed pipe and feed branch pipes connected to the main feed pipe and connected in parallel. Each feed branch pipe is connected to one of the fixed-bed reactors.
[0011] The separation module includes a gas-liquid separator and a degassing tank; the inlet of the gas-liquid separator is connected to the outlet of the last fixed-bed reactor; the outlet of each fixed-bed reactor is also connected to the degassing tank through a discharge pipeline; the discharge pipeline is divided into a main discharge pipe and parallel discharge branch pipes connected to the main discharge pipe; each discharge branch pipe is connected to one of the fixed-bed reactors; the outlet of the gas-liquid separator is also connected to the inlet of the degassing tank;
[0012] The collection module includes a waste liquid storage tank and a product collection tank; the inlets of the waste liquid storage tank and the product collection tank are respectively connected to the outlet of the degassing tank.
[0013] In this invention, when pretreating (e.g., rinsing) each of the fixed-bed reactors, the parallel piping between the fixed-bed reactors allows for individual pretreating of each reactor. After pretreating, the feed liquid discharged from the fixed-bed reactors bypasses the gas-liquid separator and is directly connected to the degassing tank for collection. Alternatively, the series piping between the fixed-bed reactors can sequentially and continuously pretreat all the fixed-bed reactors at once.
[0014] In this invention, the parallel pipelines between the fixed-bed reactors can also be used to short-circuit one or more of the fixed-bed reactors after blockage occurs during the production process, so as to ensure the normal operation of the production process.
[0015] In some preferred embodiments, a first valve is provided on the feed main between every two fixed-bed reactors; a second valve is provided on each of the discharge branch pipes; a third valve is provided on the connecting pipe between the outlet of each fixed-bed reactor and the inlet of the next fixed-bed reactor, the third valve being located downstream of the first valve; the opening and closing of the first valve, the second valve and the third valve are used to coordinate and control the parallel and series flow of materials between the fixed-bed reactors.
[0016] In some preferred embodiments, a preheater is provided between the liquid raw material storage tank, the solvent storage tank and the reaction module, and the preheater is used to heat the raw materials and solvent.
[0017] In some preferred embodiments, a feed pump is provided between the liquid raw material storage tank, the solvent storage tank and the preheater, the feed pump being used to pump the raw material and solvent into the fixed bed reactor; the feed pump is equipped with a mass flow meter for detecting the flow rate to accurately control the amount of material conveyed in the pipeline.
[0018] In some preferred embodiments, a raw material filter is provided between the liquid raw material storage tank and the feed pump, the raw material filter being used to remove solid impurities from the raw material.
[0019] In one specific embodiment, the outlet of the raw material filter and the outlet of the solvent storage tank are connected to the inlet of the feed pump via a three-way valve.
[0020] In some preferred embodiments, a gas mass flow meter is provided on the feed manifold between the gas storage tank and the reaction module to detect and control the amount of gas flowing out; the gas storage tank includes a high-pressure nitrogen cylinder and a high-pressure hydrogen cylinder; both the high-pressure nitrogen cylinder and the high-pressure hydrogen cylinder are connected to a pressure gauge, a pressure reducing valve, and a shut-off valve to control the pressure of the flowing gas or to shut off the gas.
[0021] In some preferred embodiments, the gas mass flow meter is further provided with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence; the signal receiving module is electrically connected to a pressure gauge located downstream of the gas mass flow meter, and is used to receive the pressure value of the first fixed bed reactor.
[0022] In the above scheme, the signal processing module can be used to determine whether the pressure of the first fixed-bed reactor exceeds or falls below the set theoretical pressure (e.g., 4 MPa); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the pressure of the first fixed-bed reactor (e.g., <3.8 MPa or >4.2 MPa) deviates from the set theoretical pressure; the signal output locking module is connected to the solenoid valve of the gas mass flow meter, and is used to issue a signal and lock the outlet of the gas mass flow meter when the pressure of the first fixed-bed reactor (e.g., <3.5 MPa or >4.5 MPa) deviates too much from the set theoretical pressure.
[0023] In one specific embodiment, the outlet of the high-pressure nitrogen cylinder and the outlet of the high-pressure hydrogen cylinder are connected to the inlet of the gas mass flow meter via a three-way valve.
[0024] In one specific embodiment, the outlet of the gas mass flow meter and the outlet of the preheater are connected to the inlet of the first fixed-bed reactor via a three-way valve.
[0025] In this invention, the inner cavity of the fixed bed reactor is uniformly filled with catalyst particles with a particle size of 100-1000 μm; the gas and liquid are mixed through a three-way valve and then enter the fixed bed reactor, flowing through the gas-liquid disperser to contact the catalyst particles.
[0026] In some preferred embodiments, a condenser is provided between the gas-liquid separator and the reaction module, the condenser being used to cool and condense the material.
[0027] In some preferred embodiments, a transfer pump is provided between the waste liquid storage tank, the product collection tank and the degassing tank, the transfer pump being used for directional material conveying; the transfer pump is equipped with a mass flow meter for detecting the flow rate to accurately control the amount of material conveyed in the pipeline.
[0028] In some preferred embodiments, a product filter is provided between the product collection tank and the transfer pump, the product filter being used to remove solid impurities from the material flowing out of the fixed-bed reactor.
[0029] In one specific embodiment, the outlet of the product filter is connected to the inlet of the waste liquid storage tank and the inlet of the product collection tank via a three-way valve.
[0030] In some preferred embodiments, the reaction module includes 2 to 8 fixed-bed reactors.
[0031] In some preferred embodiments, the reaction module includes four fixed-bed reactors.
[0032] In some preferred embodiments, the gas-liquid separator includes an adjustable back pressure valve, a level gauge, and a vacuum pressure valve. During actual operation, the adjustable back pressure valve, the level gauge, and the vacuum pressure valve cooperate to adjust the liquid level in the gas-liquid separator. The gas-liquid separator is also equipped with a control interlock device, which includes a signal receiving module, a signal processing module, and a signal output locking module connected in sequence. The signal receiving module is electrically connected to the level gauge and is used to receive the liquid level value of the solution in the gas-liquid separator.
[0033] In the above scheme, the pressure of the adjustable back pressure valve is preferably 0.1 to 5 MPa.
[0034] In the above scheme, the liquid level of the level gauge is preferably 5% to 50% of the volume of the gas-liquid separator.
[0035] In the above scheme, the signal processing module can be used to determine whether the liquid level of the solution in the gas-liquid separator exceeds or falls below the set theoretical liquid level (e.g., 20%); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the liquid level value of the solution in the gas-liquid separator (e.g., <15% or >25%) deviates from the set theoretical liquid level; the signal output locking module is connected to the vacuum pressure valve, and is used to issue a signal and lock the outlet of the gas-liquid separator when the liquid level value of the solution in the gas-liquid separator (e.g., <10% or >30%) deviates too much from the set theoretical liquid level.
[0036] In some preferred embodiments, the degassing tank includes a level gauge and a vacuum pressure valve; during actual operation, the level gauge and the vacuum pressure valve cooperate to adjust the liquid level in the degassing tank; the degassing tank is also equipped with a control interlocking device, which includes a signal receiving module, a signal processing module, and a signal output locking module connected in sequence; the signal receiving module is electrically connected to the level gauge and is used to receive the liquid level value of the solution in the degassing tank.
[0037] In the above scheme, the liquid level of the level gauge is preferably 1% to 50% of the volume of the degassing tank.
[0038] In the above scheme, the signal processing module can be used to determine whether the liquid level of the solution in the degassing tank exceeds or falls below the set theoretical liquid level (e.g., 20%); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the liquid level value of the solution in the degassing tank (e.g., <15% or >25%) deviates from the set theoretical liquid level; the signal output locking module is connected to the vacuum pressure valve, and is used to issue a signal and lock the outlet of the degassing tank when the liquid level value of the solution in the degassing tank (e.g., <10% or >30%) deviates too much from the set theoretical liquid level.
[0039] The positive and progressive effects of this utility model are as follows:
[0040] (1) The continuous hydrogenation reaction system provided by this utility model can fully pre-treat the catalyst. Pre-treating each of the fixed-bed reactors individually is more thorough than conventional pre-treatment methods. This not only reduces the risk of catalyst and its debris clogging the fixed-bed reactor during production and improves process stability, but also enables the catalyst to be effectively activated, significantly improving the product yield, purity and production efficiency.
[0041] (2) The continuous hydrogenation reaction system provided by this utility model can short-circuit one or more of the fixed bed reactors after the blockage occurs in the fixed bed reactor during the production process, so as to ensure the normal operation of the production process safely and efficiently. Attached Figure Description
[0042] Figure 1 This is a schematic diagram of the continuous hydrogenation reaction system of Embodiment 1 of this utility model.
[0043] Figure 2 This is a schematic diagram of the continuous hydrogenation reaction system of Comparative Example 1 of this utility model.
[0044] Explanation of reference numerals in the attached figures:
[0045] Liquid raw material storage tank 1
[0046] Solvent storage tank 2
[0047] High-pressure nitrogen cylinder 3
[0048] High-pressure hydrogen cylinder 4
[0049] Raw material filter 5
[0050] Gas mass flow meter 6
[0051] Feed pump 7
[0052] Preheater 8
[0053] First fixed-bed reactor 9
[0054] Second fixed-bed reactor 10
[0055] Third fixed-bed reactor 11
[0056] Fourth fixed-bed reactor 12
[0057] First gas-liquid disperser 13
[0058] Second gas-liquid disperser 14
[0059] Third gas-liquid disperser 15
[0060] Fourth gas-liquid disperser 16
[0061] Condenser 17
[0062] Gas-liquid separator 18
[0063] Degassing tank 19
[0064] Transfer pump 20
[0065] Product Filter 21
[0066] Waste liquid storage tank 22
[0067] Product collection container 23
[0068] First valves 101, 103 and 105
[0069] Second valves 102, 104, 106 and 108
[0070] Third valves 109, 110 and 111
[0071] Gate valves 107, 112, 113, 114 and 115. Detailed Implementation
[0072] The specific embodiments of this utility model will be further described below with reference to the accompanying drawings. It should be noted that these descriptions are for the purpose of aiding understanding of this utility model, but do not constitute a limitation thereof. Furthermore, the technical features involved in the various embodiments of this utility model described below can be combined with each other as long as they do not conflict with each other.
[0073] Example 1
[0074] This embodiment discloses a continuous hydrogenation reaction system, such as Figure 1 As shown, the continuous hydrogenation reaction system includes a feeding module, an inlet module, a reaction module, a separation module, and a collection module; wherein,
[0075] The feeding module includes a liquid raw material storage tank 1 and a solvent storage tank 2;
[0076] The intake module includes a gas storage tank;
[0077] The reaction module includes four fixed-bed reactors; each fixed-bed reactor is equipped with an inlet, an outlet, and a gas-liquid disperser; the outlet of the previous fixed-bed reactor is connected to the inlet of the next fixed-bed reactor; the inlet of each fixed-bed reactor is also connected to the gas outlet of the gas storage tank, the discharge outlet of the liquid raw material storage tank 1, and the discharge outlet of the solvent storage tank 2 through feed pipelines; the feed pipelines are divided into a main feed pipe and feed branch pipes connected to the main feed pipe and connected in parallel; each feed branch pipe is connected to a fixed-bed reactor.
[0078] The separation module includes a gas-liquid separator 18 and a degassing tank 19; the inlet of the gas-liquid separator 18 is connected to the outlet of the last fixed-bed reactor; the outlet of each fixed-bed reactor is also connected to the degassing tank 19 through a discharge pipeline; the discharge pipeline is divided into a main discharge pipeline and discharge branch pipelines connected to the main discharge pipeline and connected in parallel; each discharge branch pipeline is connected to a fixed-bed reactor; the outlet of the gas-liquid separator 18 is also connected to the inlet of the degassing tank 19.
[0079] The collection module includes a waste liquid storage tank 22 and a product collection tank 23; the inlets of the waste liquid storage tank 22 and the product collection tank 23 are respectively connected to the outlet of the degassing tank 19.
[0080] In this embodiment, when flushing each fixed-bed reactor, the parallel pipelines between each fixed-bed reactor can individually flush each fixed-bed reactor; after flushing, the liquid discharged from the fixed-bed reactor does not pass through the gas-liquid separator 18, but is directly connected to the degassing tank 19 for collection.
[0081] In this embodiment, the parallel pipelines between the fixed-bed reactors can also be used to short-circuit one or more fixed-bed reactors after blockage occurs during the production process, so as to ensure the normal operation of the production process.
[0082] In this embodiment, a first valve 101, 103, and 105 is provided on the feed main pipe between every two fixed-bed reactors; a second valve 102, 104, 106, and 108 is provided on each discharge branch pipe; a third valve 109, 110, and 111 is provided on the connecting pipe between the outlet of each fixed-bed reactor and the inlet of the next fixed-bed reactor, and the third valve is located downstream of the first valve; the opening and closing of the first, second, and third valves are used to coordinate and control the parallel and series flow of materials between the fixed-bed reactors.
[0083] In this embodiment, a preheater 8 is provided between the liquid raw material storage tank 1, the solvent storage tank 2 and the reaction module. The preheater 8 is used to heat the raw materials and solvent.
[0084] In this embodiment, a feed pump 7 is provided between the liquid raw material storage tank 1, the solvent storage tank 2 and the preheater 8. The feed pump 7 is used to pump the raw materials and solvents into the fixed bed reactor. The feed pump 7 is equipped with a mass flow meter to detect the flow rate value in order to accurately control the amount of material conveyed in the pipeline.
[0085] In this embodiment, a raw material filter 5 is provided between the liquid raw material storage tank 1 and the feed pump 7. The raw material filter 5 is used to remove solid impurities from the raw material.
[0086] In this embodiment, the outlet of the raw material filter 5 and the outlet of the solvent storage tank 2 are connected to the inlet of the feed pump 7 via a three-way valve.
[0087] In this embodiment, a gas mass flow meter 6 is provided between the gas storage tank and the reaction module to detect and control the amount of gas flowing out; the gas storage tank includes a high-pressure nitrogen cylinder 3 and a high-pressure hydrogen cylinder 4; both the high-pressure nitrogen cylinder 3 and the high-pressure hydrogen cylinder 4 are connected to a pressure gauge, a pressure reducing valve and a shut-off valve to control the pressure of the flowing gas or to shut off the gas.
[0088] In this embodiment, the gas mass flow meter 6 is also equipped with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence; the signal receiving module is electrically connected to a pressure gauge located downstream of the gas mass flow meter 6, and is used to receive the pressure value of the first fixed bed reactor.
[0089] In this embodiment, the signal processing module is used to determine whether the pressure of the first fixed-bed reactor exceeds or falls below the set theoretical pressure (4MPa); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the pressure of the first fixed-bed reactor is lower than 3.8MPa or higher than 4.2MPa; the signal output locking module is connected to the solenoid valve of the gas mass flow meter 6, and is used to issue a signal and lock the outlet of the gas mass flow meter 6 when the pressure of the first fixed-bed reactor is lower than 3.5MPa or higher than 4.5MPa.
[0090] In this embodiment, the outlet of the high-pressure nitrogen cylinder 3 and the outlet of the high-pressure hydrogen cylinder 4 are connected to the inlet of the gas mass flow meter 6 through a three-way valve.
[0091] In this embodiment, the outlet of the gas mass flow meter 6 and the outlet of the preheater 8 are connected to the inlet of the first fixed-bed reactor through a three-way valve.
[0092] In this embodiment, the inner cavity of the fixed bed reactor is uniformly filled with catalyst particles with a particle size of 200-1000 μm. The gas and liquid are mixed through a three-way valve and then enter the fixed bed reactor, flowing through a gas-liquid disperser to contact the catalyst particles.
[0093] In this embodiment, a condenser 17 is provided between the gas-liquid separator 18 and the reaction module. The condenser 17 is used to cool and condense the material.
[0094] In this embodiment, a transfer pump 20 is provided between the waste liquid storage tank 22, the product collection tank 23 and the degassing tank 19. The transfer pump 20 is used for directional material conveying. The transfer pump 20 is equipped with a mass flow meter to detect the flow rate value in order to accurately control the amount of material conveyed in the pipeline.
[0095] In this embodiment, a product filter 21 is provided between the product collection tank 23 and the transfer pump 20. The product filter 21 is used to remove solid impurities from the material flowing out of the fixed bed reactor.
[0096] In this embodiment, the outlet of the product filter 21 is connected to the inlet of the waste liquid storage tank 22 and the inlet of the product collection tank 23 via a three-way valve.
[0097] In this embodiment, the reaction module includes a first fixed-bed reactor 9, a second fixed-bed reactor 10, a third fixed-bed reactor 11, and a fourth fixed-bed reactor 12. Each fixed-bed reactor is equipped with a first gas-liquid disperser 13, a second gas-liquid disperser 14, a third gas-liquid disperser 15, and a fourth gas-liquid disperser 16.
[0098] In this embodiment, the gas-liquid separator 18 includes an adjustable back pressure valve, a level gauge, and a vacuum pressure valve. The adjustable back pressure valve, level gauge, and vacuum pressure valve cooperate with each other to adjust the liquid level of the gas-liquid separator 18. The gas-liquid separator 18 is also provided with a control interlock device, which includes a signal receiving module, a signal processing module, and a signal output locking module connected in sequence. The signal receiving module is electrically connected to the level gauge and is used to receive the liquid level value of the solution in the gas-liquid separator 18.
[0099] In this embodiment, the pressure of the adjustable back pressure valve is 0.1 to 5 MPa.
[0100] In this embodiment, the liquid level in the level gauge reaches 5% to 50% of the volume of the gas-liquid separator 18.
[0101] In this embodiment, the signal processing module is used to determine whether the liquid level of the solution in the gas-liquid separator 18 exceeds or falls below the set theoretical liquid level (20%); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the liquid level of the solution in the gas-liquid separator 18 is lower than 15% or higher than 25%; the signal output locking module is connected to the vacuum pressure valve, and is used to issue a signal and lock the outlet of the gas-liquid separator 18 when the liquid level of the solution in the gas-liquid separator 18 is lower than 10% or higher than 30%.
[0102] In this embodiment, the degassing tank 19 includes a level gauge and a vacuum pressure valve. The level gauge and the vacuum pressure valve cooperate to adjust the liquid level of the degassing tank 19. The degassing tank 19 is also provided with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence. The signal receiving module is electrically connected to the level gauge and is used to receive the liquid level value of the solution in the degassing tank 19.
[0103] In this embodiment, the liquid level in the level gauge reaches 1% to 50% of the volume of the degassing tank 19.
[0104] In this embodiment, the signal processing module is used to determine whether the liquid level of the solution in the degassing tank 19 exceeds or falls below the set theoretical liquid level (20%); the signal output locking module is electrically connected to the alarm module, and is used to control the alarm module to issue an audible and visual alarm when the liquid level of the solution in the degassing tank 19 is lower than 15% or higher than 25%; the signal output locking module is connected to the vacuum pressure valve, and is used to issue a signal and lock the outlet of the degassing tank 19 when the liquid level of the solution in the degassing tank 19 is lower than 10% or higher than 30%.
[0105] The workflow of the continuous hydrogenation reaction system in this embodiment is as follows:
[0106] This embodiment uses a continuous hydrogenation reaction system to produce compound B from substrate A. The specific chemical reaction formula is shown below.
[0107]
[0108] Liquid raw material storage tank 1 contains a mixed solution of isopropanol / methyl tert-butyl ether containing substrate A, solvent storage tank 2 contains a mixed solvent of isopropanol / methyl tert-butyl ether, and high-pressure nitrogen cylinder 3 and high-pressure hydrogen cylinder 4 are connected in parallel to gas mass flow meter 6.
[0109] Each fixed-bed reactor is filled with 300g of glass beads at the bottom, followed by 500g of Pd / C catalyst on the glass beads; shut-off valves 101, 103, 105, 102, 104, 106, 108, 113, and 114 are closed, and shut-off valves 109, 110, 111, 107, 112, and 115 are opened. Nitrogen gas from high-pressure nitrogen cylinder 3 flows sequentially through the first fixed-bed reactor 9, the second fixed-bed reactor 10, the third fixed-bed reactor 11, and the fourth fixed-bed reactor 12 at a flow rate of 50NL / min to inert the catalyst.
[0110] Close shut-off valves 109 and 112, and open shut-off valves 102 and 113; the isopropanol / methyl tert-butyl ether solution in solvent storage tank 2 is transported to the first fixed-bed reactor 9 at a flow rate of 1045 mL / min; the liquid level gauge of degassing tank 19 is set to 20%; the transfer pump 20 is turned on to transport the rinsing liquid in degassing tank 19 to waste liquid storage tank 22 at a flow rate of 1045 mL / min; once no obvious black solid powder is seen to have been flushed out of the rinsing liquid, the pretreatment of the catalyst in the first fixed-bed reactor 9 is considered complete;
[0111] Close shut-off valves 102 and 110, and open shut-off valves 101 and 104; the isopropanol / methyl tert-butyl ether solution in solvent storage tank 2 is transported to the second fixed-bed reactor 10 at a flow rate of 1045 mL / min; the level gauge of degassing tank 19 is set to 20%; the transfer pump 20 is turned on to transport the rinsing liquid in degassing tank 19 to waste liquid storage tank 22 at a flow rate of 1045 mL / min; once no obvious black solid powder is seen to have been flushed out of the rinsing liquid, the pretreatment of the catalyst in the second fixed-bed reactor 10 is considered complete;
[0112] Close shut-off valves 104 and 111, and open shut-off valves 103 and 106; the isopropanol / methyl tert-butyl ether solution in solvent storage tank 2 is transported to the third fixed-bed reactor 11 at a flow rate of 1045 mL / min; the level gauge of degassing tank 19 is set to 20%; the transfer pump 20 is turned on to transport the rinsing liquid in degassing tank 19 to waste liquid storage tank 22 at a flow rate of 1045 mL / min; once no obvious black solid powder is seen to have been flushed out of the rinsing liquid, the pretreatment of the catalyst in the third fixed-bed reactor 11 is considered complete;
[0113] Close shut-off valve 106 and open shut-off valves 105 and 108; the isopropanol / methyl tert-butyl ether solution in solvent storage tank 2 is transported to the fourth fixed-bed reactor 12 at a flow rate of 1045 mL / min; the liquid level of the level gauge of degassing tank 19 is set to 20%; the transfer pump 20 is turned on to transport the rinsing liquid in degassing tank 19 to waste liquid storage tank 22 at a flow rate of 1045 mL / min; once no obvious black solid powder is seen to have been flushed out in the rinsing liquid, the pretreatment of the catalyst in the fourth fixed-bed reactor 12 is considered complete.
[0114] After the catalyst pretreatment in all fixed-bed reactors is completed, shut-off valves 101, 103, 105, 102, 104, 106, 108, 113, and 114 are closed, and shut-off valves 109, 110, 111, 107, 112, and 115 are opened; the isopropanol / methyl tert-butyl ether solution in solvent storage tank 2 is sequentially delivered to the first, second, third, and fourth fixed-bed reactors at a flow rate of 1045 mL / min.
[0115] Adjust the pressure of the back pressure valve 19 of the gas-liquid separator 18 to 1.0 MPa; adjust the set liquid level of the liquid level gauge of the gas-liquid separator 18 to 20%;
[0116] High-pressure nitrogen cylinder 3 is switched to hydrogen cylinder 4 and flows sequentially through the first fixed-bed reactor 9, the second fixed-bed reactor 10, the third fixed-bed reactor 11, and the fourth fixed-bed reactor 12 at a flow rate of 50 NL / min.
[0117] Adjust the temperatures of the first fixed-bed reactor 9, the second fixed-bed reactor 10, the third fixed-bed reactor 11, and the fourth fixed-bed reactor 12 to 45–75°C;
[0118] After the system pressure of the first fixed-bed reactor 9, the second fixed-bed reactor 10, the third fixed-bed reactor 11, and the fourth fixed-bed reactor 12 stabilizes, the solvent storage tank 2 is switched to the liquid raw material storage tank 1 and the raw material is sequentially transported to the first, second, third, and fourth fixed-bed reactors at a flow rate of 1045 mL / min; the shut-off valve 115 is closed and the shut-off valve 114 is opened.
[0119] The central control results determine whether to adjust the liquid flow rate and gas flow rate; if one or more fixed-bed reactors become blocked during operation, the blocked fixed-bed reactor should be shorted by using the parallel pipeline between the fixed-bed reactors.
[0120] The production capacity of this embodiment is 300 kg / day. During operation, no blockage occurred in the fixed-bed reactor. The yield of product compound B is 95%, and the purity of product compound B is >95%.
[0121] Comparative Example 1
[0122] Parallel pipelines between the fixed-bed reactors were not installed; other settings were the same as in Example 1.
[0123] This comparative example cannot perform separate pretreatment of the catalyst. Because the catalyst particles in the fixed-bed reactor are small, when the catalyst is pretreated, the catalyst and its debris from the previous fixed-bed reactor are easily carried into the next fixed-bed reactor with the solution. This causes the catalyst and its debris to accumulate continuously in the fixed-bed reactor, resulting in a slow and continuous increase in the pressure drop during operation, until the fixed-bed reactor is blocked.
[0124] However, once blockage occurs, it is impossible to short-circuit one or a few fixed-bed reactors. All fixed-bed reactors need to be treated as a whole. This not only has a long treatment cycle and high safety risks, but also reduces the effective utilization rate of the catalyst by 10% to 30%, resulting in serious waste of the catalyst. In addition, there is a large loss of residual material in the fixed-bed reactors and pipelines. Generally, a blockage will result in a loss of about 2 to 5% of the material, and the yield of product compound B will decrease by 2 to 5% year-on-year.
Claims
1. A continuous hydrogenation reaction system, characterized in that, The continuous hydrogenation reaction system includes a feeding module, an inlet module, a reaction module, a separation module, and a collection module; wherein, The feeding module includes a liquid raw material storage tank and a solvent storage tank; The air intake module includes a gas storage tank; The reaction module includes N fixed-bed reactors, where N is a positive integer greater than or equal to 2. Each fixed-bed reactor is equipped with an inlet, an outlet, and a gas-liquid disperser. The outlet of one fixed-bed reactor is connected to the inlet of the next fixed-bed reactor. The inlet of each fixed-bed reactor is also connected to the gas outlet of the gas storage tank, the discharge outlet of the liquid raw material storage tank, and the discharge outlet of the solvent storage tank via feed pipelines. The feed pipelines are divided into a main feed pipe and feed branch pipes connected to the main feed pipe and connected in parallel. Each feed branch pipe is connected to one of the fixed-bed reactors. The separation module includes a gas-liquid separator and a degassing tank; the inlet of the gas-liquid separator is connected to the outlet of the last fixed-bed reactor; the outlet of each fixed-bed reactor is also connected to the degassing tank through a discharge pipeline; the discharge pipeline is divided into a main discharge pipe and parallel discharge branch pipes connected to the main discharge pipe; each discharge branch pipe is connected to one of the fixed-bed reactors; the outlet of the gas-liquid separator is also connected to the inlet of the degassing tank; The collection module includes a waste liquid storage tank and a product collection tank; the inlets of the waste liquid storage tank and the product collection tank are respectively connected to the outlet of the degassing tank.
2. The continuous hydrogenation reaction system as described in claim 1, characterized in that, A first valve is provided on the feed manifold between each two fixed-bed reactors; Each of the aforementioned discharge branch pipes is equipped with a second valve; A third valve is provided on the connecting pipeline between the outlet of each of the fixed-bed reactors and the inlet of the next fixed-bed reactor, and the third valve is located downstream of the first valve; The opening and closing of the first valve, the second valve, and the third valve are all used to coordinate and control the parallel and series flow of materials between the fixed-bed reactors.
3. The continuous hydrogenation reaction system as described in claim 1, characterized in that, A preheater is provided between the liquid raw material storage tank, the solvent storage tank and the reaction module, and the preheater is used to heat the raw materials and solvent.
4. The continuous hydrogenation reaction system as described in claim 3, characterized in that, A feed pump is provided between the liquid raw material storage tank, the solvent storage tank and the preheater. The feed pump is used to pump the raw materials and solvent into the fixed bed reactor. The feed pump is equipped with a mass flow meter to detect the flow rate and accurately control the amount of material conveyed in the pipeline.
5. The continuous hydrogenation reaction system as described in claim 4, characterized in that, A raw material filter is provided between the liquid raw material storage tank and the feed pump, and the raw material filter is used to remove solid impurities from the raw material.
6. The continuous hydrogenation reaction system as described in claim 1, characterized in that, A gas mass flow meter is installed on the feed main pipe between the gas storage tank and the reaction module to detect and control the amount of gas flowing out. The gas storage tank includes a high-pressure nitrogen cylinder and a high-pressure hydrogen cylinder; both the high-pressure nitrogen cylinder and the high-pressure hydrogen cylinder are connected to a pressure gauge, a pressure reducing valve and a shut-off valve, which are used to control the pressure of the outflowing gas or to shut off the gas. The gas mass flow meter is also equipped with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence; the signal receiving module is electrically connected to a pressure gauge located downstream of the gas mass flow meter, and is used to receive the pressure value of the first fixed bed reactor.
7. The continuous hydrogenation reaction system as described in claim 1, characterized in that, A condenser is provided between the gas-liquid separator and the reaction module, and the condenser is used to cool and condense the material. The gas-liquid separator includes an adjustable back pressure valve, a level gauge, and a vacuum pressure valve. The gas-liquid separator is also equipped with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence; the signal receiving module is electrically connected to the liquid level gauge and is used to receive the liquid level value of the solution in the gas-liquid separator.
8. The continuous hydrogenation reaction system as described in claim 1, characterized in that, A transfer pump is provided between the waste liquid storage tank, the product collection tank and the degassing tank. The transfer pump is used for directional material conveying. The transfer pump is equipped with a mass flow meter to detect the flow rate and accurately control the amount of material conveyed in the pipeline. The degassing tank includes a level gauge and a vacuum pressure valve; The degassing tank is also equipped with a control interlock device, which includes a signal receiving module, a signal processing module and a signal output locking module connected in sequence; the signal receiving module is electrically connected to the level gauge and is used to receive the level value of the solution in the degassing tank.
9. The continuous hydrogenation reaction system as described in claim 8, characterized in that, A product filter is provided between the product collection tank and the transfer pump. The product filter is used to remove solid impurities from the material flowing out of the fixed bed reactor.
10. The continuous hydrogenation reaction system as described in claim 1, characterized in that, The reaction module includes 2 to 8 fixed-bed reactors.