Efficient tower type continuous hydrogenation reaction system

Abstract

The utility model discloses a high-efficiency tower type continuous hydrogenation reaction system which comprises a gas-liquid-solid three-phase separation module, a reaction module I, a reaction module II and a discharging module which are sequentially communicated with one another from top to bottom, and is characterized in that two hydrogenation reactors, a catalyst filtering and recycling device and a reaction tail gas condensing device are integrated into a tower reaction system; and the pipeline design of the hydrogenation system is reduced, the air tightness of the reaction system is enhanced, and the possibility of hydrogen leakage is reduced, so that the risk of the hydrogenation reaction is reduced, and the continuous operation of the hydrogenation reaction is realized.

Description

Technical Field

[0001] The utility model relates to the technical field of hydrogenation reaction equipment, in particular to a high-efficiency tower-type continuous hydrogenation reaction system. Background Art

[0002] As domestic safety supervision requirements become increasingly stringent and competition in the fine chemical industry becomes increasingly fierce, production companies are being pushed to accelerate innovation. A large number of hydrogenation reactions are common in the field of fine chemicals (including API synthesis). Hydrogenation reactions are generally highly exothermic reactions, and over-temperature and over-pressure phenomena are prone to occur during the reaction process. In addition, the explosion limit range of hydrogen is wide, which is very prone to accidents, and there are high requirements for the airtightness of the reaction system.

[0003] At present, the mainstream hydrogenation reaction still adopts the kettle process. Although the degree of automation of the reactor is greatly improved compared with the past, the kettle reaction is still mainly an intermittent process, which involves a lot of manual operation and the risk of personal injury caused by fire and explosion. There are frequent switching operations, which bring potential safety hazards. At the same time, the kettle intermittent hydrogenation process has intermittent operations such as cyclic heating and cooling, which bring unnecessary energy loss. Finally, the kettle intermittent hydrogenation operation has many non-production links such as replacement and cleaning, which makes it impossible to improve production efficiency. In order to increase production capacity, only additional reactors can be added, which brings greater safety hazards.

[0004] This kind of production status is the pain point of the entire industry. Therefore, in order to solve the above problems, improve the production efficiency, production capacity, safety, and environmental protection level of production enterprises, and promote the development of the fine chemical industry, the utility model proposes a novel tower continuous hydrogenation system to change the traditional production mode. Utility Model Content

[0005] In view of the problems existing in the prior art, the purpose of the utility model is to provide a high-efficiency tower-type continuous hydrogenation reaction system, aiming to improve the yield of the hydrogenation reaction, while enhancing the automation and integration of the hydrogenation reaction, thereby achieving the continuity and safety of the hydrogenation reaction.

[0006] The technical solution of the utility model is as follows:

[0007] A high-efficiency tower-type continuous hydrogenation reaction system comprises a gas-liquid-solid three-phase separation module, a reaction module 1, a reaction module 2 and a discharge module which are interconnected from top to bottom, wherein the gas-liquid-solid three-phase separation module comprises a gas phase condenser, and a gas phase space and a solid-liquid separation space are provided inside a head at one end of the gas phase condenser;

[0008] The reaction module 1 includes a hydrogenation reactor 1, a circulation pump 1, a heat exchanger 1 and a venturi ejector 1, the hydrogenation reactor 1 is connected to the gas phase condenser through a flange, a feed pipe is provided on one side of the hydrogenation reactor, wherein the liquid outlet on one side of the hydrogenation reactor is connected to the circulation pump 1, the heat exchanger 1, the venturi ejector 1 and the material inlet on one side of the hydrogenation reactor through a pipeline, wherein the gas outlet on the side of the gas phase space is connected to the venturi ejector 1 and the material inlet on one side of the hydrogenation reactor through a pipeline;

[0009] The discharging module comprises a discharging tower and a discharging pump, and the material outlet at the bottom of the discharging tower is connected with the discharging pump and the solid-liquid separation space through a pipeline.

[0010] Furthermore, a catalyst recovery device is provided between the solid-liquid separation space and the gas phase space.

[0011] Furthermore, the reaction module 2 includes a hydrogenation reactor 2, a circulation pump 2, a heat exchanger 2 and a venturi ejector 2, and the liquid outlet on the side of the hydrogenation reactor 2 is connected to the circulation pump 2, the heat exchanger 2, the venturi ejector 2 and the material inlet on the side of the hydrogenation reactor 2 through a pipeline.

[0012] Furthermore, the gas outlet on the side of the second hydrogenation reactor is connected to the second venturi injector and the material inlet on the side of the second hydrogenation reactor through a pipeline.

[0013] Furthermore, the second hydrogenation reactor is provided with a second jacket system; wherein a second standby circulation pump is provided between the liquid outlet on the side of the second hydrogenation reactor and the second heat exchanger.

[0014] Furthermore, the hydrogenation reactor is provided with a jacket system; wherein a standby circulation pump is provided between a liquid outlet on one side of the hydrogenation reactor and a heat exchanger.

[0015] Furthermore, a spare discharge pump is provided between the material outlet at the bottom of the discharge tower and the solid-liquid separation space; a jacket system three is provided on the outside of the discharge tower, and the jacket system three can pass both refrigerant and heat medium, and the refrigerant used in the jacket system three is circulating water, low-temperature water or chilled ethylene glycol.

[0016] Furthermore, a tail gas outlet is provided at the top of the gas phase condenser, and a material outlet is provided at the side of the solid-liquid separation space.

[0017] Furthermore, the refrigerant used in the jacket system 1 is one or more of circulating water, low-temperature water, and refrigerated ethylene glycol; the refrigerant used in the gas phase condenser is circulating water, low-temperature water, or refrigerated ethylene glycol.

[0018] Furthermore, the refrigerant used in the jacket system 2 is one or more of circulating water, low-temperature water, and refrigerated ethylene glycol.

[0019] Furthermore, low temperature water refers to 7° tap water.

[0020] Compared with the prior art, the beneficial effects of the utility model are as follows:

[0021] 1) The utility model integrates two hydrogenation reactors, a catalyst filtering and recovery device, and a reaction tail gas condensing device into a tower reaction system, which reduces the piping design of the hydrogenation system, enhances the air tightness of the reaction system, reduces the possibility of hydrogen leakage, thereby reducing the risk of hydrogenation reaction and realizing continuous operation of hydrogenation reaction;

[0022] 2) The utility model enhances the heat transfer and mass transfer capacity during the reaction process by means of external circulation, separates the reaction liquid from the catalyst by the sedimentation process, and realizes the continuous application of the catalyst, thereby realizing the continuity of the reaction, increasing production capacity and reducing risks;

[0023] 3) Compared with the traditional kettle reaction system, the reaction system of the utility model solves the problems of over-temperature and over-pressure of the reaction system caused by large reaction exotherm, fast reaction rate and slow heat exchange of the reactor jacket, as well as the risk of misoperation and leakage caused by frequent inerting, catalyst discharging and catalyst recovery, thereby reducing the reaction risk. At the same time, the public engineering medium of each module can be selected according to the reaction system and reaction operating conditions, thereby improving the adaptability of the device. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the overall structure of the utility model system.

[0025] In the figure: 1. gas-liquid-solid three-phase separation module; 1a. gas phase condenser; 1b. gas phase space; 1c. solid-liquid separation space; 1d. catalyst recovery device; 2. reaction module one; 2a. hydrogenation reactor one; 2b. circulation pump one; 2c. heat exchanger one; 2d. venturi ejector one; 2e. jacket system one; 2f. spare circulation pump one; 3. reaction module two; 3a. hydrogenation reactor two; 3b. circulation pump two; 3c. heat exchanger two; 3d. venturi ejector two; 3e. jacket system two; 3f. spare circulation pump two; 4. discharge module; 4a. discharge tower; 4b. discharge pump; 4c. spare discharge pump; 4d. jacket system three. DETAILED DESCRIPTION

[0026] The present invention will be further described below in conjunction with the accompanying drawings and embodiments, but the scope of protection of the present invention is not limited to the described scope.

[0027] like Figure 1 As shown, a high-efficiency tower-type continuous hydrogenation reaction system comprises a gas-liquid-solid three-phase separation module 1, a reaction module 1 2, a reaction module 2 3 and a discharge module 4 which are interconnected from top to bottom.

[0028] The gas-liquid-solid three-phase separation module 1 includes a gas phase condenser 1a. A gas phase space 1b and a solid-liquid separation space 1c are arranged inside the head at one end of the gas phase condenser 1a. A catalyst recovery device 1d is arranged between the solid-liquid separation space 1c and the gas phase space 1b. Through the sedimentation process, the material passes through the catalyst recovery device 1d, thereby realizing the separation of the reaction liquid and the catalyst and realizing the continuous application of the catalyst.

[0029] In this embodiment, the refrigerant used by the gas phase condenser 1a is circulating water, low-temperature water or refrigerated ethylene glycol.

[0030] Reaction module 2 includes a hydrogenation reactor 2a, a circulation pump 2b, a heat exchanger 2c and a venturi ejector 2d. The hydrogenation reactor 2a is connected to the gas phase condenser 1a through a flange. A feed pipe is provided on the side of the hydrogenation reactor 2a, wherein the liquid outlet on the side of the hydrogenation reactor 2a is connected to the circulation pump 2b, the heat exchanger 2c, the venturi ejector 2d and the material inlet on the side of the hydrogenation reactor 2a through a pipeline, wherein the gas outlet on the side of the gas phase space 1b is connected to the venturi ejector 2d and the material inlet on the side of the hydrogenation reactor 2a through a pipeline.

[0031] A jacket system 2e is provided outside the hydrogenation reactor 2a; a spare circulation pump 2f is provided between the liquid outlet on the side of the hydrogenation reactor 2a and the heat exchanger 2c. In this embodiment, the refrigerant used in the jacket system 2e is one or more of circulating water, low-temperature water, and refrigerated ethylene glycol. The refrigerant is selected according to the reaction characteristics.

[0032] The discharging module 4 comprises a discharging tower 4a and a discharging pump 4b. The material outlet at the bottom of the discharging tower 4a is connected to the discharging pump 4b and the solid-liquid separation space 1c through a pipeline.

[0033] A spare discharge pump 4c is provided between the material outlet at the bottom of the discharge tower 4a and the solid-liquid separation space 1c; a jacket system three 4d is provided on the outside of the discharge tower 4a, and the jacket system three can pass both refrigerant and heat medium, and the refrigerant used by the jacket system three is circulating water, low-temperature water or refrigerated ethylene glycol.

[0034] The reaction module 2 3 includes a hydrogenation reactor 2 3a, a circulation pump 2 3b, a heat exchanger 2 3c and a venturi ejector 2 3d. The liquid outlet on the side of the hydrogenation reactor 2 3a is connected to the circulation pump 2 3b, the heat exchanger 2 3c, the venturi ejector 2 3d and the material inlet on the side of the hydrogenation reactor 2 3a through a pipeline.

[0035] The gas outlet at the side of the hydrogenation reactor 2 3a is connected to the venturi ejector 2 3d and the material inlet at the side of the hydrogenation reactor 2 3a through a pipeline.

[0036] A jacket system 2 3e is provided outside the hydrogenation reactor 2 3a, wherein a spare circulation pump 2 3f is provided between the liquid outlet of the side of the hydrogenation reactor 2 3a and the heat exchanger 2 3c. The refrigerant used in the jacket system 2 3e is one or more of circulating water, low-temperature water, and refrigerated ethylene glycol.

[0037] A tail gas outlet is provided at the top of the gas phase condenser 1a, and a material outlet is provided at the side of the solid-liquid separation space 1c.

[0038] In this embodiment, the gas phase condenser 1a is connected to the hydrogenation reactor 1 2a through a flange, the hydrogenation reactor 1 2a is connected to the hydrogenation reactor 2 3a through a flange, and the hydrogenation reactor 2 3a is connected to the discharge tower 4a through a flange.

[0039] In the present invention, low temperature water refers to 7° tap water.

[0040] The process of hydrogenation reaction using the utility model system is as follows:

[0041] 1) The reaction raw materials enter the tower through the top of the reaction module-2, and the hydrogen enters the tower through the bottom of the discharge module 4. The liquid moves downward and the gas moves upward. The gas and liquid contact in the reaction module-2 to carry out the hydrogenation reaction. The reaction liquid is pressurized by the circulation pump-2b, cooled by the heat exchanger-2c, and mixed with the hydrogen return pipeline in the gas phase space 1b through the venturi ejector-2d before entering the reaction module-2; the combination of the heat exchanger-2c and the jacket system-2e can increase the heat exchange area to meet the characteristics of the large heat release of the hydrogenation reaction. At the same time, after the hydrogen return pipeline and the liquid phase return pipeline pass through the venturi ejector-2d, the solubility of hydrogen in the liquid is enhanced to improve the reaction efficiency;

[0042] 2) The reaction liquid enters the reaction module 2 3 through the reaction module 1 2, and the reaction liquid is pressurized by the circulation pump 2 3a, and then cooled by the heat exchanger 2 3c, and then mixed with the hydrogen return pipeline of the reaction module 2 3 through the venturi injector 2 3d, and then enters the reaction module 2 3; the combination of the heat exchanger 2 3c and the jacket system 2 3e can increase the heat exchange area to meet the characteristics of the large heat release of the hydrogenation reaction. At the same time, after the hydrogen return pipeline and the liquid phase return pipeline pass through the venturi injector 2 3d, the solubility of hydrogen in the liquid is enhanced to improve the reaction efficiency;

[0043] 3) The reaction liquid enters the discharge module 4 through the reaction module 2 3, and is transported to the solid-liquid separation space 1c through the discharge pump 4b. At the rear end of the reaction, the heat release is small, so the jacket system 3 4c is set to ensure the discharge temperature;

[0044] 4) The reaction liquid is in the solid-liquid separation space 1c, the gas phase is condensed by the gas phase condenser 1a and then discharged from the system, the liquid phase is filtered to intercept the solid catalyst, the liquid is discharged from the tower, and the catalyst sinks to the reaction module 2 for repeated use.

[0045] The raw material for the hydrogenation reaction in step 1) is any API, pesticide, flavor or intermediate; the catalyst is palladium, platinum or rhodium; and the solvent is methanol, isopropanol or toluene. Example 1

[0046] The reaction system of the utility model was used to test the hydrogenation reaction in the production process of dydrogesterone. The hydrogenation reaction solvent was methanol and the catalyst was palladium carbon. In the reactor operation, 40 kg of palladium carbon was used per batch, the catalyst recovery rate was 60%, and the reaction yield was 96%. In the tower hydrogenation reaction, the catalyst was recycled, the loss was about 5%, and the reaction yield was 98%. Example 2

[0047] The reaction system of the utility model was used to test the hydrogenation reaction in the production process of aprepitant. The solvent of the hydrogenation reaction was tetrahydrofuran and the catalyst was palladium carbon. In the reactor operation, 5 kg of palladium carbon was used per batch, the catalyst recovery rate was 40%, and the reaction yield was 94%. In the tower hydrogenation reaction, the catalyst was recycled, the loss was about 5%, and the yield was 97%. Example 3

[0048] The reaction system of the utility model was used to test the hydrogenation reaction in the production process of lubiprostone. The solvent of the hydrogenation reaction was ethyl acetate and the catalyst was palladium carbon. In the reactor operation, 1 kg of palladium carbon was used per batch, the catalyst recovery rate was 0%, and the reaction yield was 95%. In the tower hydrogenation reaction, the catalyst was recycled, the loss was about 2%, and the yield was 98%.

Claims

1. A high-efficiency tower-type continuous hydrogenation reaction system, comprising a gas-liquid-solid three-phase separation module (1), a reaction module 1 (2), a reaction module 2 (3) and a discharge module (4) which are interconnected from top to bottom, characterized in that The gas-liquid-solid three-phase separation module (1) comprises a gas phase condenser (1a), wherein a gas phase space (1b) and a solid-liquid separation space (1c) are provided inside a head at one end of the gas phase condenser (1a); The reaction module 1 (2) comprises a hydrogenation reactor 1 (2a), a circulation pump 1 (2b), a heat exchanger 1 (2c) and a venturi ejector 1 (2d); the hydrogenation reactor 1 (2a) is connected to the gas phase condenser (1a) via a flange; a feed pipe is provided on the side of the hydrogenation reactor 1 (2a); a liquid outlet on the side of the hydrogenation reactor 1 (2a) is connected to the material inlet on the side of the circulation pump 1 (2b), the heat exchanger 1 (2c), the venturi ejector 1 (2d) and the hydrogenation reactor 1 (2a) via a pipeline; a gas outlet on the side of the gas phase space (1b) is connected to the material inlet on the side of the venturi ejector 1 (2d) and the hydrogenation reactor 1 (2a) via a pipeline; The discharge module (4) comprises a discharge tower (4a) and a discharge pump (4b), and a material outlet at the bottom of the discharge tower (4a) is connected to the discharge pump (4b) and the solid-liquid separation space (1c) via a pipeline.

2. A high-efficiency tower-type continuous hydrogenation reaction system according to claim 1, characterized in that A catalyst recovery device (1d) is provided between the solid-liquid separation space (1c) and the gas phase space (1b).

3. A high-efficiency tower-type continuous hydrogenation reaction system according to claim 1, characterized in that The reaction module 2 (3) comprises a hydrogenation reactor 2 (3a), a circulation pump 2 (3b), a heat exchanger 2 (3c) and a venturi ejector 2 (3d); the liquid outlet on the side of the hydrogenation reactor 2 (3a) is connected to the circulation pump 2 (3b), the heat exchanger 2 (3c), the venturi ejector 2 (3d) and the material inlet on the side of the hydrogenation reactor 2 (3a) through a pipeline.

4. A high-efficiency tower-type continuous hydrogenation reaction system according to claim 3, characterized in that The gas outlet at the side of the hydrogenation reactor 2 (3a) is connected to the venturi ejector 2 (3d) and the material inlet at the side of the hydrogenation reactor 2 (3a) through a pipeline.

5. A high-efficiency tower-type continuous hydrogenation reaction system according to claim 3, characterized in that The second hydrogenation reactor (3a) is provided with a jacket system (3e) outside; wherein a second standby circulation pump (3f) is provided between the liquid outlet on the side of the second hydrogenation reactor (3a) and the second heat exchanger (3c).

6. A high-efficiency tower-type continuous hydrogenation reaction system according to claim 1, characterized in that The hydrogenation reactor 1 (2a) is provided with a jacket system 1 (2e) outside; wherein a standby circulation pump 1 (2f) is provided between the liquid outlet on the side of the hydrogenation reactor 1 (2a) and the heat exchanger 1 (2c).

7. The high-efficiency tower-type continuous hydrogenation reaction system according to claim 1, characterized in that A spare discharge pump (4c) is provided between the material outlet at the bottom of the discharge tower (4a) and the solid-liquid separation space (1c); wherein a jacket system three (4d) is provided outside the discharge tower (4a), and the refrigerant used in the jacket system three (4d) is circulating water or refrigerated ethylene glycol.

8. The high-efficiency tower-type continuous hydrogenation reaction system according to claim 1, characterized in that The gas phase condenser (1a) is provided with an exhaust gas outlet at the top, and a material outlet is provided at the side of the solid-liquid separation space (1c).

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