Continuous hydrogenation device and process
By adopting an S-shaped flow channel and a multi-stage microreactor structure in the continuous hydrogenation unit, the problem of insufficient gas-liquid mixing was solved, the reaction conversion rate and product purity were improved, the separation process was simplified, and safety risks and production costs were reduced.
Patent Information
- Application Number
- CN202511613714.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-06
- Publication Date
- 2025-12-16
AI Technical Summary
In existing continuous hydrogenation units, insufficient gas-liquid mixing and small catalyst contact area result in low reaction conversion rates and cumbersome separation processes, making it difficult to achieve continuous production.
A continuous hydrogenation unit is designed, which uses concentrically distributed septa to form an S-shaped flow channel to increase the contact area between the feedstock and the catalyst. It also incorporates multi-stage microreactors and catalyst coatings, and uses a DCS control system to monitor and adjust reaction parameters in real time to ensure safety.
It improved the reaction conversion rate, enhanced product purity, simplified the separation process, reduced the probability of safety accidents, extended the catalyst lifespan, and reduced production costs.
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Figure CN121130752A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical reaction technology, specifically to a continuous hydrogenation apparatus and process. Background Technology
[0002] Pre-hydrogenation reactions are mainly divided into batch and continuous types. Continuous types mainly include multi-reactor series continuous hydrogenation units and single-reactor internal circulation continuous hydrogenation units. Both types of continuous hydrogenation units have achieved continuous hydrogenation reaction, but the products generally contain catalyst powder, which requires further separation and purification. Moreover, the separation process is cumbersome and it is not easy to achieve continuous production.
[0003] A continuous hydrogenation reactor and reaction process are disclosed in CN110756120A. The reactor includes a high-pressure reactor, a heat exchanger, and a membrane module. During the reaction, the substrate, hydrogen, and powdered catalyst react in the high-pressure reactor. The reaction solution is then transported to the membrane module via the heat exchanger. The membrane module performs high-precision filtration and separation of the product and catalyst in the solution. The separated catalyst is then returned to the reactor for continued use.
[0004] The traditional hydrogenation reactor has an unreasonable internal structure design, resulting in insufficient gas-liquid mixing, small contact area and short contact time between raw materials and catalyst, leading to low reaction conversion rate. Summary of the Invention
[0005] (a) Technical problems to be solved The purpose of this invention is to provide a continuous hydrogenation apparatus and process to solve the above-mentioned problems.
[0006] (II) Technical Solution To achieve the above objectives, the present invention provides the following technical solution: The present invention provides a continuous hydrogenation apparatus, comprising a gas supply system, a liquid supply system, a heating system, a hydrogenation reactor, a gas-liquid mixing distributor, a cooling system, a gas-liquid separation system, and a product collection system; The gas supply system and the liquid supply system are respectively connected to the inlet of the gas-liquid mixing distributor through pipelines, and the outlet of the gas-liquid mixing distributor is connected to the inlet of the reactor through a pipeline; The heating system is located between the liquid supply system and the gas-liquid mixing distributor, and is used to preheat the raw material liquid; The cooling system is a condenser, and the outlet of the hydrogenation reactor is connected to the inlet of the condenser via a pipeline; The gas-liquid separation system includes a gas-liquid separation tank and a second buffer tank. The outlet of the condenser is connected to the inlet of the gas-liquid separation tank through a pipeline, and the gas phase outlet of the gas-liquid separation tank is connected to the inlet of the second buffer tank through a pipeline. The product collection system includes a back pressure valve and a product collection tank. The back pressure valve is located at the gas phase outlet of the second buffer tank. The liquid phase outlet of the gas-liquid separator and the liquid phase outlet of the second buffer tank are connected in sequence to the regulating valve and the product collection tank through pipelines.
[0007] Furthermore, the gas supply system includes a hydrogen supply device, a nitrogen supply device, a hydrogen mass flow meter, a nitrogen mass flow meter, and a first buffer tank. The hydrogen supply device is connected to the hydrogen mass flow meter and the first buffer tank in sequence via pipelines. The nitrogen supply device is connected to the nitrogen mass flow meter and the first buffer tank in sequence via pipelines. The outlet of the first buffer tank is connected to the inlet of the gas-liquid mixing distributor via a pipeline.
[0008] Furthermore, the liquid supply system includes a hydrogenation feedstock supply device and a high-pressure diaphragm pump. The hydrogenation feedstock supply device is connected to the high-pressure diaphragm pump via a pipeline. The heating system is a preheater. The outlet of the high-pressure diaphragm pump is connected to the inlet of the preheater via a pipeline. The outlet of the preheater is connected to the inlet of the gas-liquid mixing distributor via a pipeline.
[0009] Furthermore, the hydrogenation reactor includes a hollow reaction vessel with openings at both the top and bottom. The upper and lower ends of the reaction vessel are respectively sealed with an upper tank cover and a lower tank cover. The upper end of the reaction vessel is provided with two first feed pipe joints, and the lower tank cover is provided with a second feed pipe joint. The reaction vessel contains a plurality of first partitions and a plurality of second partitions arranged concentrically. The first partitions and the second partitions are spaced apart from each other. An S-shaped flow channel is formed between the first partitions and the second partitions. A catalytic structure is provided in the flow channel. The lower end of the first partition is fixedly mounted on the lower tank cover, and the upper end of the second partition is fixedly mounted on the upper tank cover.
[0010] Furthermore, the reaction vessel is provided with a central channel for connecting the tail end of the flow channel and the second feed pipe joint to each other. The central channel is provided with a spiral rib, and a central shaft is fixedly provided in the middle of the spiral rib. The spiral spacing of the spiral rib is filled with a first catalyst filling layer.
[0011] Furthermore, the catalytic structure includes a first micro-reaction channel disposed within the flow channel, the inner wall of the micro-reaction channel being coated with a catalyst, and heat exchangers being disposed within both the first and second septa.
[0012] Furthermore, the catalytic structure includes a second catalyst filling layer, which fills the flow channel.
[0013] Furthermore, the catalytic structure includes a primary microreactor, a secondary microreactor, and a tertiary microreactor connected in sequence. The second microreaction channels in the primary, secondary, and tertiary microreactors are all coated with a catalyst coating, and the coarse section of the second microreaction channel is provided with a crescent-shaped baffle column.
[0014] A continuous hydrogenation process includes the following steps: S1: First, pretreatment is carried out by turning on the nitrogen supply equipment and adjusting the nitrogen flow rate through the nitrogen mass flow meter so that the nitrogen enters the pipeline and hydrogenation reactor through the first buffer tank for purging to replace the air in the pipeline. At the same time, the system pressure is adjusted to the set back pressure value through the back pressure valve. S2: Add the hydrogenation feedstock to the hydrogenation feedstock supply equipment, turn on the high-pressure diaphragm pump, and deliver the feedstock liquid to the preheater. The feedstock liquid is preheated to 30-250℃ by the electric heating module of the preheater. S3: Turn on the hydrogen supply equipment, adjust the hydrogen flow rate through the hydrogen mass flow meter, so that the hydrogen is stably output from the first buffer tank and enters the gas-liquid mixer together with the preheated raw material liquid, and is fully mixed in the distributor to form a gas-liquid mixture. S4: The gas-liquid mixture output from the gas-liquid mixer is fed into the hydrogenation reactor through the first feed pipe joint and the second feed pipe joint. The gas-liquid mixture flows through the catalytic structure and completes the hydrogenation reaction under the action of the catalyst coating. During the reaction, the reaction temperature is monitored in real time by multi-segment multi-point thermometers, which facilitates temperature adjustment. S5: The material after the hydrogenation reaction enters the condenser, and is cooled to room temperature by the cold water supplied by the cold water supply unit. Then it is sent to the gas-liquid separator, where gas-liquid separation is achieved. The liquid phase is the hydrogenation product and the gas phase is unreacted hydrogen. After the S6 gas-liquid separation, the hydrogenation product is sent to the hydrogenation product collection tank after the flow rate is controlled by the pneumatic liquid level regulating valve and the regulating valve. The unreacted hydrogen enters the second buffer tank through the gas phase outlet of the gas-liquid separator. After the pressure is stabilized by the back pressure valve, it is discharged through the high-altitude exhaust port. S7: After the reaction is complete, shut off the raw material supply, open the cleaning solution storage tank and switching valve, and use a high-pressure diaphragm pump to deliver the cleaning solution to the pipeline and hydrogenation reactor to clean the system.
[0015] Furthermore, the DCS control system collects data on hydrogen flow rate, nitrogen flow rate, raw material liquid flow rate, reaction temperature, reaction pressure, condenser outlet temperature, and gas-liquid separator level in real time, and displays them in real time through the 360 Force Control configuration software. When any of the parameters exceed the set range, the system automatically triggers an alarm and cuts off the feed of the high-pressure diaphragm pump and hydrogen supply equipment, while simultaneously starting nitrogen purging to ensure the safety of the device.
[0016] (III) Beneficial Effects Compared with the prior art, the beneficial effects of the present invention are as follows: 1. The reactor is equipped with a first and second partition sleeve arranged in concentric circles to form an S-shaped flow channel, which prolongs the residence time of materials. At the same time, it provides a variety of catalytic structures, such as micro-reaction channels with catalyst coating on the inner wall, packed catalyst layers, and multi-stage microreactors, which increase the contact area between raw materials and catalysts and improve the reaction conversion rate. Among them, crescent-shaped baffle columns are set in the coarse section of the multi-stage microreactor, which can further enhance the uniformity of gas-liquid mixing, avoid incomplete local reactions, and improve product purity. 2. By placing the second spacer on the upper tank cover and the first spacer on the lower tank cover, the catalyst structure can be easily cleaned and replaced by separating and removing the first and second spacers when disassembling the upper and lower tank covers.
[0017] By purging and replacing the air in the pipeline with nitrogen, and controlling the pressure of the system with a back pressure valve, the risk of explosive mixtures is eliminated at the source. The DCS control system collects key parameters such as pressure, temperature and flow rate in real time. When the parameters exceed the set range, an alarm is automatically triggered, the feed is cut off and nitrogen purging is started, realizing emergency protection and greatly reducing the probability of safety accidents. 4. By using multi-segment, multi-point thermometers to monitor the temperature of different areas of the reactor in real time, and in conjunction with the preheater electric heating module, the heat exchanger in the jacket or the heat transfer oil module, the reaction temperature can be precisely adjusted to avoid over-reaction; at the same time, it supports in-situ regeneration of the catalyst assisted by cleaning fluid or hydrogen, which extends the catalyst's service life and reduces production costs. Attached Figure Description
[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0019] Figure 1 This is a schematic diagram of the continuous hydrogenation process of the present invention; Figure 2 This is a schematic diagram of the structure of the reactor of the present invention in the first embodiment; Figure 3 This is a schematic diagram of the second embodiment of the reactor of the present invention; Figure 4 This is a schematic diagram of the third embodiment of the reactor of the present invention; Figure 5 This is a schematic diagram of the internal structure of the microreactor of the present invention.
[0020] The reference numerals in the attached drawings are explained as follows: 1. Hydrogen supply equipment; 2. Nitrogen supply equipment; 3. Hydrogen mass flow meter; 4. Nitrogen mass flow meter; 5. First buffer tank; 6. Hydrogen feedstock supply equipment; 7. High-pressure diaphragm pump; 8. Preheater; 9. Reactor; 901. Reaction tank body; 902. Upper tank cover; 903. Lower tank cover; 904. First feed pipe connector; 905. Second feed pipe connector; 906. Central channel; 907. Spiral rib; 908. Central shaft; 909. First catalyst packing layer; 91. 0. Flow channel; 911. First septum; 912. Second septum; 913. First microreactor channel; 914. Heat exchanger; 915. Second catalyst packing layer; 916. Primary microreactor; 917. Secondary microreactor; 918. Tertiary microreactor; 919. Coarse section channel; 920. Fine section channel; 921. Baffle column; 10. Gas-liquid mixing distributor; 11. Condenser; 12. Gas-liquid separator; 13. Second buffer tank; 14. Back pressure valve; 15. Regulating valve; 16. Product collection tank. Detailed Implementation
[0021] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be described in detail below. Obviously, the described embodiments are merely some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other implementation methods obtained by those skilled in the art without creative effort are within the scope of protection of this invention.
[0022] See Figures 1-5As shown, this invention provides a continuous hydrogenation apparatus, including a gas supply system, a liquid supply system, a heating system, a hydrogenation reactor 9, a gas-liquid mixing distributor 10, a cooling system, a gas-liquid separation system, a product collection system, and a DCS control system. The gas supply system and the liquid supply system are respectively connected to the inlet of the gas-liquid mixing distributor 10 through pipelines, and the outlet of the gas-liquid mixing distributor 10 is connected to the inlet of the reactor 9 through a pipeline. The heating system is located between the liquid supply system and the gas-liquid mixing distributor 10 for preheating the raw material liquid. The cooling system is a condenser 11, which is a coil-type condenser with a design pressure of 7 MPa. The outlet of the hydrogenation reactor 9 is connected to the inlet of the condenser 11 through a pipeline. The gas-liquid separation system includes a gas-liquid separator... The system includes a gas-liquid separator 12 and a second buffer tank 13. The gas-liquid separator 12 is designed to a pressure of 7 MPa. The outlet of the condenser 11 is connected to the inlet of the gas-liquid separator 12 via a pipeline. The gas phase outlet of the gas-liquid separator 12 is connected to the inlet of the second buffer tank 13 via a pipeline. The product collection system includes a back pressure valve 14 and a product collection tank 16. The back pressure valve 14 is located at the gas phase outlet of the second buffer tank 13 and is used to control the gas phase outlet pressure of the gas-liquid separator 12. The exhaust port of the second buffer tank 13 is designed for high-altitude discharge to release a small amount of buffered atmospheric pressure hydrogen gas. The liquid phase outlets of the gas-liquid separator 12 and the second buffer tank 13 are connected sequentially to a regulating valve 15 and a product collection tank 16 via pipelines. All pipelines used for connection are pressure-resistant, and the pressure resistance rating of the pipelines and valves is 10 MPa.
[0023] The DCS control system integrates computer technology, communication technology, graphic display technology, and control technology, and is electrically connected to hydrogen mass flow meter 3, nitrogen mass flow meter 4, high-pressure diaphragm pump 7, preheater 8, hydrogenation reactor 9, condenser 11, and regulating valve 14. The DCS control system includes Siemens PLC-S7 series controllers and Sanwei Force Control configuration software, which are used to realize the decentralized control, centralized operation, hierarchical management of the equipment, as well as the reception, processing, display, and alarm of field detection signals, and generate production records and reports.
[0024] The gas supply system includes a hydrogen supply device 1, a nitrogen supply device 2, a hydrogen mass flow meter 3, a nitrogen mass flow meter 4, and a first buffer tank 5. The hydrogen supply device 1 is connected to the hydrogen mass flow meter 3 and the first buffer tank 5 sequentially via pipelines. The nitrogen supply device 2 is connected to the nitrogen mass flow meter 4 and the first buffer tank 5 sequentially via pipelines. The outlet of the first buffer tank 5 is connected to the inlet of the gas-liquid mixing distributor 10 via a pipeline. The design pressure of both the hydrogen mass flow meter 3 and the nitrogen mass flow meter 4 is 0-10 MPa, and the design flow rate is 2000 NLPH.
[0025] The liquid supply system includes a hydrogenation feedstock supply device 6 and a high-pressure diaphragm pump 7. When the effective volume of the hydrogenation reactor 9 is 5L, the design flow rate of the high-pressure diaphragm pump 7 is 0-48L / h; when the effective volume of the hydrogenation reactor 9 is 2L, the design flow rate of the high-pressure diaphragm pump 7 is 0-24L / h, and the design pressure is 7MPa. The hydrogenation feedstock supply device 6 is connected to the high-pressure diaphragm pump 7 via a pipeline. The heating system is a preheater 8. The outlet of the high-pressure diaphragm pump 7 is connected to the inlet of the preheater 8 via a pipeline, and the outlet of the preheater 8 is connected to the inlet of the gas-liquid mixing distributor 10 via a pipeline. The preheater 8 is a pipeline-type explosion-proof preheater with an internal electric heating module, a design pressure of 7MPa, a maximum liquid flow rate of 48L / h, and a preheating temperature range of 0-260℃. The hydrogenation reactor 9 includes a hollow reaction vessel 901 with openings at both the top and bottom. The upper and lower ends of the reaction vessel 901 are respectively sealed with an upper tank cover 902 and a lower tank cover 903. The upper end of the reaction vessel 901 is provided with two first feed pipe joints 904, and the lower tank cover 903 is provided with a second feed pipe joint 905. The reaction vessel 901 is provided with a plurality of first partitions 911 and a plurality of second partitions 912 arranged in concentric circles. The first partitions 911 and the second partitions 912 are arranged at intervals. An S-shaped flow channel 910 is formed between the first partitions 911 and the second partitions 912. A catalytic structure is provided in the flow channel 910. The lower end of the first partition 911 is fixedly mounted on the lower tank cover 903, and the upper end of the second partition 912 is fixedly mounted on the upper tank cover 902.
[0026] The reaction vessel 901 is provided with a central channel 906 for connecting the tail end of the flow channel 910 and the second feed pipe joint 905. The central channel 906 is provided with a spiral rib 907. A central shaft 908 is fixedly provided in the middle of the spiral rib 907. The spiral spacing of the spiral rib 907 is filled with a first catalyst filling layer 909.
[0027] The first embodiment of the catalytic structure: The catalytic structure includes a first micro-reaction channel 913 disposed in the flow channel 910, the inner wall of the micro-reaction channel 913 is provided with a catalyst coating, and heat exchangers 914 are provided in both the first septum 911 and the second septum 912.
[0028] A second embodiment of the catalytic structure: The catalytic structure includes a second catalyst filling layer 915, which is filled in the flow channel 910.
[0029] The third embodiment of the catalytic structure: The catalytic structure includes a primary microreactor 916, a secondary microreactor 917 and a tertiary microreactor 918 connected in sequence. The second micro-reaction channels in the primary microreactor 916, the secondary microreactor 917 and the tertiary microreactor 918 are all coated with a catalyst coating. The coarse section 919 of the second micro-reaction channel is provided with a crescent-shaped baffle column 921.
[0030] The continuous hydrogenation process of this invention: First, pretreatment is performed by turning on the nitrogen supply equipment 2 and adjusting the nitrogen flow rate through the nitrogen mass flow meter 3, so that the nitrogen enters the pipeline and hydrogenation reactor 9 through the first buffer tank 5 to purge and replace the air in the pipeline. At the same time, the system pressure is adjusted to the set back pressure value through the back pressure valve. If the raw material tank or hydrogenation product collection tank 16 has a nitrogen protection requirement, the nitrogen branch pipeline can be connected to the raw material tank or product tank for sealed protection. Add the hydrogenation feedstock to the hydrogenation feedstock supply equipment 6, turn on the high-pressure diaphragm pump 7, and transport the feedstock liquid to the preheater 8. The feedstock liquid is preheated to 30-250℃ by the electric heating module of the preheater 8. Turn on the hydrogen supply device 1, adjust the hydrogen flow rate through the hydrogen mass flow meter 3, so that the hydrogen is stably output through the first buffer tank 5 and enters the gas-liquid mixing distributor 10 together with the preheated raw material liquid, and is fully mixed in the distributor to form a gas-liquid mixture. The gas-liquid mixture output from the gas-liquid mixer distributor 10 is fed into the hydrogenation reactor 9 through the first feed pipe connector 904 and the second feed pipe connector 905. The gas-liquid mixture then flows through the catalytic structure and completes the hydrogenation reaction under the action of the catalyst coating. During the reaction, the reaction temperature is monitored in real time by multi-segment, multi-point thermometers. The thermometers are spaced along the axial direction of the reaction tank 901 to monitor the reaction temperature in different areas of the reaction tank 901 in real time, thereby facilitating temperature adjustment. If the temperature is abnormal, it is adjusted by the preheater 8 or the heat transfer oil module. After the hydrogenation reaction, the material enters the condenser 11 and is cooled to room temperature by the cold water supplied by the cold water supply unit. Then it is sent to the gas-liquid separator 12, where gas-liquid separation is achieved. The liquid phase is the hydrogenation product and the gas phase is unreacted hydrogen. After gas-liquid separation, the hydrogenation product is sent to the hydrogenation product collection tank 16 after the flow rate is controlled by the pneumatic liquid level regulating valve and regulating valve 15. Unreacted hydrogen enters the second buffer tank 13 through the gas phase outlet of the gas-liquid separator 12. After the pressure is stabilized by the back pressure valve 14, it is discharged through the high-altitude exhaust port. After the reaction is completed, the raw material supply is shut off, the cleaning solution storage tank and switching valve are opened, and the cleaning solution is delivered to the pipeline and hydrogenation reactor 9 through the high-pressure diaphragm pump 7 to clean the system. If catalyst regeneration is required, the temperature is adjusted through the heat transfer oil module, and the catalyst is regenerated in situ in conjunction with the cleaning solution or hydrogen.
[0031] The DCS control system collects real-time data on hydrogen flow rate, nitrogen flow rate, feed liquid flow rate, reaction temperature, reaction pressure, condenser outlet temperature, and gas-liquid separator level, and displays this data in real-time through the 360 Force Control configuration software. When any of these parameters exceed the set range, such as reaction pressure > 7.5 MPa or reaction temperature > 270°C, the system automatically triggers an alarm and cuts off the feed from the high-pressure diaphragm pump 7 and hydrogen supply equipment 1, while simultaneously starting nitrogen purging to ensure the safety of the device.
[0032] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A continuous hydrogenation apparatus, characterized in that: It includes a gas supply system, a liquid supply system, a heating system, a hydrogenation reactor (9), a gas-liquid mixing distributor (10), a cooling system, a gas-liquid separation system, and a product collection system; The gas supply system and the liquid supply system are respectively connected to the inlet of the gas-liquid mixing distributor (10) through pipelines, and the outlet of the gas-liquid mixing distributor (10) is connected to the inlet of the reactor (9) through a pipeline. The heating system is located between the liquid supply system and the gas-liquid mixing distributor (10) and is used to preheat the raw material liquid; The cooling system is a condenser (11), and the outlet of the hydrogenation reactor (9) is connected to the inlet of the condenser (11) via a pipe; The gas-liquid separation system includes a gas-liquid separation tank (12) and a second buffer tank (13). The outlet of the condenser (11) is connected to the inlet of the gas-liquid separation tank (12) through a pipe, and the gas phase outlet of the gas-liquid separation tank (12) is connected to the inlet of the second buffer tank (13) through a pipe. The product collection system includes a back pressure valve (14) and a product collection tank (16). The back pressure valve (14) is located at the gas phase outlet of the second buffer tank (13). The liquid phase outlet of the gas-liquid separator (12) and the liquid phase outlet of the second buffer tank (13) are connected in sequence to the regulating valve (15) and the product collection tank (16) through pipelines.
2. The continuous hydrogenation apparatus according to claim 1, characterized in that: The gas supply system includes a hydrogen supply device (1), a nitrogen supply device (2), a hydrogen mass flow meter (3), a nitrogen mass flow meter (4), and a first buffer tank (5). The hydrogen supply device (1) is connected to the hydrogen mass flow meter (3) and the first buffer tank (5) in sequence through a pipeline. The nitrogen supply device (2) is connected to the nitrogen mass flow meter (4) and the first buffer tank (5) in sequence through a pipeline. The outlet of the first buffer tank (5) is connected to the inlet of the gas-liquid mixing distributor (10) through a pipeline.
3. The continuous hydrogenation apparatus according to claim 1, characterized in that: The liquid supply system includes a hydrogenation feedstock supply device (6) and a high-pressure diaphragm pump (7). The hydrogenation feedstock supply device (6) is connected to the high-pressure diaphragm pump (7) through a pipeline. The heating system is a preheater (8). The outlet of the high-pressure diaphragm pump (7) is connected to the inlet of the preheater (8) through a pipeline. The outlet of the preheater (8) is connected to the inlet of the gas-liquid mixing distributor (10) through a pipeline.
4. The continuous hydrogenation apparatus according to claim 1, characterized in that: The hydrogenation reactor (9) includes a hollow reaction vessel (901) with openings at the top and bottom. The upper and lower ends of the reaction vessel (901) are respectively sealed with an upper tank cover (902) and a lower tank cover (903). The upper end of the reaction vessel (901) is provided with two first feed pipe joints (904), and the lower tank cover (903) is provided with a second feed pipe joint (905). The reaction vessel (901) is provided with a plurality of first partitions (911) and a plurality of second partitions (912) arranged in concentric circles. The first partitions (911) and the second partitions (912) are spaced apart from each other. An S-shaped flow channel (910) is formed between the first partitions (911) and the second partitions (912). A catalytic structure is provided in the flow channel (910). The lower end of the first partition (911) is fixedly mounted on the lower tank cover (903), and the upper end of the second partition (912) is fixedly mounted on the upper tank cover (902).
5. The continuous hydrogenation apparatus according to claim 4, characterized in that: The reaction vessel (901) is provided with a central channel (906) for connecting the tail end of the flow channel (910) and the second feed pipe joint (905) to each other. The central channel (906) is provided with a spiral rib (907). A central shaft (908) is fixedly provided in the middle of the spiral rib (907). The spiral spacing of the spiral rib (907) is filled with a first catalyst filling layer (909).
6. The continuous hydrogenation apparatus according to claim 4, characterized in that: The catalytic structure includes a first micro-reaction channel (913) disposed in a flow channel (910), the inner wall of the micro-reaction channel (913) is provided with a catalyst coating, and heat exchangers (914) are provided in both the first septum (911) and the second septum (912).
7. The continuous hydrogenation apparatus according to claim 4, characterized in that: The catalytic structure includes a second catalyst filling layer (915), which fills the flow channel (910).
8. The continuous hydrogenation apparatus according to claim 1, characterized in that: The catalytic structure includes a first-stage microreactor (916), a second-stage microreactor (917), and a third-stage microreactor (918) connected in sequence. The second micro-reaction channels in the first-stage microreactor (916), the second-stage microreactor (917), and the third-stage microreactor (918) are all coated with a catalyst coating. The coarse section (919) of the second micro-reaction channel is provided with a crescent-shaped baffle column (921).
9. A continuous hydrogenation process, characterized in that, The continuous hydrogenation apparatus according to any one of claims 1-8 comprises the following steps: S1: First, pretreatment is carried out. The nitrogen supply equipment (2) is turned on, and the nitrogen flow rate is adjusted by the nitrogen mass flow meter (3) so that the nitrogen enters the pipeline and hydrogenation reactor (9) through the first buffer tank (5) to purge and replace the air in the pipeline. At the same time, the system pressure is adjusted to the set back pressure value by the back pressure valve. S2: Add the hydrogenation feedstock to the hydrogenation feedstock supply equipment (6), turn on the high-pressure diaphragm pump (7), and transport the feedstock liquid to the preheater (8). The feedstock liquid is preheated to 30-250℃ by the electric heating module of the preheater (8). S3: Turn on the hydrogen supply equipment (1), adjust the hydrogen flow rate through the hydrogen mass flow meter (3), and after the hydrogen is stably output through the first buffer tank (5), it enters the gas-liquid mixing distributor (10) together with the preheated raw material liquid, and is fully mixed in the distributor to form a gas-liquid mixture; S4: The gas-liquid mixture output from the gas-liquid mixing distributor (10) is fed into the hydrogenation reactor (9) through the first feed pipe joint (904) and the second feed pipe joint (905). The gas-liquid mixture flows through the catalytic structure and completes the hydrogenation reaction under the action of the catalyst coating. During the reaction, the reaction temperature is monitored in real time by a multi-segment multi-point thermometer, which facilitates temperature adjustment. S5: The material after hydrogenation reaction enters the condenser (11), and is cooled to room temperature by the cold water supplied by the cold water supply unit. Then it is sent to the gas-liquid separator (12) to achieve gas-liquid separation. The liquid phase is the hydrogenation product and the gas phase is unreacted hydrogen. S6: After gas-liquid separation, the hydrogenation product is sent to the hydrogenation product collection tank (16) after the flow rate is controlled by the pneumatic liquid level regulating valve and regulating valve (15). Unreacted hydrogen enters the second buffer tank (13) through the gas phase outlet of the gas-liquid separator (12). After the pressure is stabilized by the back pressure valve (14), it is discharged through the high-altitude exhaust port. S7: After the reaction is completed, shut off the raw material supply, open the cleaning liquid storage tank and switching valve, and use the high-pressure diaphragm pump (7) to transport the cleaning liquid to the pipeline and hydrogenation reactor (9) to clean the system.
10. A continuous hydrogenation process according to claim 9, characterized in that, The DCS control system collects data on hydrogen flow rate, nitrogen flow rate, raw material liquid flow rate, reaction temperature, reaction pressure, condenser outlet temperature, and gas-liquid separator level in real time, and displays them in real time through the 360 Force Control configuration software. When any of the parameters exceed the set range, the system automatically triggers an alarm and cuts off the feed of the high-pressure diaphragm pump (7) and hydrogen supply equipment (1), while simultaneously starting nitrogen purging to ensure the safety of the device.
Citation Information
Patent Citations
Continuous hydrogenation reaction device and reaction process
CN110756120A
Fluid-enhanced mixing device for continuous hydrogenation reaction and process method of device
CN109985572A
Insertion sheet type microreactor
CN210303610U
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