Intermittent hydrogenation reaction system

Abstract

The invention discloses an intermittent hydrogenation reaction system, and belongs to the technical field of hydrogenation reaction systems. Comprising a hydrogenation reaction kettle, a first jet device, a secondary pressurizing unit, a second jet device, a hydrogen recycling unit and an emptying pipe valve, wherein the input end of the first jet device is connected with a Y-shaped tee joint; the other two ends of the Y-shaped tee joint are connected with a nitrogen pressure pipeline and a hydrogen pressure pipeline; the middle end of the first jet device is connected to the catalyst feeding unit; the secondary pressurizing unit comprises a pressure-multiplying hydrogen tank, the pressure-multiplying hydrogen tank is connected with a first switch valve through a flange, the first switch valve is connected to an inclined tee joint, and the other two ends of the inclined tee joint are connected to the output end of a first jet device and a second switch valve respectively; according to the intermittent hydrogenation reaction system, multiple times of hydrogen participating in the reaction can be recycled and fully utilized, dynamic gas-liquid mixing is achieved, the hydrogen, a catalyst and liquid are fully mixed, the completeness of the hydrogenation reaction is guaranteed, and hydrogen energy consumption is reduced.

Description

Technical Field

[0001] The present invention specifically relates to an intermittent hydrogenation reaction system, belonging to the technical field of hydrogenation reaction systems. Background Art

[0002] When producing ruthenium trichloride, it needs to undergo a hydrogenation reaction, such as reacting metallic ruthenium powder with hydrogen to generate ruthenium hydroxide, which is then converted into ruthenium trichloride through subsequent treatment. During the hydrogenation reaction, it is necessary to ensure that the hydrogenation reaction is more complete, and the amount of hydrogen participating in the reaction is generally 4-5 times more than that. At present, most domestic manufacturers exhaust the excess hydrogen by venting after each reaction, and then proceed to the production of the next reaction. This operation not only wastes resources and increases production costs, but also poses certain safety risks when a large amount of hydrogen is vented. For this reason, Chinese Patent Publication No.: CN106590940A discloses A device and method for safely adding catalyst to an intermittent hydrogenation reaction are provided. The device and method are intended to reduce hydrogen emissions during the hydrogenation reaction. The structure adds catalyst to a catalyst hopper, opens a pneumatic on / off valve and a first-hand valve, and then closes them; nitrogen replacement is then performed. However, the structure cannot fully utilize hydrogen. Existing hydrogenation processes for hydrogenation reactions generally introduce hydrogen once, with a utilization rate generally less than 60%. Unreacted hydrogen is directly discharged, resulting in resource waste (200-400 m³ of hydrogen is lost per ton of product). Furthermore, hydrogen has low solubility in the liquid phase, and mass transfer resistance results in a slow reaction rate. Summary of the Invention

[0003] To solve the above problems, the present invention proposes an intermittent hydrogenation reaction system, which can circulate and fully utilize multiple hydrogen participating in the reaction, realize dynamic gas-liquid mixing, and fully mix the hydrogen, catalyst and liquid participating in the reaction, thereby ensuring the integrity of the hydrogenation reaction and reducing hydrogen energy consumption.

[0004] The intermittent hydrogenation reaction system of the present invention comprises: Hydrogenation reactor; A first ejector, wherein the input end of the first ejector is connected to a Y-shaped tee; the other two ends of the Y-shaped tee are connected to a nitrogen pressure pipeline and a hydrogen pressure pipeline; the middle end of the first ejector is connected to a catalyst feeding unit; A secondary pressurizing unit, the secondary pressurizing unit comprising a pressure-doubling hydrogen tank, the pressure-doubling hydrogen tank being flange-connected to a first switch valve, the first switch valve being connected to an oblique tee, the other two ends of the oblique tee being respectively connected to the first ejector output end and the second switch valve; A second ejector, the second ejector being fixed inside the hydrogenation reactor; an input end of the second ejector being connected to a second on-off valve; a middle end of the second ejector being connected to a liquid extraction pipe; an output end of the second ejector being provided with a cover; a bottom of the liquid extraction pipe being lower than a bottom surface of the cover; the cover being screwed onto the output end of the second ejector, the cover being above the liquid level inside the hydrogenation reactor, and the liquid extraction pipe extending below the liquid level; A hydrogen recycling unit, comprising a buffer tank, the buffer tank being connected to the interior of the hydrogenation reactor via a third switch valve; the buffer tank is also connected to a pressure-doubled hydrogen tank via a first compressor; The pressure-doubled hydrogen tank and the buffer tank are both equipped with pressure transmitters; An exhaust pipe valve, one end of which is connected to the hydrogenation reactor, and the other end is connected to the exhaust equipment.

[0005] During operation, the hydrogenation reaction material flow is first added to the hydrogenation reactor, then the nitrogen pressure pipeline is opened, and nitrogen is injected into the first ejector. At this time, the catalyst feeding unit is closed, and the nitrogen replaces the feed pipeline of the catalyst feeding unit and the hydrogenation reactor multiple times, and the nitrogen is discharged through the exhaust equipment to discharge the air inside the feed pipeline and the hydrogenation reactor. After the nitrogen replacement is completed, hydrogen and catalyst are mixed and fed, the nitrogen pressure pipeline is closed, and the catalyst feeding unit is activated. The catalyst feeding unit feeds the first ejector, and at the same time, the hydrogen pressure pipeline provides hydrogen to the first ejector, and uses hydrogen as the gas source for conveying air to achieve full mixing of hydrogen and catalyst, and convey it to the side of the second ejector with hydrogen. During the conveying process, the conveying pipeline is pressurized with secondary hydrogen by the double-pressure hydrogen tank to ensure that the input end of the second ejector is sufficient air pressure, after the hydrogen and catalyst pass through the second ejector, a negative pressure is generated at the middle end of the second ejector, thereby drawing the mixed liquid inside the hydrogenation reactor into the second ejector through the liquid extraction pipe, so as to achieve full mixing of the catalyst, reaction fluid and hydrogen, and then re-inject it into the hydrogenation reactor after mixing; when the feeding is completed, the hydrogen pressure pipeline is closed, wherein the amount of supplementary hydrogen fed into the hydrogen pressure pipeline and the amount of catalyst fed need to be matched, specifically: the flow rate of the catalyst entering the first ejector is controlled, so that after all the catalyst is put into the hydrogenation reactor, the amount of hydrogen supplemented meets the supplementation requirement; when the hydrogen is supplemented, the hydrogen recycling unit continues to operate, and the pressure-doubled hydrogen tank continues to provide a hydrogen source to the first ejector through the first switch valve, so as to achieve dynamic and full mixing of hydrogen and the mixed liquid inside the hydrogenation reactor, and to maintain the hydrogen pressure inside the hydrogenation reactor.

[0006] Furthermore, the catalyst feeding unit includes a temporary storage tank, a rotary valve is installed at the bottom of the temporary storage tank, a metering tube is connected to the bottom of the rotary valve, and a fourth switch valve is provided at the bottom of the metering tube; the bottom of the fourth switch valve is connected to the middle end of the first ejector, and the fourth switch valve is an opening valve; an arc plate is provided between a group of adjacent valve plates of the rotary valve, and the arc plate fits the inner wall of the rotary valve; when the catalyst feeding unit is working, the fourth switch valve is closed, and the rotary valve continues to operate until the catalyst fills the metering tube and is sealed by the arc plate; then, the fourth switch valve is opened to the set opening, the first ejector works, and the hydrogen source injects hydrogen into the first ejector, the hydrogen entrains the catalyst, and the hydrogen and the catalyst are fully mixed, and finally injected into the hydrogenation reactor; when the catalyst is fed, the rotary valve is closed first, and the fourth switch valve is opened, and the air inside the metering tube is evacuated and replaced with nitrogen through the first ejector to achieve air replacement in the feed pipeline.

[0007] Furthermore, the lower part of the metering tube is integrally formed with a disc seat, and the disc seat is provided with a plurality of arc grooves; a tube seat is screwed on the bottom of the metering tube, and the tube seat is connected to the fourth switch valve through a flange, and a long bolt is inserted in the arc groove; the bottom of the long bolt is screwed on the upper end face of the tube seat, and a nut that is tightened against the bottom of the disc seat is screwed on the long bolt; the metering tube can be calibrated on site. During calibration, a container of calibrated capacity is used for measurement. During measurement, the fourth switch valve is closed, and the rotary valve continues to operate. When the space between the metering tube and the rotary valve is filled with catalyst, the fourth switch valve is opened and metered through the container. By rotating the metering tube and the tube seat, the capacity between the rotary valve and the fourth switch valve can be adjusted. After the capacity is adjusted to the set value, the long bolt is locked with the tube seat, the long bolt is locked with the disc seat through the nut, and the tightening bolt on the outside of the tube seat is tightened against the metering tube; measurement calibration is achieved.

[0008] Furthermore, a filter is connected to the top of the temporary storage tank through a flange, and an exhaust pipe is provided on the upper part of the filter; a feeding pipe is provided on the upper part of the temporary storage tank, and the feeding pipe is connected to the pneumatic conveying equipment through a pneumatic conveying pipe, and the gas source of the pneumatic conveying equipment is a nitrogen source; during feeding, the nitrogen source is connected to the pneumatic conveying equipment, the catalyst is loaded into the pneumatic conveying equipment, and is fed into the pneumatic conveying pipe and the feeding pipe along with the nitrogen source, and finally stored in the temporary storage tank; the nitrogen source is discharged through the filter, and finally the nitrogen source is discharged through the exhaust pipe. The nitrogen serves as both a power source for catalyst feeding and an air replacement source in the temporary storage tank, and can discharge the air in the temporary storage tank.

[0009] Furthermore, the output end of the exhaust pipe is connected to a second compressor; the output end of the second compressor is connected to a fifth switch valve; the fifth switch valve is connected to a nitrogen storage tank. When the temporary storage tank is loaded with a catalyst flow, a nitrogen source is used as a pneumatic power source to deliver the catalyst to the temporary storage tank. The nitrogen source can be filled into the nitrogen storage tank through the exhaust pipe, the second compressor and the second switch valve.

[0010] Furthermore, a membrane separator is connected in series between the buffer tank and the third switch valve; the separation membrane of the membrane separator is a Pd-Ag alloy membrane, and the purity of hydrogen on the permeate side is ≥95%; the purity meets the reuse requirements.

[0011] Furthermore, a pressure relief valve is connected between the buffer tank and the third switch valve, and the input end of the pressure relief valve is connected to the interior of the hydrogenation reactor; when the gas pressure in the hydrogenation reactor exceeds the pressure value of the pressure relief valve, hydrogen enters the buffer tank until the pressure of the hydrogenation reactor drops to the starting pressure of the pressure relief valve, the pressure relief valve is closed, and then the hydrogen in the buffer tank is pumped into the nitrogen storage tank through the second compressor.

[0012] Furthermore, a feed gate valve and a stirring motor for driving a stirring paddle are installed on the top of the hydrogenation reactor; a safety gap is provided between the stirring paddle and the cover body, and a grid plate is fixed to the inner bottom surface of the cover body. During the hydrogenation reaction, the stirring paddle is driven to rotate by the stirring motor, and the stirring paddle fully stirs the mixed liquid in the hydrogenation reactor. At the same time, in combination with the gas-liquid mixing of the second ejector, an in-depth hydrogenation reaction can be achieved; the second ejector fully mixes the hydrogen and the mixed liquid, and disturbs the gas-liquid flow direction through the grid plate, thereby enhancing the gas-liquid mixing effect and improving the hydrogenation reaction effect.

[0013] Furthermore, the output end of the exhaust device is connected to a cryogenic trap; an external exhaust pipe is provided on the cryogenic trap. When the hydrogenation reactor produces ruthenium trichloride, the hydrogenation reactor provides a reaction heat source. During the reaction, reaction hot steam (such as RuO4) is generated. The hot steam is sent to the cryogenic trap through the exhaust device to deep-cold liquefy RuO4, so that RuO4 with high added value can be recovered.

[0014] Furthermore, a through-tube is integrally formed on the top of the hydrogenation reactor, the bottom end of the through-tube is fixed to the input end of the second ejector via a flange, and the top end of the through-tube is fixed to the second switch valve via a flange. The through-tube enables a sealed connection between the second ejector and the second switch valve, thereby ensuring the sealing of the hydrogen source connected to the hydrogenation reactor.

[0015] Compared with the prior art, the intermittent hydrogenation reaction system of the present invention adopts multiple times of recovered hydrogen as a basic gas source, and supplements new hydrogen to ensure that the hydrogenation reaction has a sufficient hydrogen source. During the hydrogenation reaction, the nitrogen gas source and the first ejector cooperate to purge the hydrogenation reactor while simultaneously performing gas replacement on the metering and feeding pipelines to remove air. During the production of the hydrogenation reactor, an intermittent production mode of single feeding and single discharging is adopted. Each time the material is added, the hydrogen pressure pipeline and the first ejector cooperate to achieve pneumatic conveying of the catalyst. At the same time, the hydrogen used for pneumatic conveying is used as a supplementary hydrogen source for a new hydrogenation reaction, and the recovered hydrogen source is reused as the basic hydrogen source for the hydrogenation reaction. The hydrogen can be fully utilized, and the basic hydrogen source achieves dynamic gas-liquid mixing to achieve a complete hydrogenation reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the overall structure of the intermittent hydrogenation reaction system of the present invention.

[0017] Figure 2 For the present invention Figure 1 Schematic diagram of the locally enlarged structure at point A in the middle.

[0018] Figure 3 This is a schematic structural diagram of an embodiment of a catalyst feeding unit of the present invention.

[0019] Figure 4 This is a schematic structural diagram of another embodiment of the catalyst feeding unit of the present invention.

[0020] Figure 5 This is a schematic diagram of the overall structure of the intermittent hydrogenation reaction system and membrane separator installed in the present invention.

[0021] Figure 6 This is a schematic diagram of the overall structure of the intermittent hydrogenation reaction system and the pressure relief valve installation of the present invention.

[0022] Figure 7 This is a schematic diagram of the installation structure of the cover body and grid plate of the present invention.

[0023] Figure 1: Hydrogenation reactor, 2: First ejector, 3: Y-shaped tee, 4: Nitrogen pressure line, 5: Hydrogen pressure line, 6: Catalyst feeding unit, 7: Pressure-doubling hydrogen tank, 8: First switch valve, 9: Oblique tee, 10: Second switch valve, 11: Second ejector, 12: Liquid extraction pipe, 13: Cover, 14: Buffer tank, 15: Third switch valve, 16: First compressor, 17: Pressure transmitter, 18: Drain valve, 19: Temporary storage tank , 20, rotary valve, 21, metering tube, 22, fourth switch valve, 23, disc seat, 24, arc groove, 25, pipe seat, 26, long bolt, 27, nut, 28, filter, 29, drain pipe, 30, feeding pipe, 31, second compressor, 32, fifth switch valve, 33, nitrogen storage tank, 34, membrane separator, 35, pressure relief valve, 36, feed gate valve, 37, stirring paddle, 38, stirring motor, 39, through pipe, 40, grid plate. DETAILED DESCRIPTION

[0024] Example: like Figures 1 to 7 The intermittent hydrogenation reaction system shown comprises: Hydrogenation reactor 1; A first ejector 2, wherein the input end of the first ejector 2 is connected to a Y-shaped tee 3; the other two ends of the Y-shaped tee 3 are connected to a nitrogen pressure pipeline 4 and a hydrogen pressure pipeline 5; the middle end of the first ejector 2 is connected to a catalyst feeding unit 6; A secondary pressurizing unit, comprising a pressure-doubling hydrogen tank 7, to which a first switch valve 8 is connected via a flange. The first switch valve 8 is connected to an oblique tee 9, the other two ends of which are respectively connected to the output end of the first ejector 2 and the second switch valve 10; A second ejector 11 is fixed inside the hydrogenation reactor 1; the input end of the second ejector 11 is connected to the second on-off valve 10; the middle end of the second ejector 11 is connected to a liquid extraction pipe 12; the output end of the second ejector 11 is provided with a cover 13; the bottom of the liquid extraction pipe 12 is lower than the bottom surface of the cover 13; the cover 13 is screwed onto the output end of the second ejector 11, the cover 13 covers the liquid surface inside the hydrogenation reactor 1, and the liquid extraction pipe 12 extends below the liquid surface. A hydrogen recycling unit includes a buffer tank 14, which is connected to the interior of the hydrogenation reactor 1 through a third switch valve 15; the buffer tank 14 is also connected to the pressure-doubled hydrogen tank 7 through a first compressor 16; The pressure-doubled hydrogen tank 7 and the buffer tank 14 are both equipped with a pressure transmitter 17; The drain valve 18 has one end connected to the hydrogenation reactor 1 and the other end connected to the exhaust device.

[0025] During operation, the feed flow of the hydrogenation reaction is first added to the hydrogenation reactor 1, and then the nitrogen pressure pipeline 4 is opened, and nitrogen is injected into the first ejector 2. At this time, the catalyst feeding unit 6 is closed, and the nitrogen replaces the feed pipeline of the catalyst feeding unit 6 and the hydrogenation reactor 1 multiple times, and the nitrogen is discharged through the exhaust equipment to discharge the air inside the feed pipeline and the hydrogenation reactor 1. After the nitrogen replacement is completed, the hydrogen and catalyst are mixed and fed, the nitrogen pressure pipeline 4 is closed, and the catalyst feeding unit 6 is activated. The catalyst feeding unit 6 feeds the first ejector 2, and at the same time, the hydrogen pressure pipeline 5 provides hydrogen to the first ejector 2, and uses hydrogen as the gas source for conveying air to achieve full mixing of hydrogen and catalyst, and convey it to the side of the second ejector 11 with hydrogen. During the conveying process, the conveying pipeline is pressurized with secondary hydrogen by the double-pressure hydrogen tank 7 to ensure that the input end of the second ejector 11 is sufficient After the hydrogen and catalyst pass through the second ejector 11, a negative pressure is generated at the middle end of the second ejector 11, thereby drawing the mixed liquid inside the hydrogenation reactor 1 into the second ejector 11 through the liquid extraction pipe 12, so as to achieve full mixing of the catalyst, reaction fluid and hydrogen, and then inject them back into the hydrogenation reactor 1 after mixing; when the feeding is completed, the hydrogen pressure pipeline 5 is closed, wherein the amount of supplementary hydrogen fed into the hydrogen pressure pipeline 5 and the amount of catalyst fed need to be matched, specifically: the flow rate of the catalyst entering the first ejector 2 is controlled, so that after all the catalyst is put into the hydrogenation reactor 1, the amount of hydrogen supplemented meets the supplementation requirement; when the hydrogen is supplemented, the hydrogen recycling unit continues to operate, and the pressure-doubled hydrogen tank 7 continues to provide a hydrogen source to the first ejector 2 through the first switch valve 8, so as to achieve dynamic and full mixing of hydrogen and the mixed liquid inside the hydrogenation reactor 1, and to maintain the hydrogen pressure inside the hydrogenation reactor 1.

[0026] The catalyst feeding unit 6 includes a temporary storage tank 19, a rotary valve 20 is installed at the bottom of the temporary storage tank 19, the bottom of the rotary valve 20 is connected to a metering pipe 21, and a fourth switch valve 22 is provided at the bottom of the metering pipe 21; the bottom of the fourth switch valve 22 is connected to the middle end of the first ejector 2, and the fourth switch valve 22 is an opening valve; an arc plate is provided between a group of adjacent valve plates of the rotary valve 20, and the arc plate is attached to the inner wall of the rotary valve 20; when the catalyst feeding unit 6 is working, the fourth switch valve 22 is closed, and the rotary valve 20 is opened. The valve 20 continues to operate until the catalyst fills the metering tube 21 and is closed by the arc plate; then, the fourth switch valve 22 is opened to the set opening, the first ejector 2 works, and the hydrogen source injects hydrogen into the first ejector 2. The hydrogen entrains the catalyst and achieves full mixing of hydrogen and catalyst, and finally injects it into the hydrogenation reactor 1; when the catalyst is fed, the rotary valve 20 is first closed and the fourth switch valve 22 is opened. The air inside the metering tube 21 is evacuated and replaced with nitrogen through the first ejector 2 to achieve air replacement in the feed pipeline.

[0027] The lower part of the metering tube 21 is integrally formed with a disc seat 23, and a plurality of arc-shaped grooves 24 are opened on the disc seat 23; a tube seat 25 is screwed to the bottom of the metering tube 21, and the tube seat 25 is connected to the fourth switch valve 22 through a flange, and a long bolt 26 is inserted into the arc-shaped groove 24; the bottom of the long bolt 26 is screwed to the upper end surface of the tube seat 25, and a nut 27 that is tightened against the bottom of the disc seat 23 is screwed on the long bolt 26; the metering tube 21 can be calibrated on site. During calibration, a container with a calibrated capacity is used for measurement. , close the fourth switch valve 22, the rotary valve 20 continues to operate, and when the space between the metering tube 21 and the rotary valve 20 is filled with catalyst, open the fourth switch valve 22, and measure it through the container, and by rotating the metering tube 21 and the tube seat 25, the capacity between the rotary valve 20 and the fourth switch valve 22 can be adjusted until the capacity is adjusted to the set value, the long bolt 26 is locked with the tube seat 25, the long bolt 26 and the disc seat 23 are locked by the nut 27, and the tightening bolt outside the tube seat 25 is tightened with the metering tube 21; to achieve measurement calibration.

[0028] The top of the temporary storage tank 19 is connected to a filter 28 through a flange, and an exhaust pipe 29 is provided on the upper part of the filter 28; a feeding pipe 30 is provided on the upper part of the temporary storage tank 19, and the feeding pipe 30 is connected to the pneumatic conveying equipment through a pneumatic conveying pipe, and the gas source of the pneumatic conveying equipment is a nitrogen gas source; during feeding, the nitrogen gas source is connected to the pneumatic conveying equipment, the catalyst is loaded into the pneumatic conveying equipment, and is fed into the pneumatic conveying pipe and the feeding pipe 30 along with the nitrogen gas source, and finally stored in the temporary storage tank 19; the nitrogen gas source is discharged through the filter 28 and finally discharged through the exhaust pipe 29. The nitrogen gas serves as both a power source for catalyst feeding and an air replacement gas source in the temporary storage tank 19, and can discharge the air in the temporary storage tank 19.

[0029] The output end of the exhaust pipe 29 is connected to a second compressor 31; the output end of the second compressor 31 is connected to a fifth switch valve 32; the fifth switch valve 32 is connected to a nitrogen storage tank 33. When the temporary storage tank 19 is loaded with a catalyst flow, a nitrogen source is used as a pneumatic power source to deliver the catalyst to the temporary storage tank 19. The nitrogen source can be filled into the nitrogen storage tank 33 through the exhaust pipe 29, the second compressor 31 and the second switch valve 10.

[0030] A membrane separator 34 is connected in series between the buffer tank 14 and the third switch valve 15 ; the separation membrane of the membrane separator 34 is a Pd-Ag alloy membrane, and the purity of hydrogen on the permeate side is ≥95%; the purity meets the reuse requirements.

[0031] A pressure relief valve 35 is connected between the buffer tank 14 and the third switch valve 15, and the input end of the pressure relief valve 35 is connected to the interior of the hydrogenation reactor 1; when the air pressure in the hydrogenation reactor 1 exceeds the pressure value of the pressure relief valve 35, hydrogen enters the buffer tank 14 until the pressure of the hydrogenation reactor 1 drops to the starting pressure of the pressure relief valve 35, and the pressure relief valve 35 is closed. Then, the hydrogen in the buffer tank 14 is pumped into the nitrogen storage tank 33 through the second compressor 31.

[0032] A feed gate valve 36 and a stirring motor 38 for driving a stirring paddle 37 are installed on the top of the hydrogenation reactor 1; a safety gap is set between the stirring paddle 37 and the cover body 13, and a grid plate 40 is fixed to the inner bottom surface of the cover body 13. During the hydrogenation reaction, the stirring paddle 37 is driven to rotate by the stirring motor 38, and the stirring paddle 37 fully stirs the mixed liquid in the hydrogenation reactor 1. At the same time, in conjunction with the gas-liquid mixing of the second ejector 11, an in-depth hydrogenation reaction can be achieved; the second ejector 11 fully mixes the hydrogen and the mixed liquid, and disturbs the gas-liquid flow direction through the grid plate 40, thereby enhancing the gas-liquid mixing effect and improving the hydrogenation reaction effect.

[0033] The output end of the exhaust device is connected to a cryogenic trap; an external exhaust pipe is provided on the cryogenic trap. When the hydrogenation reactor 1 produces ruthenium trichloride, the hydrogenation reactor 1 provides a reaction heat source. During the reaction, reaction hot steam (such as RuO4) is generated. The hot steam is sent to the cryogenic trap through the exhaust device to deep-cold liquefy RuO4, so that RuO4 with high added value can be recovered.

[0034] The top of the hydrogenation reactor 1 is integrally formed with a through-tube 39, the bottom end of the through-tube 39 is fixed to the input end of the second ejector 11 through a flange, and the top end of the through-tube 39 is fixed to the second switch valve 10 through a flange. The through-tube 39 can achieve a sealed connection between the second ejector 11 and the second switch valve 10, thereby ensuring the sealing of the hydrogen source connected to the hydrogenation reactor 1.

[0035] The above embodiments are only preferred implementations of the present invention. Therefore, any equivalent changes or modifications made according to the structures, features and principles described in the scope of application of the present invention are included in the scope of application of the present invention.

Claims

1. An intermittent hydrogenation reaction system, characterized in that: include: Hydrogenation reactor; a first ejector, wherein an input end of the first ejector is connected to a Y-shaped tee; The other two ends of the Y-shaped tee are connected to a nitrogen pressure pipeline and a hydrogen pressure pipeline; the middle end of the first ejector is connected to a catalyst feeding unit; A secondary pressurizing unit, the secondary pressurizing unit comprising a pressure-doubling hydrogen tank, the pressure-doubling hydrogen tank being flange-connected to a first switch valve, the first switch valve being connected to an oblique tee, the other two ends of the oblique tee being respectively connected to the first ejector output end and the second switch valve; a second ejector, the second ejector being fixed inside the hydrogenation reactor; an input end of the second ejector being connected to a second switch valve; a middle end of the second ejector being connected to a liquid extraction pipe; an output end of the second ejector being provided with a cover; a bottom of the liquid extraction pipe being lower than a bottom surface of the cover; A hydrogen recycling unit, comprising a buffer tank, the buffer tank being connected to the interior of the hydrogenation reactor via a third switch valve; the buffer tank is also connected to a pressure-doubled hydrogen tank via a first compressor; The pressure-doubled hydrogen tank and the buffer tank are both equipped with pressure transmitters; An exhaust pipe valve, one end of which is connected to the hydrogenation reactor, and the other end is connected to the exhaust equipment.

2. The intermittent hydrogenation reaction system according to claim 1, characterized in that: The catalyst feeding unit includes a temporary storage tank, a rotary valve is installed at the bottom of the temporary storage tank, the bottom of the rotary valve is connected to a metering pipe, and a fourth switch valve is provided at the bottom of the metering pipe; the bottom of the fourth switch valve is connected to the middle end of the first ejector, and the fourth switch valve is an opening valve; an arc plate is provided between a group of adjacent valve plates of the rotary valve, and the arc plate is in contact with the inner wall of the rotary valve.

3. The intermittent hydrogenation reaction system according to claim 2, characterized in that: The lower part of the metering tube is integrally formed with a disc seat, and a plurality of arc-shaped grooves are provided on the disc seat; a tube seat is screwed onto the bottom of the metering tube, and the tube seat is connected to the fourth switch valve through a flange, and a long bolt is inserted into the arc-shaped groove; the bottom of the long bolt is screwed onto the upper end face of the tube seat, and a nut is screwed onto the long bolt to be tightened against the bottom of the disc seat.

4. The intermittent hydrogenation reaction system according to claim 2, characterized in that: The top of the temporary storage tank is connected to a filter through a flange, and an exhaust pipe is provided on the upper part of the filter; a feeding pipe is provided on the upper part of the temporary storage tank, and the feeding pipe is connected to the pneumatic conveying equipment through a pneumatic conveying pipe, and the gas source of the pneumatic conveying equipment is a nitrogen gas source.

5. The intermittent hydrogenation reaction system according to claim 4, characterized in that: The output end of the exhaust pipe is connected to a second compressor; the output end of the second compressor is connected to a fifth switch valve; and the fifth switch valve is connected to a nitrogen storage tank.

6. The intermittent hydrogenation reaction system according to claim 1, characterized in that: A membrane separator is connected in series between the buffer tank and the third switch valve; the separation membrane of the membrane separator is a Pd-Ag alloy membrane, and the purity of hydrogen on the permeate side is ≥95%.

7. The intermittent hydrogenation reaction system according to claim 1, characterized in that: A pressure relief valve is connected between the buffer tank and the third switch valve, and an input end of the pressure relief valve is communicated with the interior of the hydrogenation reactor.

8. The intermittent hydrogenation reaction system according to claim 1, characterized in that: A feed gate valve and a stirring motor for driving a stirring paddle are installed on the top of the hydrogenation reactor; a safety gap is set between the stirring paddle and the cover body, and a grid plate is fixed on the inner bottom surface of the cover body.

9. The intermittent hydrogenation reaction system according to claim 1, characterized in that: The output end of the exhaust device is connected to a cryogenic trap; an external exhaust pipe is provided on the cryogenic trap.

10. The intermittent hydrogenation reaction system according to claim 1, characterized in that: The top of the hydrogenation reactor is integrally formed with a through-tube, the bottom end of the through-tube is fixed to the input end of the second ejector through a flange, and the top end of the through-tube is fixed to the second switch valve through a flange.

Images