Reaction device and reaction system for treating waste catalyst with solid carbide slag

Abstract

The application discloses a reaction device and a reaction system for treating waste catalyst by solid calcium carbide slag, which comprises a rack, a kettle body rotatably connected to the rack, a mixing cavity in the kettle body, a feeding port and a discharging port communicated with the mixing cavity, a liquid-phase feeding pipe with one end extended into the mixing cavity and connected with a spraying pipe, and a vacuum extraction pipe with one end extended into the mixing cavity and connected with a filter at one end and a vacuum pump at the other end, wherein the filter is arranged above the spraying pipe, and the kettle body can rotate relative to the liquid-phase feeding pipe and the vacuum extraction pipe. Through the rotation of the kettle body and the step-by-step introduction of the waste catalyst into the kettle body, the mixing reaction is more sufficient.

Description

Technical Field

[0001] This application relates to the technical field of waste catalyst treatment, and in particular to a reaction apparatus and reaction system for treating waste catalysts with solid carbide slag. Background Technology

[0002] Liquid-phase catalytic fluorination is a common process in fluorochemical production. For example, in the process of producing HFC 113a through the fluorination of tetrachloroethylene, antimony pentachloride is used as a catalyst. After a period of time, this catalyst deactivates and becomes waste catalyst. The conventional methods for treating waste fluorination catalysts are hydrolysis or incineration. However, both hydrolysis and incineration present challenges due to their complex composition, primarily containing halogenated hydrocarbons, resulting in high treatment costs, difficulty in treatment, and significant environmental impact from incomplete treatment of fluorinated wastewater.

[0003] To address the issue of waste fluorination catalyst disposal, methods using carbide slag for treating waste catalysts have emerged in the market. For example, the utility model patent with authorization announcement number CN212425659U discloses "a device for treating waste antimony pentachloride," which introduces liquid-phase waste catalyst into a reactor containing carbide slag for chemical reaction treatment. This reactor is generally a screw type, and continuous stirring is used to achieve mixing and reaction between the waste catalyst and carbide slag. However, the mixing in this type of reaction device is prone to being insufficient, leading to incomplete reaction. Utility Model Content

[0004] To improve the adequacy of the mixing reaction between carbide slag and spent catalyst, the first objective of this application is to provide a reaction apparatus for treating spent catalyst with solid carbide slag.

[0005] The reaction apparatus for treating waste catalysts from solid carbide slag provided in this application adopts the following technical solution: A reaction apparatus for treating waste catalysts from solid carbide slag, comprising: frame; The vessel body is rotatably connected to the frame, and the vessel body has a mixing chamber and an inlet and an outlet communicating with the mixing chamber; A liquid phase inlet pipe extends one end into the mixing chamber, and the liquid phase inlet pipe is connected to a spray pipe; and A vacuum tube extends into the mixing chamber at one end, a filter is connected to one end of the vacuum tube, and a vacuum pump is connected to the other end of the vacuum tube. The filter is positioned above the spray tube. The vessel body can rotate relative to the liquid phase inlet pipe and the vacuum pipe.

[0006] By adopting the above technical solution, solid carbide slag is placed in the mixing chamber of the reactor body. The reactor body itself can rotate relative to the frame to replace the traditional screw stirring structure for agitating the material. Waste catalyst is introduced into the reactor body through the liquid phase inlet pipe. Since the reactor body can rotate relative to the liquid phase inlet pipe, the waste catalyst can be introduced gradually and according to a fixed metering and time. This allows the solid carbide slag in the reactor body to always have a sufficient mixing reaction with a fixed amount of waste catalyst. At the same time, the waste catalyst can increase the contact range between itself and the solid carbide slag through the spray pipe, which can more effectively improve the mixing. The waste gas generated by the reaction is carried out of the reactor body through the vacuum pipe and is treated by the subsequent waste gas treatment device before being discharged.

[0007] Preferably, the filter comprises: A cylindrical body, the cylindrical body having a cavity connected to a vacuum tube, and the cylindrical body having a plurality of filter holes on its outer peripheral surface; and A baffle is connected to the top of the cylinder and extends along the height direction of the cylinder. The lower end face of the baffle is spaced apart from the outer circumferential surface of the cylinder.

[0008] By adopting the above technical solution, the exhaust gas generated during the mixing reaction will contain solid particles. Some particles can be blocked by the filter and enter the vacuum tube. However, after the reaction has been going on for a period of time, they tend to accumulate on the upper surface of the filter, affecting the filtration effect. The baffle can reduce the dust accumulation in the area above the filter and improve the service life of the filter.

[0009] Preferably, the end face of the baffle away from the cylinder is an arc-shaped surface.

[0010] By adopting the above technical solution, the curved surface design allows some of the dust falling onto the baffle to slide off under its own gravity, thereby reducing dust accumulation on the baffle.

[0011] Preferably, it further includes a first rotating assembly, a second rotating assembly, and a drive assembly mounted on a frame; the first rotating assembly and the second rotating assembly are respectively connected to both ends of the vessel body, the drive assembly is connected to the first rotating assembly, the vacuum tube passes through the first rotating assembly and the two can rotate relative to each other, and the liquid phase inlet pipe passes through the second rotating assembly and the two can rotate relative to each other.

[0012] By adopting the above technical solution, the driving component drives the first rotating component to rotate, and the first rotating component drives the vessel to rotate. At the same time as the vessel rotates, the second rotating component rotates synchronously as a passive rotating component. The first rotating component and the second rotating component are respectively placed at both ends of the vessel to ensure the stability of the vessel's rotation. The vacuum tube and the liquid phase inlet tube are respectively inserted into the first rotating component and the second rotating component to achieve relative rotation with respect to the vessel, ensuring the introduction of waste catalyst and the removal of waste gas generated by the reaction.

[0013] Preferably, the first rotating component includes: A first bearing seat, one end of which is connected to the vessel body; First bearing housing; mounted on the frame, and A first rotating shaft is installed inside a first bearing housing and one end is connected to the first bearing housing; The first rotating shaft has a first guide channel for the vacuum tube to pass through, the first shaft seat has a first mounting hole for the vacuum tube to pass through, and the drive assembly is connected to the first rotating shaft.

[0014] By adopting the above technical solution, the drive component drives the first rotating shaft to rotate relative to the first bearing seat. The first rotating shaft is connected to the first bearing seat and synchronously drives the first bearing seat to rotate. The first bearing seat is connected to the vessel body and thus drives the vessel body to rotate. At the same time, the first rotating shaft is installed on the first bearing seat to ensure a certain limit on axial movement while providing support, thereby improving the stability of the first rotating shaft during rotation.

[0015] Preferably, the second rotating component includes: The second shaft seat, one end of which is connected to the vessel body; Second bearing housing; mounted on the frame, and The second rotating shaft is installed inside the second bearing housing and one end is connected to the second bearing housing; The second rotating shaft has a second guide channel for the liquid phase inlet pipe to pass through, and the second shaft seat has a second mounting hole for the liquid phase inlet pipe to pass through.

[0016] By adopting the above technical solution, during the rotation of the vessel body, the connected second shaft seat is driven to rotate, the second shaft seat drives the second rotating shaft to rotate, and the second rotating shaft is installed on the second bearing seat to maintain the stability during rotation.

[0017] Preferably, the driving component includes: motor, The speed reducer is connected to the motor; The reducer is connected to the first rotating shaft via a belt drive.

[0018] By adopting the above technical solution, the output torque of the motor is increased by the reducer and then driven by the belt drive to rotate the first shaft.

[0019] To improve the adequacy of the mixing reaction between carbide slag and spent catalyst, a second objective of this application is to provide a reaction system.

[0020] The reaction system provided in this application adopts the following technical solution: A reaction system includes a waste catalyst storage tank, a transfer pump, the aforementioned reaction apparatus, a vacuum pump, a water washing tower, an alkali washing tower, and a recovery tank, connected in sequence; the outlet end of the transfer pump is connected to the inlet end of a liquid phase inlet pipe, and the outlet end of the vacuum pipe is connected to the inlet end of the vacuum pump. By adopting the above technical solution, the waste catalyst is pumped out of the storage tank by the transfer pump and gradually introduced into the reaction device. The waste gas generated by the reaction is discharged from the vacuum pipe by the vacuum pump and passes through the water washing tower and the alkali washing tower in sequence to neutralize the dust particles and acidic substances. Finally, the waste liquid is discharged into the recovery pool and the treated waste gas meets the emission standards.

[0021] Preferably, the vacuum pump and water washing tower device is further equipped with a total condenser, and the outlet of the total condenser is connected to a collection tank.

[0022] By adopting the above technical solutions, the total condenser can better condense and recover waste gas.

[0023] Preferably, the vacuum tube is connected to a manifold, and a first control valve is installed on the pipe connecting the manifold and the vacuum pump; a backflushing nitrogen pipe is also connected to the manifold, and a second control valve is installed on the backflushing nitrogen pipe.

[0024] By adopting the above technical solution, the backflush nitrogen pipe can introduce nitrogen into the vacuum tube. After the reaction is completed, the nitrogen gas introduced into the reaction device in reverse can effectively blow out and clean the dust in the filter, especially the filter holes. At the same time, nitrogen gas, as an inert gas, can play a certain role in ensuring reaction safety when placed in the mixing chamber.

[0025] In summary, this application includes at least one of the following beneficial technical effects: 1. By rotating the reactor body and gradually introducing the waste catalyst into the reactor body, the mixing reaction is made more complete; 2. By setting up filters and connecting vacuum pipes, the waste gas generated in the reaction can be treated in the subsequent process and discharged in compliance with standards, thus achieving environmental protection. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the reaction apparatus in Example 1; Figure 2The first embodiment mainly shows the connection diagram of the upper baffle of the filter; Figure 3 This is a schematic diagram of the reaction system in Example 2.

[0027] Explanation of reference numerals in the attached drawings: 10. Reaction apparatus; 11. Frame; 12. Vessel body; 121. Mixing chamber; 122. Feed inlet; 123. Discharge outlet; 13. Liquid phase inlet pipe; 131. Spray pipe; 14. Vacuum pipe; 15. Filter; 151. Cylinder; 1511. Chamber; 152. Baffle; 1521. Arc-shaped surface; 153. Connecting block; 16. First rotating assembly; 161. First bearing seat; 162. First rotating shaft; 163. First bearing seat; 17. Second rotating assembly; 171. Second bearing seat; 172. Second rotating shaft; 173. Second bearing housing; 18. Drive assembly; 181. Motor; 182. Reducer; 183. Pulley; 184. Belt; 19. Manifold; 191. First control valve; 192. Second control valve; 193. Backflush nitrogen pipe; 20. Waste catalyst storage tank; 30. Meter; 40. Transfer pump; 50. Vacuum pump; 60. Water washing tower; 70. Alkali washing tower; 80. Recovery tank; 90. Total condenser; 91. Cooling water inlet pipe; 92. Cooling water return pipe; 100. Collection tank; 110. Circulation pump; 120. Solid carbide slag. Detailed Implementation

[0028] The present application will be further described in detail below with reference to the accompanying drawings.

[0029] It should be noted that when an element is referred to as being "fixed to" another element, it can be directly attached to the other element or there may be an intervening element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or there may be an intervening element. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only possible implementation.

[0030] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the specification of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items. Example 1

[0031] Figure 1 and Figure 2A schematic diagram of a reaction apparatus for treating spent catalyst with solid carbide slag is shown. The apparatus includes a frame 11 and a vessel 12 rotatable relative to the frame 11. The vessel 12 is a single-cone vessel with a mixing chamber 121 inside. An inlet 122 and an outlet 123, respectively, are located at both ends of the vessel 12 and communicate with the mixing chamber 121. In this embodiment, before reacting the spent catalyst, solid carbide slag 120 is poured into the inlet 122. The total mass ratio of carbide slag to spent catalyst is: carbide slag: spent catalyst = 1:0.7.

[0032] The reaction apparatus 10 also includes a first rotating assembly 16, a second rotating assembly 17, and a drive assembly 18. The first rotating assembly 16 and the second rotating assembly 17 are respectively connected to the two sides of the vessel body 12, and the drive assembly 18 is connected to the first rotating assembly 16. Thus, the first rotating assembly 16 is the driving component, and the second rotating assembly 17 is the driven component.

[0033] The first rotating assembly 16 includes a first bearing seat 161, a first bearing housing 163, and a first rotating shaft 162. The first bearing housing 163 is mounted on the frame 11, and the first bearing seat 161 is connected to the vessel body 12. The connection between the two can be a flange connection or welding, allowing them to rotate as a single unit. The first rotating shaft 162 is mounted on the first bearing housing 163, with both ends extending from within the first bearing housing 163. One end is connected to the first bearing seat 161, and the other end is connected to the drive assembly 18.

[0034] The second rotating assembly 17 includes a second shaft seat 171, a second bearing seat 173, and a second rotating shaft 172. The second bearing seat 173 is mounted on the frame 11. The second shaft seat 171 is connected to the side of the vessel body 12 opposite to the first shaft seat 161, and the connection between the two can be a flange connection or welding, allowing them to rotate as a single unit. The second rotating shaft 172 is mounted on the second bearing seat 173, and one end is connected to the second shaft seat 171.

[0035] The drive assembly 18 includes a motor 181 and a reducer 182 mounted on the frame 11. The motor 181 is connected to the reducer 182. In this embodiment, the motor 181 is connected to the reducer 182 via a belt 184, but a gear transmission can also be used. Both the output shaft of the reducer 182 and the first rotating shaft 162 are equipped with belt pulleys 183, which are connected by a belt 184, thereby connecting the first rotating shaft 162 to the drive assembly 18.

[0036] The reaction apparatus 10 also includes a liquid phase inlet pipe 13 and a vacuum pipe 14. A first guide channel is provided inside the first rotating shaft 162, and a first mounting hole communicating with the mixing chamber 121 is provided in the first shaft seat 161. One end of the vacuum pipe 14 extends from the first guide channel, enters and passes through the first mounting hole, and is placed inside the mixing chamber 121. A sealing ring is provided between the outer wall of the vacuum pipe 14 and the inner wall of the first mounting hole. A filter 15 is also connected to one end of the vacuum pipe 14 placed inside the mixing chamber 121, and a vacuum pump 50 is connected to the other end of the vacuum pipe 14.

[0037] A second guide channel is provided inside the second rotating shaft 172, and a second mounting hole is provided in the second shaft seat 171 to connect to the mixing chamber 121. One end of the liquid phase inlet pipe 13 extends from the second guide channel and passes through the second mounting hole to be placed inside the mixing chamber 121. A sealing ring is provided between the outer wall of the liquid phase inlet pipe 13 and the inner wall of the second mounting hole. One end of the liquid phase inlet pipe 13 placed inside the mixing chamber 121 is connected to a spray pipe 131. The spray pipe 131 has multiple spray heads arranged at intervals. A filter 15 is placed vertically above the spray pipe 131. The filter 15 is connected to the vacuum pipe 14 by welding. Similarly, the spray pipe 131 is also connected to the liquid phase inlet pipe 13 by welding. This allows the vertical height difference between the filter 15 and the spray pipe 131 to be adjusted as needed, and also facilitates installation. Both the liquid phase inlet pipe 13 and the vacuum pipe 14 are kept in a relative rotational connection with the vessel body 12. That is, when the vessel body 12 rotates, both the liquid phase inlet pipe 13 and the vacuum pipe 14 remain stationary.

[0038] The filter 15 includes a cylindrical body 151. The outer surface of the cylindrical body 151 is provided with a plurality of filter holes. Two spaced connecting blocks 153 are also connected to the cylindrical body 151. A baffle 152 is provided on the two connecting blocks 153. The baffle 152 extends along the height direction of the cylindrical body 151. The upper surface of the baffle 152 is an arc-shaped surface 1521. The entire baffle 152 is placed above the cylindrical body 151 and has a certain distance from the cylindrical body 151 to reduce the obstruction of the filter holes.

[0039] In the reaction apparatus 10 of this application, when processing the spent catalyst, the spent catalyst is gradually injected from one side of the liquid phase inlet pipe 13, and the spray pipe 131 is used to expand the injection range and increase the contact range with the solid carbide slag 120. The vessel body 12 rotates forward and backward under the drive component 18 to further improve the mixing of the spent catalyst and the solid carbide slag 120. The amount of spent catalyst injected each time can be fixed, thereby achieving a full and continuous reaction of the spent catalyst. Example 2

[0040] See Figure 3A reaction system includes a spent catalyst storage tank 20, a transfer pump 40, a reaction device 10 (as described in Example 1), a vacuum pump 50, a total condenser 90, a water washing tower 60, an alkali washing tower 70, and a recovery tank 80, all connected in sequence. The spent catalyst storage tank 20 is connected to a metering device 30. The connection between the metering device 30 and the spent catalyst storage tank 20 to ensure a fixed output volume is existing technology and will not be described in detail in this embodiment. A certain amount of spent catalyst is pumped into the reaction device 10 via the transfer pump 40, the output of which is connected to the liquid phase inlet pipe 13.

[0041] One end of the vacuum tube 14 is also connected to a manifold 19. The manifold 19 is divided into two branches that connect to the vacuum pump 50 and the backflushing nitrogen tube 193. A first control valve 191 is installed on the pipeline between the manifold 19 and the vacuum pump 50, and a second control valve 192 is installed on the backflushing nitrogen tube 193. The first control valve 191 and the second control valve 192 can be solenoid valves or manual valves to control the connection between the manifold 19 and the vacuum pump 50 or the backflushing nitrogen tube 193.

[0042] The output end of the vacuum pump 50 is connected to the total condenser 90. The total condenser 90 is also connected to a cooling water inlet pipe 91 and a cooling water return pipe 92. The cooling water circulates in the total condenser 90 to condense the exhaust gas. The liquid outlet of the total condenser 90 is connected to a recovery tank for recovering the condensed liquid.

[0043] Both the water washing tower 60 and the alkali washing tower 70 are equipped with a circulation pump 110. The circulation pump 110 realizes the circulation of condensate in the water washing tower 60 and the circulation of alkali solution in the alkali washing tower 70. Both the water washing tower 60 and the alkali washing tower 70 are spray type. After the exhaust gas passes through the water washing tower 60, dust particles can be further removed. After passing through the alkali washing tower 70, acidic substances in the exhaust gas are neutralized. The exhaust gas that meets the standards is discharged from the exhaust port of the alkali washing tower 70, and the liquid after treatment enters the recovery tank 80 from the liquid outlet of the alkali washing tower 70.

[0044] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A reaction apparatus for treating waste catalysts from solid carbide slag, characterized in that, include: Rack (11); The vessel body (12) is rotatably connected to the frame (11). The vessel body (12) has a mixing chamber (121) and an inlet (122) and an outlet (123) communicating with the mixing chamber (121). A liquid inlet pipe (13) extends at one end into a mixing chamber (121), and the liquid inlet pipe (13) is connected to a spray pipe (131); and A vacuum tube (14) extends into a mixing chamber (121) at one end. A filter (15) is connected to one end of the vacuum tube (14), and a vacuum pump (50) is connected to the other end of the vacuum tube (14). The filter (15) is placed above the spray tube (131). The vessel body (12) can rotate relative to the liquid inlet pipe (13) and the vacuum pipe (14).

2. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 1, characterized in that, The filter (15) includes: A cylindrical body (151) having a cavity (1511) connected to a vacuum tube (14), and a plurality of filter holes formed on the outer peripheral surface of the cylindrical body (151); and A baffle (152) is connected above the cylinder (151) and extends along the height direction of the cylinder (151). The lower end face of the baffle (152) has a gap with the outer peripheral surface of the cylinder (151).

3. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 2, characterized in that, The end face of the baffle (152) away from the cylinder (151) is an arc-shaped surface (1521).

4. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 1, characterized in that, It also includes a first rotating assembly (16), a second rotating assembly (17) and a drive assembly (18) mounted on a frame (11); the first rotating assembly (16) and the second rotating assembly (17) are respectively connected to the two ends of the vessel body (12), the drive assembly (18) is connected to the first rotating assembly (16), the vacuum tube (14) passes through the first rotating assembly (16) and the two can rotate relative to each other, and the liquid phase inlet pipe (13) passes through the second rotating assembly (17) and the two can rotate relative to each other.

5. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 4, characterized in that, The first rotating assembly (16) includes: The first bearing seat (161) is connected at one end to the vessel body (12); First bearing housing (163); mounted on frame (11), and The first rotating shaft (162) is installed in the first bearing seat (163) and one end is connected to the first bearing seat (161); The first rotating shaft (162) has a first guide channel for the vacuum tube (14) to pass through, the first shaft seat (161) has a first mounting hole for the vacuum tube (14) to pass through, and the drive assembly (18) is connected to the first rotating shaft (162).

6. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 4, characterized in that, The second rotating assembly (17) includes: The second shaft seat (171) has one end connected to the vessel body (12); Second bearing housing (173); mounted on frame (11), and The second rotating shaft (172) is installed inside the second bearing housing (173) and one end is connected to the second bearing housing (171); The second rotating shaft (172) has a second guide channel through which the liquid phase inlet pipe (13) passes, and the second shaft seat (171) has a second mounting hole through which the liquid phase inlet pipe (13) passes.

7. The reaction apparatus for treating waste catalyst in solid carbide slag according to claim 5, characterized in that, The driving component (18) includes: Motor (181) A speed reducer (182) is connected to a motor (181); The reducer (182) is connected to the first rotating shaft (162) via a belt (184).

8. A reaction system, characterized in that, It includes a waste catalyst storage tank (20), a transfer pump (40), a reaction device (10) as described in any one of claims 1-6, a vacuum pump (50), a water washing tower (60), an alkali washing tower (70), and a recovery tank (80) connected in sequence; the outlet end of the transfer pump (40) is connected to the inlet end of the liquid phase inlet pipe (13), and the outlet end of the vacuum pipe (14) is connected to the inlet end of the vacuum pump (50).

9. The reaction system according to claim 8, characterized in that, The vacuum pump (50) and water washing tower (60) device is also equipped with a total condenser (90), and the outlet of the total condenser (90) is connected to a collection tank (100).

10. The reaction system according to claim 8, characterized in that, The vacuum tube (14) is connected to a manifold (19), and a first control valve (191) is provided on the pipe connecting the manifold (19) and the vacuum pump (50); a backflush nitrogen pipe (193) is also connected to the manifold (19), and a second control valve (192) is provided on the backflush nitrogen pipe (193).

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