Device and method for removing MIBK (methyl isobutyl ketone) in raffinate for extracting and separating zirconium and hafnium

Abstract

The invention provides a device and a method for removing MIBK (methyl isobutyl ketone) in raffinate for extracting and separating zirconium and hafnium, the device comprises a tank body, a liquid distribution ring is fixedly connected in the tank body, one side of the liquid distribution ring penetrates through the tank body and is outwards communicated with a feeding pipe, a plurality of spray heads are arranged below the liquid distribution ring in a penetrating manner, the outer end of the tank body is fixedly connected with a bracket, and the bracket is fixedly connected with a rotating shaft. According to the device, raffinate can be quickly conveyed into the tank body by arranging a liquid distribution ring and a spray head, rotation of a rotating shaft and a rotating plate can be completed in cooperation with a gear assembly, the fallen raffinate is scattered, it is ensured that the raffinate can uniformly fall on a steam heating pipe, and the raffinate is uniformly heated; meanwhile, the contact area of the gas phase and the liquid phase can be increased in cooperation with the condensation assembly, the phase splitting barrel and the grid plate, the MIBK separation efficiency is improved, and the purpose of rapidly removing oil is achieved through the principle that the volatility is affected by factors such as liquid diffusion and temperature.

Description

Technical Field

[0001] The present invention relates to the technical field of MIBK extraction, and specifically to a device and method for removing MIBK from the raffinate in the extraction and separation of zirconium and hafnium. Background Art

[0002] In the process of extracting and separating zirconium (Zr) and hafnium (Hf) with MIBK (methyl isobutyl ketone), the raffinate refers to the remaining aqueous solution after extraction, which may contain a small amount of incompletely separated MIBK. Since MIBK is an organic solvent, direct discharge will cause environmental pollution and may affect subsequent processes (such as wastewater treatment or metal recovery), so it needs to be removed. Many methods for separating zirconium and hafnium have been studied at home and abroad, such as solvent extraction separation method. The main methods for removing oil from the MIBK extraction and separation system of zirconium and hafnium are rectification and distillation. The distillation method mainly includes an evaporator and a condenser, and the equipment structure is simple, but there are problems of poor production continuity and high energy consumption. Rectification includes structures such as a reboiler, a rectification column, and a condenser. The reboiler provides heat. In the rectification column, MIBK, a small amount of water, and trace entrained materials are vaporized from the raffinate. After being condensed by the condenser, MIBK is recovered, and the water and entrained materials are returned to the rectification column. The method is safe and environmentally friendly, but has high energy consumption and low processing efficiency. Summary of the Invention

[0003] (I) Technical Problems to be Solved Aiming at the deficiencies of the prior art, the present invention provides a device and method for removing MIBK from the raffinate in the extraction and separation of zirconium and hafnium, and solves the problems of poor production continuity and high energy consumption existing in the existing removal devices.

[0004] (II) Technical Solutions To achieve the above objectives, the present invention is realized through the following technical solutions: A device for removing MIBK from the raffinate in the extraction and separation of zirconium and hafnium, including a tank body. A liquid distribution ring is fixedly connected inside the tank body. One side of the liquid distribution ring penetrates through the tank body and communicates with a feed pipe outward. A plurality of nozzles are arranged through the lower part of the liquid distribution ring. A support is fixedly connected to the outer end of the tank body. One outer end of the support is fixedly connected to a fixing frame. A rotating shaft is rotatably connected to the middle part above the tank body, and the rotating shaft is rotatably connected to the fixing frame. A first gear is fixedly connected to the rotating shaft. One end of the upper part of the tank body is fixedly connected with a motor. The output end of the motor penetrates through the fixed frame and is fixedly connected with a second gear upwards. The first gear and the second gear are meshed with each other. A plurality of rotating plates are fixedly connected to the part of the rotating shaft inside the tank body. Three groups of first mounting blocks are fixedly connected to the part of the tank body close to the lower end of the bracket. A connecting tank is correspondingly installed at the lower end of the tank body. Three outer ends of the connecting tank are fixedly connected with second mounting blocks. A positioning bolt is threadedly connected inside the first mounting block and the second mounting block; Two inner ends of the connecting tank are provided with chutes. A second grid plate is correspondingly installed inside the connecting tank. A first grid plate is correspondingly arranged at the lower end of the second grid plate. A filter plate is correspondingly arranged at the lower end of the first grid plate. Two outer ends of the second grid plate, the first grid plate and the filter plate are fixedly connected with limit blocks. The limit blocks correspond to the chutes. A discharge pipe penetrates through the bottom of the connecting tank. An electromagnetic valve is installed inside the discharge pipe.

[0005] Preferably, a plurality of positioning grooves are formed inside the chute. A slot is formed inside the limit block.

[0006] Preferably, a spring is fixedly connected inside the slot. The other end of the spring is fixedly connected with a limit plate. The other end of the limit plate is fixedly connected with a positioning column. The positioning column penetrates through the limit block and corresponds to the positioning groove. Two inner ends of the slot are fixedly connected with sliding rods. The limit plate is slidably connected to the sliding rods.

[0007] Preferably, a positioning frame is fixedly connected to the middle part of the inner side of the tank body. A steam heating pipe is fixedly connected to the upper end of the positioning frame. Both ends of the steam heating pipe penetrate through the tank body.

[0008] Preferably, two groups of mounting frames are fixedly connected to the other end of the outer side of the tank body. A phase separation barrel is fixedly connected inside the mounting frames.

[0009] Preferably, a condenser is fixedly connected inside the upper mounting frame. The other end of the connecting pipe penetrates through the upper part of the tank body. The other end of the connecting pipe penetrates through the inside of the condenser. The condenser is communicated with the phase separation barrel.

[0010] Preferably, a three-way pipe penetrates through the bottom of the phase separation barrel.

[0011] The method for removing MIBK from the raffinate in the extraction and separation of zirconium and hafnium includes the following removal methods: S1. Feed the raffinate into the interior of the cloth ring through the feed pipe and spray it downward through a number of nozzles below. At this time, starting the motor can drive the second gear to rotate. Under the meshing action, it can drive the first gear and the rotating shaft to rotate. Under the action of the rotating shaft, a number of internal rotating plates can be driven to rotate, breaking up the falling raffinate to ensure that the raffinate can evenly fall on the steam heating pipe, expanding its heating effect. S2. Connect the inlet and outlet ends of the steam heating pipe to an external steam device, so that hot steam enters the interior of the steam heating pipe to heat the internal cavity of the tank, improving the stability of heating. S3. After the raffinate is heated by the steam heating pipe, the bubbles generated by the two grid plates quickly separate the MIBK in the raffinate from the liquid phase. The volatilized MIBK, water vapor, and a small amount of entrained materials are quickly liquefied inside the condenser. The organic phase MIBK returns to the separation system, and the water and a small amount of entrained materials return to the oil removal device. Under the action of the rotating component, heating component, and grid plate, the contact area between the gas and liquid phases is increased, accelerating the MIBK separation efficiency. Based on the principle of the influence of factors such as liquid diffusion and temperature on volatility, the purpose of rapid oil removal is achieved.

[0012] Working principle: During use, feed the raffinate into the interior of the cloth ring 25 through the feed pipe 16 and spray it downward through a number of nozzles 36 below. At this time, starting the motor 15 can drive the second gear 14 to rotate. Under the meshing action, it can drive the first gear 12 and the rotating shaft 13 to rotate. Under the action of the rotating shaft 13, a number of internal rotating plates 24 can be driven to rotate, breaking up the falling raffinate to ensure that the raffinate can evenly fall on the steam heating pipe 17, expanding its heating effect. Connect the inlet and outlet ends of the steam heating pipe 17 to an external steam device, so that hot steam enters the interior of the steam heating pipe 17 to heat the internal cavity of the tank 1, improving the stability of heating. After the raffinate is heated by the steam heating pipe 17, the bubbles generated by the two grid plates quickly separate the MIBK in the raffinate from the liquid phase. The volatilized MIBK, water vapor, and a small amount of entrained materials are quickly liquefied inside the condenser 10. The organic phase MIBK returns to the separation system, and the water and a small amount of entrained materials return to the oil removal device. Under the action of the rotating component, heating component, and grid plate, the contact area between the gas and liquid phases is increased, accelerating the MIBK separation efficiency. Based on the principle of the influence of factors such as liquid diffusion and temperature on volatility, the purpose of rapid oil removal is achieved. When it is necessary to disassemble and replace the grid plate and the filter plate 20, turn the positioning bolt 19 so that the two mounting blocks are disengaged. At this time, the staff can take out the connecting tank 3 from below the tank body 1. Then, press the limiting plates 31 in the limiting blocks 29 at both ends of the second grid plate 22 inward. Under the action of the spring 30, the limiting plates 31 can drive the positioning columns 33 to move inward. At this time, the positioning columns 33 are disengaged from the positioning grooves 27, and the staff can directly pull the second grid plate 22 upward to take it out and replace it. The first grid plate 21 and the filter plate 20 can be disassembled and replaced in the same way, improving the use effect of the entire removal device.

[0013] (III) Beneficial effects The present invention provides a device and method for removing MIBK from the raffinate of extracting and separating zirconium and hafnium. It has the following beneficial effects: 1. By setting the liquid distribution ring and the spray head, the present invention can quickly transport the raffinate into the tank body. Cooperating with the gear assembly, it can complete the rotation of the rotating shaft and the rotating plate, break up the falling raffinate, ensure that the raffinate can evenly fall on the steam heating pipe, expand its heating effect, and at the same time, cooperating with the condensation assembly, the phase separation bucket and the grid plate can increase the contact area between the gas and liquid phases, accelerate the MIBK separation efficiency, and achieve the purpose of quickly removing oil through the principle of the influence of factors such as liquid diffusion and temperature on volatility.

[0014] 2. By setting the first mounting block, the second mounting block and the positioning bolt, the present invention can quickly disassemble and assemble the connecting tank, and the grid plate and the filter plate inside the connecting tank can also be quickly disassembled and assembled, thereby improving the use effect of the entire device.

[0015] 3. By setting a chute inside the connecting tank, the present invention can correspond to the limiting blocks on the grid plate and the filter plate, and at the same time, the internal positioning assembly can cooperate with the positioning groove to achieve the effect of quick disassembly. Brief description of the drawings

[0016] Figure 1 is the front view of the device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium proposed by the present invention; Figure 2 is the cross-sectional view of the device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium proposed by the present invention; Figure 3 is the schematic diagram of the connecting tank of the device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium proposed by the present invention; Figure 4 is the schematic diagram of the grid plate of the device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium proposed by the present invention; Figure 5 is the schematic diagram of the liquid distribution ring of the device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium proposed by the present invention.

[0017] Among them, 1. tank body; 2. fixing frame; 3. connecting tank; 4. discharge pipe; 5. solenoid valve; 6. support; 7. tee; 8. mounting frame; 9. phase separation barrel; 10. condenser; 11. connecting pipe; 12. first gear; 13. rotating shaft; 14. second gear; 15. motor; 16. feed pipe; 17. steam heating pipe; 18. first mounting block; 19. positioning bolt; 20. filter plate; 21. first grid plate; 22. second grid plate; 23. positioning frame; 24. rotating plate; 25. liquid distribution ring; 26. chute; 27. positioning groove; 28. second mounting block; 29. limiting block; 30. spring; 31. limiting plate; 32. sliding rod; 33. positioning column; 34. slot; 36. spray head. Specific implementation manner

[0018] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0019] Embodiment: As Figures 1-5 shown, the embodiment of the present invention provides a device for removing MIBK from the raffinate of extracting and separating zirconium and hafnium, including a tank body 1. A liquid distribution ring 25 is fixedly connected inside the tank body 1. One side of the liquid distribution ring 25 penetrates through the tank body 1 and communicates outward with a feed pipe 16. A plurality of spray heads 36 are arranged through the lower part of the liquid distribution ring 25. The feed pipe 16 can send the raffinate into the inside of the liquid distribution ring 25 and spray it downward through the spray heads 36. The spray heads 36 are arranged around the liquid distribution ring 25, and can achieve the effect of uniform spraying. A support 6 is fixedly connected to the outer end of the tank body 1. One outer end of the support 6 is fixedly connected to a fixing frame 2. The middle part above the tank body 1 is rotatably connected with a rotating shaft 13, and the rotating shaft 13 is rotatably connected to the fixing frame 2. A first gear 12 is fixedly connected to the rotating shaft 13. The rotating shaft 13 can drive the first gear 12 and a plurality of groups of rotating plates 24 inside to rotate; One end above the tank body 1 is fixedly connected with a motor 15. The output end of the motor 15 penetrates through the fixed frame 2 and is fixedly connected with a second gear 14 upward. The first gear 12 meshes with the second gear 14. A plurality of rotating plates 24 are fixedly connected to the part of the rotating shaft 13 located inside the tank body 1. Three groups of first mounting blocks 18 are fixedly connected to the part of the tank body 1 close to the lower end of the bracket 6. A connecting tank 3 is correspondingly installed at the lower end of the tank body 1. Three outer ends of the connecting tank 3 are fixedly connected with second mounting blocks 28. A positioning bolt 19 is threadedly connected inside the first mounting block 18 and the second mounting block 28. Starting the motor 15 can drive the second gear 14 to rotate. Under the meshing action, it can drive the first gear 12 and the rotating shaft 13 to rotate. Under the action of the rotating shaft 13, it can drive a plurality of internal rotating plates 24 to rotate, so as to disperse the falling raffinate liquid, ensure that the raffinate liquid can evenly fall on the steam heating pipe 17, expand its heating effect, and the connecting tank 3 can be disassembled and assembled under the action of the first mounting block 18, the second mounting block 28 and the positioning bolt 19, which is convenient for the staff to maintain and repair the internal components; Chutes 26 are opened at both inner ends of the connecting tank 3. A second grid plate 22 is correspondingly installed inside the connecting tank 3. A first grid plate 21 is correspondingly arranged at the lower end of the second grid plate 22. A filter plate 20 is correspondingly arranged at the lower end of the first grid plate 21. Limiting blocks 29 are fixedly connected to both outer ends of the second grid plate 22, the first grid plate 21 and the filter plate 20. The limiting blocks 29 correspond to the chutes 26. A discharge pipe 4 penetrates through the bottom of the connecting tank 3. An electromagnetic valve 5 is installed inside the discharge pipe 4. By setting the limiting blocks 29 to correspond to the chutes 26, it is convenient for the quick installation of the second grid plate 22, the first grid plate 21 and the filter plate 20. At the same time, the bottom discharge pipe 4 is controlled by the electromagnetic valve 5 to open and close; A number of positioning grooves 27 are opened inside the chutes 26. An opening groove 34 is opened inside the limiting block 29. A spring 30 is fixedly connected inside the opening groove 34. The other end of the spring 30 is fixedly connected with a limiting plate 31. The other end of the limiting plate 31 is fixedly connected with a positioning post 33. The positioning post 33 penetrates through the limiting block 29 and corresponds to the positioning groove 27. Slide rods 32 are fixedly connected to both inner ends of the opening groove 34. The limiting plate 31 is slidably connected to the slide rods 32. When it is necessary to disassemble and replace the grid plate and the filter plate 20, turn the positioning bolt 19 to separate the two mounting blocks. At this time, the staff can take out the connecting tank 3 from below the tank body 1. Then, press the limiting plate 31 in the limiting blocks 29 at both ends of the second grid plate 22 inward. Under the action of the spring 30, the limiting plate 31 can drive the positioning post 33 to move inward. At this time, the positioning post 33 disengages from the positioning groove 27. The staff can directly pull up the second grid plate 22 to take it out and replace it. The first grid plate 21 and the filter plate 20 can be disassembled and replaced in the same way, improving the use effect of the whole removal device; In the middle of the inner side of the tank body 1, a positioning frame 23 is fixedly connected. At the upper end of the positioning frame 23, a steam heating pipe 17 is fixedly connected. Both ends of the steam heating pipe 17 penetrate through the tank body 1. The inlet and outlet ends of the steam heating pipe 17 are connected to external steam equipment, so that hot steam enters the interior of the steam heating pipe 17 to heat the internal cavity of the tank body 1, improving the stability of heating. On the other end of the outer side of the tank body 1, two mounting frames 8 are fixedly connected. Inside the mounting frames 8, a phase separation barrel 9 is fixedly connected. Inside the upper mounting frame 8, a condenser 10 is fixedly connected. On the other end above the tank body 1, a connecting pipe 11 penetrates through. The other end of the connecting pipe 11 penetrates through the interior of the condenser 10, and the condenser 10 is communicated with the phase separation barrel 9. At the bottom of the phase separation barrel 9, a three-way pipe 7 penetrates through. After the raffinate is heated by the steam heating pipe 17, the MIBK in the raffinate is quickly separated from the liquid phase by the bubbles generated by the two grid plates. The volatilized MIBK, water vapor, and a small amount of entrained materials are quickly liquefied inside the condenser 10. The organic phase MIBK returns to the separation system, and the water and a small amount of entrained materials return to the oil removal device. Under the action of the rotating assembly, heating assembly, and grid plates, the contact area between the gas and liquid phases is increased, accelerating the MIBK separation efficiency. According to the principle of the influence of factors such as liquid diffusion and temperature on volatility, the purpose of quickly removing oil is achieved.

[0020] A method for removing MIBK from the raffinate in the extraction and separation of zirconium and hafnium includes the following removal methods: S1: Feed the raffinate into the interior of the cloth ring 25 through the feed pipe 16 and spray it downward through a number of nozzles 36 below. At this time, starting the motor 15 can drive the second gear 14 to rotate. Under the meshing action, it can drive the first gear 12 and the rotating shaft 13 to rotate. Under the action of the rotating shaft 13, a number of rotating plates 24 inside can be driven to rotate, dispersing the falling raffinate to ensure that the raffinate can evenly fall on the steam heating pipe 17, expanding its heating effect. S2: Connect the inlet and outlet ends of the steam heating pipe 17 to external steam equipment, so that hot steam enters the interior of the steam heating pipe 17 to heat the internal cavity of the tank body 1, improving the stability of heating. S3: After the raffinate is heated by the steam heating pipe 17, the MIBK in the raffinate is quickly separated from the liquid phase by the bubbles generated by the two grid plates. The volatilized MIBK, water vapor, and a small amount of entrained materials are quickly liquefied inside the condenser 10. The organic phase MIBK returns to the separation system, and the water and a small amount of entrained materials return to the oil removal device. Under the action of the rotating assembly, heating assembly, and grid plates, the contact area between the gas and liquid phases is increased, accelerating the MIBK separation efficiency. According to the principle of the influence of factors such as liquid diffusion and temperature on volatility, the purpose of quickly removing oil is achieved.

[0021] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An MIBK removal device for raffinate in the extraction and separation of zirconium and hafnium, comprising a tank body (1), characterized in that: Inside the tank body (1), a liquid distribution ring (25) is fixedly connected. One side of the liquid distribution ring (25) penetrates through the tank body (1) and communicates outward with a feed pipe (16). A number of spray nozzles (36) are arranged through the lower part of the liquid distribution ring (25). The outer end of the tank body (1) is fixedly connected with a support (6). One outer end of the support (6) is fixedly connected with a fixing frame (2). In the middle of the upper part of the tank body (1), a rotating shaft (13) is rotatably connected, and the rotating shaft (13) is rotatably connected to the fixing frame (2). A first gear (12) is fixedly connected to the rotating shaft (13); One end of the upper part of the tank body (1) is fixedly connected with a motor (15). The output end of the motor (15) penetrates through the fixing frame (2) and is fixedly connected upward with a second gear (14). The first gear (12) meshes with the second gear (14). A number of rotating plates (24) are fixedly connected to the part of the rotating shaft (13) inside the tank body (1). Three groups of first mounting blocks (18) are fixedly connected to the part of the tank body (1) near the lower end of the support (6). A connecting tank (3) is correspondingly installed at the lower end of the tank body (1). Three outer ends of the connecting tank (3) are fixedly connected with second mounting blocks (28). A positioning bolt (19) is threadedly connected inside the first mounting block (18) and the second mounting block (28); Chutes (26) are opened at both inner ends of the connecting tank (3). A second grid plate (22) is correspondingly installed inside the connecting tank (3). A first grid plate (21) is correspondingly arranged at the lower end of the second grid plate (22). A filter plate (20) is correspondingly arranged at the lower end of the first grid plate (21). Limiting blocks (29) are fixedly connected to both outer ends of the second grid plate (22), the first grid plate (21) and the filter plate (20). The limiting blocks (29) correspond to the chutes (26). A discharge pipe (4) penetrates through the bottom of the connecting tank (3). A solenoid valve (5) is installed inside the discharge pipe (4).

2. The MIBK removal device for the raffinate of extracting and separating zirconium and hafnium according to claim 1, characterized in that: A number of positioning grooves (27) are opened inside the chutes (26). A slot (34) is opened inside the limiting block (29).

3. The MIBK removal device for the raffinate of extracting and separating zirconium and hafnium according to claim 2, wherein: A spring (30) is fixedly connected inside the slot (34). The other end of the spring (30) is fixedly connected with a limiting plate (31). The other end of the limiting plate (31) is fixedly connected with a positioning post (33). The positioning post (33) penetrates through the limiting block (29) and corresponds to the positioning groove (27). Slide rods (32) are fixedly connected to both inner ends of the slot (34). The limiting plate (31) is slidably connected to the slide rods (32).

4. The MIBK removal device for the raffinate obtained by extracting and separating zirconium and hafnium according to claim 1, characterized in that: A positioning frame (23) is fixedly connected to the middle part of the inner side of the tank body (1). A steam heating pipe (17) is fixedly connected to the upper end of the positioning frame (23), and both ends of the steam heating pipe (17) penetrate through the tank body (1).

5. The MIBK removal device for the raffinate of zirconium and hafnium extraction and separation according to claim 1, characterized in that: Two groups of mounting frames (8) are fixedly connected to the other outer end of the tank body (1). A phase separation barrel (9) is fixedly connected inside the mounting frame (8).

6. The MIBK removal device for the raffinate in the extraction and separation of zirconium and hafnium according to claim 5, characterized in that: Inside the upper mounting bracket (8) described above, a condenser (10) is fixedly connected. At the other end above the tank body (1), a connecting pipe (11) is penetrated. The other end of the connecting pipe (11) is penetrated inside the condenser (10), and the condenser (10) is communicated with the phase separation tank (9).

7. The MIBK removal device for the raffinate of zirconium and hafnium extraction and separation according to claim 5, characterized in that: At the bottom of the phase separation tank (9), a three-way pipe (7) is penetrated.

8. Method for removing MIBK from raffinate in extraction and separation of zirconium and hafnium, characterized in that, It includes the following removal methods: S1. Send the raffinate into the inside of the cloth ring (25) through the feed pipe (16) and spray it downward through a number of nozzles (36) below. At this time, starting the motor (15) can drive the gear two (14) to rotate. Under the meshing action, it can drive the gear one (12) and the rotating shaft (13) to rotate. Under the action of the rotating shaft (13), a number of internal rotating plates (24) can be driven to rotate, so as to disperse the falling raffinate and ensure that the raffinate can evenly fall on the steam heating pipe (17) to expand its heating effect. S2. Connect the inlet and outlet ends of the steam heating pipe (17) to an external steam device, so that hot steam enters the inside of the steam heating pipe (17) to heat the internal cavity of the tank body (1) and improve the heating stability. After the raffinate is heated by the steam heating pipe (17), the MIBK in the raffinate is quickly separated from the liquid phase through the bubbles generated by the two grid plates. The volatilized MIBK, water vapor and a small amount of entrained materials are quickly liquefied inside the condenser (10). The organic phase MIBK returns to the separation system, and the water and a small amount of entrained materials return to the oil removal device. Under the action of the rotating assembly, the heating assembly and the grid plate, the contact area between the gas and liquid phases is increased, and the MIBK separation efficiency is accelerated. Through the principle of the influence of factors such as liquid diffusion and temperature on volatility, the purpose of quickly removing oil is achieved.

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