Rectification tower for producing electronic grade hydrofluoric acid

Abstract

The application relates to a rectifying tower for producing electronic-grade hydrogen fluoride. The rectifying tower for producing electronic-grade hydrogen fluoride comprises a tower body, a plurality of tower plates arranged in the tower body, overflow weirs and a plurality of air inlets arranged on the tower plates, a liquid lifting pipe arranged on each air inlet, a filler assembly arranged on the upper side of the liquid lifting pipe, a sealing box arranged on the left and right sides of the liquid lifting pipe, a liquid inlet communicated with the sealing box and arranged on the left and right sides of the lower end of the liquid lifting pipe, a communication hole arranged on the sealing box and used for feeding liquid into the sealing box, a first one-way valve arranged in the liquid inlet and used for feeding liquid into the liquid lifting pipe, a second one-way valve arranged in the communication hole and used for feeding liquid into the sealing box, a turbine rotatably arranged in the liquid lifting pipe, a rotating shaft of the turbine extending outward to the upper side of the sealing box, and a first magnet fixedly connected to the end of the turbine. The application avoids the problem that high-speed gas in the liquid lifting pipe flows to the outside of the liquid lifting pipe through the liquid inlet, thereby reducing the liquid flow speed into the liquid lifting pipe, and realizes stable and continuous liquid feeding into the liquid lifting pipe.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of rectifying column, and particularly relates to a rectifying column for production of electronic-grade hydrofluoric acid. BACKGROUND

[0002] Electronic-grade hydrofluoric acid is a strong acid cleaning agent and a corrosive agent, and is mainly used for production of ultra-large scale integrated circuits. The rectifying method is a commonly used method for preparing electronic-grade hydrofluoric acid, and the rectifying column is an important device in the method.

[0003] At present, the rectifying column mainly includes a packed rectifying column and a plate rectifying column. The packed rectifying column is a continuous gas-liquid mass transfer device, and gas-liquid two phases are in continuous countercurrent contact and mass transfer and heat transfer, and the concentration of gas-liquid two phases changes continuously along the height of the column. In the plate rectifying column, gas-liquid two phases are in countercurrent contact layer by layer and mass transfer and heat transfer, and the concentration of gas-liquid two phases changes in a stepwise manner along the height of the column. The packed rectifying column has simple structure, small pressure drop, and is convenient for processing corrosive materials, materials prone to foaming, and vacuum operation, but has large volume, large weight, low mass transfer efficiency, and poor operation stability, and is not suitable for processing turbid liquid, dust-containing gas, and substances containing solid particles and prone to fouling. The plate rectifying column performs mass transfer and heat transfer through stratification, and gas-liquid two phases must be kept in close and sufficient contact on each tray to provide a large and constantly updated phase contact surface for the mass transfer process, reduce the mass transfer resistance, and make gas-liquid two phases flow in countercurrent as much as possible to provide the maximum mass transfer power.

[0004] With the increasing requirement for the purity of electronic-grade hydrofluoric acid, the traditional packed rectifying column and plate rectifying column cannot meet the demand of gas-liquid mass transfer. On this basis, a parallel jet packed tray appears in the prior art. The parallel jet packed tray is a combination of packing and tray, relies on the packing to realize mass transfer, and relies on the tray to realize multi-stage parallel flow. The liquid on the tray is lifted by the gas through the gap between the liquid lifting pipe and the tray, and the gas-liquid flows in parallel through the liquid lifting pipe, and then is mixed and mass transferred at high speed in the liquid lifting pipe, and then enters the packing to further strengthen the mass transfer and complete the gas-liquid separation. The gas continues to rise by pressure difference and enters the upper tray. The liquid basically returns to the tray in the form of clear liquid, enters the downcomer along the flow channel, and then falls to the lower tray. However, the high-speed gas in the liquid lifting pipe reduces the flow speed of the liquid flowing through the gap to the liquid lifting pipe, and the rectifying efficiency is reduced. In addition, a certain amount of liquid is still carried out of the packing with the gas, the liquid separated from the gas is returned to the rectifying column after the gas flows out of the rectifying column, and the parallel jet packed tray does not have a structure for separating the gas flowing out of the packing. Therefore, in order to ensure that the liquid can flow to the liquid lifting pipe and at the same time separate the gas flowing out of the packing, the prior art needs to be further improved. SUMMARY

[0005] In order to achieve the above object, the present application provides a kind of electronic grade hydrofluoric acid production with rectifying column.

[0006] The technical scheme of one kind of electronic grade hydrofluoric acid production with rectifying column of the present application is:

[0007] A kind of electronic grade hydrofluoric acid production with rectifying column, including tower body, the tower body is equipped with several tower plates arranged from top to bottom, the tower plate is equipped with overflow weir and several gas inlets, each the gas inlet is equipped with liquid lifting pipe respectively, the upper side of the liquid lifting pipe is equipped with packing assembly, the left and right sides of the liquid lifting pipe are respectively equipped with the sealing box fixedly connected with the tower plate, the left and right sides of the lower end of the liquid lifting pipe are respectively equipped with the liquid inlet communicated with the sealing box, the sealing box is equipped with the communication hole for liquid into the sealing box, the liquid inlet is equipped with the first one-way valve for liquid into the liquid lifting pipe, the communication hole is equipped with the second one-way valve for liquid into the sealing box, the liquid lifting pipe is rotatably installed with turbine, the rotating shaft of the turbine extends to the upper side of the sealing box, the end of the turbine is fixedly connected with the first magnet, the two magnetic poles of the first magnet are located at the upper and lower ends respectively, the sealing box is guided and sealedly installed with the movable plate moving up and down, the sealing box is equipped with the communication pipe communicated with the inside of the sealing box on the upper side of the movable plate, the upper side of the movable plate is fixedly connected with the second magnet, the two magnetic poles of the second magnet are located at the upper and lower ends respectively.

[0008] Further, the two sides of the packing assembly are respectively equipped with baffle, the side away from the packing assembly of the baffle is equipped with connecting plate, the sealing box is equipped with fixed rod, the connecting plate is equipped with guide hole matched with the fixed rod, the connecting plate is equipped with upper flange and lower flange respectively located at the upper and lower sides of the connecting plate, two springs are sleeved on the fixed rod, the two ends of one spring are fixedly connected with the upper flange and the connecting plate respectively, the two ends of the other spring are fixedly connected with the lower flange and the connecting plate respectively, the lower side of the connecting plate is equipped with the third magnet, the two magnetic poles of the third magnet are located at the upper and lower ends respectively.

[0009] Further, the magnetic poles of the two first magnets at the upper and lower ends are same, the magnetic poles of the two second magnets at the upper and lower ends are opposite, the magnetic poles of the two third magnets at the upper and lower ends are same.

[0010] Further, the cross section of the baffle is arrow-shaped, and the tip of the baffle faces the packing assembly.

[0011] Further, the side away from the liquid lifting pipe of the sealing box is equipped with preheating box, the preheating box is equipped with liquid inlet hole, the preheating box is equipped with heat exchange plate, the heat exchange plate is hollow structure, the lower end of the heat exchange plate has opening communicated with the inside of the heat exchange plate, the heat exchange plate is sealingly fixedly connected on the tower plate, and the lower end of the heat exchange plate penetrates out of the tower plate downward.

[0012] Further, the filler assembly comprises a fixed frame and fillers filled in the fixed frame, the fixed frame comprises a top plate, a front side plate, a rear side plate, a lower support net, a left support net and a right support net, the top plate, the front side plate and the rear side plate are welded and fixed, the lower support net is fixedly connected with the front side plate, the rear side plate and the liquid lifting pipe respectively, and the left support net and the right support net are fixedly connected with the top plate, the front side plate, the rear side plate and the liquid lifting pipe respectively.

[0013] The electronic-grade hydrofluoric acid production rectifying tower has the beneficial effects that:

[0014] The electronic-grade hydrofluoric acid production rectifying tower avoids the problem that the high-speed gas in the liquid lifting pipe flows to the outside of the liquid lifting pipe through the liquid inlet, thereby reducing the flow speed of the liquid into the liquid lifting pipe, the high-speed gas drives the turbine to rotate, the turbine drives the magnet to rotate, the movable plate in the sealing box reciprocates up and down, the liquid is sucked into the sealing box and the liquid in the sealing box is squeezed into the liquid lifting pipe, and stable flow of the liquid into the liquid lifting pipe is realized.

[0015] By arranging the baffle, gas-liquid separation of the gas flowing out of the filler assembly is realized. The baffle can swing up and down under the action of the magnetic force, and the liquid on the baffle is shaken off, thereby avoiding the problem that a large amount of liquid is attached to the baffle, and the gas-liquid separation effect is poor.

[0016] By arranging the preheating box and arranging the heat exchange plate in the preheating box, the liquid entering the sealing box is preheated in the preheating box, the temperature of the liquid entering the sealing box is increased, and the temperature of the liquid entering the liquid lifting pipe and the gas-liquid fluid entering the filler assembly is increased, thereby improving the mass transfer effect of the gas-liquid fluid and the filler. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 is a structural schematic diagram of the electronic-grade hydrofluoric acid production rectifying tower of the embodiment of the present application;

[0018] Figure 2 is Figure 1 is an enlarged view of A in FIG. 4;

[0019] Figure 3 is a partial structural schematic diagram of the embodiment of the present application with a baffle;

[0020] Figure 4 is Figure 3 is an enlarged view of B in FIG. 5;

[0021] Figure 5 is a partial structural schematic diagram of the embodiment of the present application with a preheating box;

[0022] In the diagram: 1. Tower body; 2. Tower plate; 3. Feed pipe; 4. Liquid outlet pipe; 5. Air inlet pipe; 6. Air outlet pipe; 7. Reflux pipe; 8. Overflow weir; 9. Air inlet; 10. Liquid lifting pipe; 11. First check valve; 12. Sealing box; 13. Second check valve; 14. Movable plate; 15. Turbine; 16. First magnet; 17. Connecting pipe; 18. Second magnet; 19. Packing assembly; 20. Fixing rod; 21. Baffle; 22. Connecting plate; 23. Upper flange; 24. Lower flange; 25. Spring; 26. Third magnet; 27. Preheating box; 28. Liquid inlet; 29. ​​Heat exchange plate. Detailed Implementation

[0023] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments:

[0024] Specific embodiments of the distillation column for producing electronic-grade hydrofluoric acid of the present invention are as follows: Figure 1 , Figure 2 As shown, the tower includes a tower body 1, which is equipped with a feed pipe 3, a liquid outlet pipe 4, a reflux pipe 7, an air inlet pipe 5, and an air outlet pipe 6. The feed pipe 3 is welded to the upper middle position on one side of the tower body 1, the air inlet pipe is welded to the lower end position on one side of the tower body 1, and the reflux pipe 7 is welded to the upper end position on the other side of the tower body 1. The liquid outlet pipe 4 is welded to the center position at the lower end of the tower body 1, and the air outlet pipe 6 is welded to the center position at the upper end of the tower body 1.

[0025] Specifically, several tower plates 2 arranged from top to bottom are welded inside the tower body 1. Each tower plate 2 is equipped with an overflow weir 8 and several air inlets 9. Each air inlet 9 is fixedly connected to a liquid lifting pipe 10. A packing assembly 19 is installed on the upper side of the liquid lifting pipe 10. Sealing boxes 12, fixedly connected to the tower plate 2 and the liquid lifting pipe 10, are located on the left and right sides of the liquid lifting pipe 10, respectively. Liquid inlets connecting the sealing boxes 12 and the liquid lifting pipe 10 are located on the left and right sides of the lower end of the liquid lifting pipe 10, respectively. A connecting hole is opened on the side of the sealing box 12 away from the liquid lifting pipe 10, located on the lower side of the sealing box 12, to allow liquid to enter the sealing box 12 through the connecting hole. A first one-way valve 11 is provided in the liquid inlet to allow liquid to enter the liquid lifting pipe 10, and a second one-way valve 13 is provided in the connecting hole to allow liquid to enter the sealing box 12. The first one-way valve 11 and the second one-way valve 13 achieve unidirectional liquid flow in the liquid inlet and the connecting hole.

[0026] A turbine 15 is rotatably installed in the liquid lifting pipe 10 through a bearing, and is located at the center of the liquid lifting pipe 10. The axis of the rotating shaft of the turbine 15 extends in the left-right direction, and the rotating shaft of the turbine 15 extends outward at both left and right ends to the upper side of the sealed box 12. The end of the turbine 15 is fixedly connected with a first magnet 16, and the two magnetic poles of the first magnet 16 are located at the upper and lower ends, respectively. A movable plate 14 moving up and down is sealingly installed in the sealed box 12. The sealed box 12 is provided with a communication pipe 17 communicating with the sealed box 12 at the upper side of the movable plate 14. The upper side of the movable plate 14 is fixedly connected with a second magnet 18, and the two magnetic poles of the second magnet 18 are located at the upper and lower ends, respectively.

[0027] When the distillation column for producing electronic grade hydrofluoric acid is used, the gas enters the liquid lifting pipe 10 from the gas inlet hole 9 of the tray 2, and the first one-way valve 11 prevents the gas from flowing into the sealed box 12. The gas drives the turbine 15 to rotate, and the first magnet 16 at both ends of the turbine 15 rotates. The magnetic pole of the end of the first magnet 16 close to the sealed box 12 alternately changes. When the magnetic pole of the first magnet 16 is opposite to the magnetic pole of the upper end of the second magnet 18 at the upper side of the movable plate 14, the movable plate 14 moves upward under the action of the magnetic force, and the liquid flows into the sealed box 12 through the second one-way valve 13. When the magnetic pole of the first magnet 16 is the same as the magnetic pole of the upper end of the second magnet 18 at the upper side of the movable plate 14, the movable plate 14 moves downward under the action of the magnetic force, and the liquid in the sealed box 12 flows into the liquid lifting pipe 10 through the first one-way valve 11. The liquid entering the liquid lifting pipe 10 is carried by the gas, enters the packing assembly 19, and exchanges heat and mass with the packing, and gas-liquid separation is realized.

[0028] The distillation column for producing electronic grade hydrofluoric acid avoids the problem that the high-speed gas in the liquid lifting pipe 10 flows out of the liquid lifting pipe 10 through the liquid inlet, thereby reducing the flow speed of the liquid into the liquid lifting pipe 10. The high-speed gas drives the turbine 15 to rotate, and the turbine 15 drives the first magnet 16 to rotate. The movable plate 14 in the sealed box 12 reciprocates up and down under the magnetic force between the first magnet 16 and the second magnet 18, sucks the liquid into the sealed box 12, and squeezes the liquid in the sealed box 12 into the liquid lifting pipe 10, thereby realizing stable flow of the liquid into the liquid lifting pipe 10.

[0029] In some embodiments, the magnetic poles at the upper and lower ends of the two first magnets 16 are the same, and the magnetic poles at the upper and lower ends of the two second magnets 18 are opposite. The magnetic poles at the upper and lower ends of the two second magnets 18 are opposite, and the directions of movement of the two movable plates 14 are opposite during the rotation of the first magnet 16, so that the liquid inlet time of the liquid inlets on both sides of the liquid lifting pipe 10 is opposite, thereby realizing continuous liquid inlet into the liquid lifting pipe 10.

[0030] In some embodiments, as shown in FIG. 5, the magnetic poles at the upper and lower ends of the two first magnets 16 are opposite, and the magnetic poles at the upper and lower ends of the two second magnets 18 are the same. Figure 3 , Figure 4As shown, the two sides of the filler assembly 19 are respectively provided with baffles 21, the cross section of the baffle 21 is arrow-shaped, the tip of the baffle 21 is towards the filler assembly 19. The center position of the side of the baffle 21 away from the filler assembly 19 is fixedly connected with a connecting plate 22, the upper side of the sealing box 12 is fixedly connected with a fixed rod 20, the connecting plate 22 has a guide hole matched with the fixed rod 20 on the connecting plate 22, and the connecting plate 22 is sleeved on the fixed rod 20 through the guide hole. The connecting plate 22 has an upper flange 23 and a lower flange 24 located on the upper and lower sides of the connecting plate 22 respectively, and the fixed rod 20 is sleeved with two springs 25, one end of one of the springs 25 is fixedly connected with the upper flange 23 and the connecting plate 22 respectively, and the other end of the other spring 25 is fixedly connected with the lower flange 24 and the connecting plate 22 respectively. The lower side of the connecting plate 22 is fixedly connected with a third magnet 26, and the two magnetic poles of the third magnet 26 are located at the upper and lower ends respectively.

[0031] When the electronic grade hydrofluoric acid production rectifying tower of the embodiment of the present application is used, the liquid drop gas carried out from the support net is separated from the baffle 21. The baffle 21 shakes up and down under the action of the magnetic force of the third magnet 26 on the connecting plate 22 and the rotating first magnet 16 and the two springs 25, and the liquid drops on the baffle 21 are shaken off, thereby avoiding the problem that a large amount of liquid is attached to the baffle 21, and the gas-liquid separation effect is poor.

[0032] In some embodiments, as shown in Figure 5 As shown, the side of the sealing box 12 away from the liquid lifting pipe 10 is fixedly connected with a preheating box 27, the communication hole is communicated with the preheating box 27, and the lower end of the side of the preheating box 27 away from the sealing box 12 is provided with a liquid inlet hole 28, so that the liquid on the tray plate 2 can enter the preheating box 27. The preheating box 27 has a heat exchange plate 29, the heat exchange plate 29 is a hollow structure, the lower end of the heat exchange plate 29 has an opening communicated with the inside of the heat exchange plate 29, the heat exchange plate 29 is sealingly and fixedly connected to the tray plate 2, and the lower end of the heat exchange plate 29 penetrates out of the tray plate 2 downward. The high-temperature gas on the lower side of the tray plate 2 can enter the hollow structure of the heat exchange plate 29, so that the heat exchange plate 29 can maintain a high temperature.

[0033] When the electronic grade hydrofluoric acid production rectifying tower of the embodiment of the present application is used, the liquid entering the preheating box 27 exchanges heat with the heat exchange plate 29, and the temperature of the liquid increases. The liquid with the increased temperature enters the sealing box 12 under the action of the movable plate 14, thereby increasing the temperature of the liquid entering the sealing box 12, and further increasing the temperature of the liquid entering the liquid lifting pipe 10 and the gas-liquid flow entering the filler assembly 19, and improving the mass transfer effect of the gas-liquid flow and the filler.

[0034] In some embodiments, the filler assembly 19 comprises a fixed frame and fillers filled in the fixed frame, the fixed frame comprises a top plate, a front side plate, a rear side plate, a lower support net, a left support net and a right support net, the top plate, the front side plate and the rear side plate are welded and fixed, the lower support net is fixedly connected with the front side plate, the rear side plate and the liquid lifting pipe 10 respectively, and the left support net and the right support net are fixedly connected with the top plate, the front side plate, the rear side plate and the liquid lifting pipe 10 respectively.

[0035] The above are only the preferred embodiments of the present application, and are not used to limit the present application, any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A distillation column for the production of electronic-grade hydrofluoric acid, characterized in that, The system includes a tower body containing several tower plates arranged from top to bottom. Each tower plate has an overflow weir and several air inlets. Each air inlet has a liquid lifting pipe, and a packing assembly is located on the upper side of each liquid lifting pipe. Sealing boxes, fixedly connected to the tower plates, are located on the left and right sides of each liquid lifting pipe. Liquid inlets, communicating with the sealing boxes, are located on the left and right sides of the lower end of each liquid lifting pipe. Each sealing box has a connecting hole for liquid to enter the sealing box. A first one-way valve for liquid to enter the liquid lifting pipe is located in each liquid inlet, and a second one-way valve for liquid to enter the sealing box is located in each connecting hole. A turbine is rotatably installed inside the liquid lifting pipe, with its rotation axis extending outward to the upper side of the sealing box. A first magnet is fixedly connected to the end of the turbine, with its two poles located at the upper and lower ends, respectively. A movable plate that moves vertically is installed inside the sealing box as a guide seal. A connecting pipe communicating with the interior of the sealing box above the movable plate is located on the sealing box. A second magnet is fixedly connected to the upper side of the movable plate, with its two poles located at the upper and lower ends, respectively.

2. The distillation column for producing electronic-grade hydrofluoric acid according to claim 1, characterized in that, The packing assembly has baffles on both sides, and a connecting plate on the side of the baffles away from the packing assembly. The sealing box has a fixing rod, and the connecting plate has guide holes that match the fixing rod. The connecting plate has an upper flange and a lower flange located on its upper and lower sides, respectively. Two springs are fitted on the fixing rod. The two ends of one spring are fixedly connected to the upper flange and the connecting plate, and the two ends of the other spring are fixedly connected to the lower flange and the connecting plate, respectively. A third magnet is provided on the lower side of the connecting plate, and the two magnetic poles of the third magnet are located at the upper and lower ends, respectively.

3. The distillation column for producing electronic-grade hydrofluoric acid according to claim 2, characterized in that, The two first magnets have the same magnetic poles at their top and bottom ends, the two second magnets have opposite magnetic poles at their top and bottom ends, and the two third magnets have the same magnetic poles at their top and bottom ends.

4. The distillation column for producing electronic-grade hydrofluoric acid according to claim 2, characterized in that, The baffle has an arrowhead-shaped cross-section, with the tip of the baffle pointing towards the packing assembly.

5. The distillation column for producing electronic-grade hydrofluoric acid according to claim 1, characterized in that, A preheating box is provided on the side of the sealed box away from the liquid extraction pipe. The preheating box is provided with a liquid inlet hole. A heat exchange plate is provided inside the preheating box. The heat exchange plate has a hollow structure. The lower end of the heat exchange plate has an opening that communicates with the hollow interior of the heat exchange plate. The heat exchange plate is sealed and fixedly connected to the tower plate. The lower end of the heat exchange plate extends downward through the tower plate.

6. The distillation column for producing electronic-grade hydrofluoric acid according to claim 1, characterized in that, The packing assembly includes a fixed frame and packing material filled within the fixed frame. The fixed frame includes a top plate, a front side plate, a rear side plate, a lower support net, a left support net, and a right support net. The top plate, front side plate, and rear side plate are welded and fixed. The lower support net is fixedly connected to the front side plate, the rear side plate, and the liquid extraction pipe, respectively. The left support net and the right support net are fixedly connected to the top plate, the front side plate, the rear side plate, and the liquid extraction pipe, respectively.

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