Electronic-grade hydrofluoric acid rectification heat exchange device

Abstract

The invention provides an electronic-grade hydrofluoric acid rectification heat exchange device, and relates to the field of heat exchange devices.The electronic-grade hydrofluoric acid rectification heat exchange device comprises a cold recovery box, the surface of the cold recovery box is provided with a hot backflow pipe and a hot circulation box, a plurality of mass transfer boxes are arranged above the cold recovery box, a plurality of mass transfer bottles are fixedly connected to the interiors of the mass transfer boxes, and the tops of the mass transfer boxes are fixedly connected with a top plate; a plurality of adjusting holes are uniformly formed in the surface of the top plate, adjusting boxes are arranged in the mass transfer boxes, high-corrosion-resistance air bags are symmetrically arranged on the surfaces of the adjusting boxes, adjusting blocks are arranged in the adjusting boxes, rotating pipes are arranged in the mass transfer bottles, and stirring paddles are arranged on the surfaces of the rotating pipes. The efficiency and the stability of the hydrofluoric acid rectification heat exchange device are improved, the adaptability of the device to the production scale and different raw materials is improved, and the energy consumption is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of heat exchange devices, and particularly to an electronic-grade hydrofluoric acid rectification heat exchange device. Background Art

[0002] As a core material for semiconductor manufacturing, photovoltaic cells, and the cleaning of precision electronic components, electronic-grade hydrofluoric acid requires a purity of over 99.999% (5N), and in particular, the concentrations of metal ions (such as Fe³⁺, Cr³⁺), particulate matter, and organic pollutants need to be strictly controlled. Currently, industrial purification is mainly achieved by combining multi-stage rectification towers with chemical adsorption methods. However, the relevant rectification towers usually rely on a single tray structure or packing type, with fixed numbers of transfer units (NTU) and heights of transfer units (HTU), making it difficult to dynamically adjust the separation efficiency according to the impurity concentration in the raw material. Moreover, the tray spacing, feed position, and reflux ratio of the relevant rectification towers usually need to be preset in advance and cannot accommodate the differential treatment requirements of multi-source raw materials such as fluorine-containing waste acid recovery liquid and industrial-grade HF crude products. The relevant processes usually use uniform heating throughout the tower to drive the vapor-liquid equilibrium through temperature differences. However, for high-purity purification, it is necessary to maintain a high temperature at the bottom of the tower (>100°C) and a low temperature at the top of the tower (<20°C), resulting in a relatively high proportion of steam consumption in the production cost. Summary of the Invention

[0003] The technical problem to be solved by the present invention is to provide an electronic-grade hydrofluoric acid rectification heat exchange device, which improves the efficiency and stability of the hydrofluoric acid rectification heat exchange device through multi-stage mass transfer and temperature-controlled gas flow regulation, enhances the adaptability of the device to production scale and different raw materials, and reduces energy consumption.

[0004] To solve the above technical problem, the technical solution of the present invention is as follows: An electronic-grade hydrofluoric acid rectification heat exchange device includes a cold recovery box, and a heat reflux pipe and a heat circulation box are arranged on the surface of the cold recovery box, including: A number of mass transfer boxes are arranged above the cold recovery box, and a number of mass transfer bottles are fixedly connected inside the mass transfer boxes. The mass transfer bottles are internally connected in sequence. By introducing a gas flow at a set temperature into one of the mass transfer boxes at the end, the corresponding mass transfer bottle is heated. The top of the mass transfer box is fixedly connected with a top plate, and a number of adjustment holes are evenly formed on the surface of the top plate. By adjusting the effective communication area between the adjustment holes and the interior of the corresponding mass transfer box, the temperature of the liquid raw material inside the corresponding mass transfer bottle is adjusted. Adjustment boxes are arranged inside the mass transfer boxes, and highly corrosion-resistant air bags are symmetrically arranged on the surface of the adjustment boxes. By adjusting the telescopic speed of the two highly corrosion-resistant air bags, the speed of gaseous hydrofluoric acid entering the mass transfer bottle is controlled. An adjustment block is arranged inside the adjustment box. By sliding the adjustment block inside the adjustment box, the corresponding highly corrosion-resistant airbag on the surface of the adjustment box can be adjusted to expand and contract, so as to maintain the stability of the air pressure inside the corresponding mass transfer bottle. A rotating tube is arranged inside the mass transfer bottle, and stirring paddles are arranged on the surface of the rotating tube. The gaseous hydrofluoric acid pumped into the corresponding mass transfer bottle by the highly corrosion-resistant airbag drives the stirring paddles to stir the liquid raw materials.

[0005] Furthermore, the mass transfer box is arranged between the cold recovery box and the heat reflux pipe. The upper surface of the mass transfer box abuts against the bottom surface of the heat circulation box. The mass transfer bottle is fixedly connected inside the mass transfer box. First one-way valves and second one-way valves are symmetrically arranged on the surface of the mass transfer box. The first one-way valve is installed in the first circular groove opened on the surface of the mass transfer box. The air outlet of the first one-way valve is connected to the inlet of the mass transfer bottle through a pipeline. The second one-way valve is connected to the inside of the air inlet of the adjacent first one-way valve through a pipeline. The rotating tube is rotatably connected to the inlet of the mass transfer bottle through a first bearing. A plurality of branch pipes are arranged on the surface of the rotating tube in an annular array. The branch pipes are fixedly connected in the second circular groove opened on the surface of the rotating tube. Spray heads are installed at the ends of the branch pipes. The stirring paddles are fixedly connected to the surface of the rotating tube.

[0006] Furthermore, two porous plates are fixedly connected inside the mass transfer bottle. The stirring paddles are located between the two porous plates. The rotating tube is located in the avoidance groove opened on the surface of the porous plate.

[0007] Furthermore, the adjustment box is fixedly connected to the inner wall of the mass transfer box. A first adjustment groove is opened inside the adjustment box. The highly corrosion-resistant airbags are all fixedly connected to the bottom surface of the adjustment box. Electric control telescopic rods are arranged directly below the highly corrosion-resistant airbags. The electric control telescopic rods are installed inside the mass transfer box. A third one-way valve and a fourth one-way valve are respectively installed in the third circular grooves symmetrically opened on the surface of the highly corrosion-resistant airbag. The first adjustment groove is connected to the inside of the air inlets of the two third one-way valves. The adjustment block is slidably connected to the inside of the first adjustment groove. A hydrophobic valve is arranged inside the mass transfer box. The air inlet of the hydrophobic valve is connected to the outlet of the mass transfer bottle through a pipeline. The air outlet of the hydrophobic valve is connected to the inside of the first adjustment groove through a pipeline. The adjustment block is always connected to the inside of the air outlet of the hydrophobic valve. A second adjustment groove is opened inside the adjustment box. The second adjustment groove is connected to the inside of the air inlet of the fourth one-way valve. The second adjustment groove is connected to the inside of the air inlet of the second one-way valve through a pipeline.

[0008] Furthermore, an adjusting plug is slidably connected inside the mass transfer box. The bottom surface of the adjusting plug abuts against the upper surface of the top plate. A driving motor is installed on the surface of the mass transfer box. The output shaft of the driving motor extends into the mass transfer box through a fourth circular groove opened on the surface of the mass transfer box. The end of the output shaft of the driving motor is fixedly connected with a first lead screw. The first lead screw is threadedly connected with the adjusting plug through a first threaded hole opened on the surface of the adjusting plug.

[0009] Furthermore, a diversion plate is fixedly connected to the bottom surface of the top plate. The surface of the diversion plate abuts against the inner wall of the mass transfer box, and the bottom surface of the diversion plate does not contact the inner bottom surface of the mass transfer box.

[0010] Furthermore, a plurality of first solenoid valves are arranged in a circular array on the surface of the mass transfer box. A four-way pipe is arranged between adjacent two of the first solenoid valves. Two of the pipe orifices of the four-way pipe are respectively connected and communicated with one of the valve orifices of adjacent two of the first solenoid valves through pipes. A collecting bottle is arranged inside the cold recovery box. One of the pipe orifices of the four-way pipe is connected and communicated with the inside of the collecting bottle through a pipe. A second solenoid valve is installed on the last pipe orifice of the four-way pipe.

[0011] Furthermore, plugging grooves are arranged in a circular array on the surface of the heat return pipe. An inserting pipe is fixedly connected inside a sixth circular groove opened on the surface of the mass transfer box. The upper surface of the heat return pipe abuts against the inner top surface of the heat circulation box. First communication grooves are arranged in a circular array on the bottom surface of the heat return pipe. A flow equalizing plate is fixedly connected inside the heat circulation box. The surface of the flow equalizing plate abuts against the surface of the heat return pipe.

[0012] Furthermore, two adjusting air pipes are arranged on the surface of the heat circulation box. The adjusting air pipes are fixedly connected with the heat circulation box through fifth circular grooves opened on the surface of the heat circulation box. The inside of one of the adjusting air pipes is connected and communicated with the inside of the heat circulation box. The inside of the other adjusting air pipe is connected and communicated with the inside of the heat return pipe. A moving plug is slidably connected inside the adjusting air pipe. An electric push rod is installed inside a seventh circular groove opened on the upper surface of the adjusting air pipe. The end of the output shaft of the electric push rod is fixedly connected with the moving plug.

[0013] The above scheme of the present invention has at least the following beneficial effects: In the above solution of the present invention, by providing internal communication between multiple mass transfer bottles and combining temperature-controlled air flow heating, the mass transfer efficiency between gaseous hydrofluoric acid and liquid raw materials is effectively improved, the rectification process is optimized, and energy consumption is reduced; the use of a highly corrosion-resistant airbag and an electric control telescopic rod to adjust the flow rate of hydrofluoric acid helps to accurately control the gas inlet rate, thereby ensuring stable air pressure and effective stirring of the liquid raw materials; the adoption of a dynamic temperature adjustment method makes the air flow and temperature control more accurate, reduces heat loss, and enhances the capacity of the entire heat exchange device. Description of the Drawings

[0014] Figure 1 is the overall structural schematic diagram provided by the present invention.

[0015] Figure 2 is the schematic diagram of the movable plug in the present invention.

[0016] Figure 3 is the schematic diagram of the mass transfer box in the present invention.

[0017] Figure 4 is the schematic diagram of the heat reflux pipe in the present invention.

[0018] Figure 5 is the schematic diagram of the highly corrosion-resistant airbag in the present invention.

[0019] Figure 6 is the schematic diagram of the perforated plate in the present invention.

[0020] Figure 7 is the schematic diagram of the adjusting block in the present invention.

[0021] Figure 8 is the present invention Figure 5 The enlarged view of part A.

[0022] In the figure: 101, cold recovery box; 102, heat reflux pipe; 103, heat circulation box; 201, mass transfer box; 202, mass transfer bottle; 203, first one-way valve; 204, drain valve; 205, adjustment box; 206, highly corrosion-resistant airbag; 207, electric control telescopic rod; 208, second one-way valve; 209, adjusting block; 210, first adjustment groove; 211, second adjustment groove; 212, third one-way valve; 213, fourth one-way valve; 214, rotating pipe; 215, branch pipe; 216, nozzle; 217, stirring paddle; 218, perforated plate; 219, top plate; 220, adjustment hole; 221, adjustment plug; 222, drive motor; 223, guide plate; 224, insertion pipe; 225, first lead screw; 301, first solenoid valve; 302, four-way pipe; 303, collecting bottle; 304, second solenoid valve; 401. Adjusting air pipe; 402. Moving plug; 403. Electric push rod; 404. Flow equalizing plate; 405. First communication groove; 406. Insertion groove 501. Intake pipe; 502. Outlet pipe Specific implementation mode

[0023] Hereinafter, exemplary embodiments of the present disclosure will be described in more detail with reference to the accompanying drawings. Although the exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided so that the present disclosure can be more thoroughly understood and the scope of the present disclosure can be completely conveyed to those skilled in the art

[0024] As Figures 1 to 8 shown, an embodiment of the present invention provides an electronic-grade hydrofluoric acid rectification heat exchange device, including a cold recovery tank 101. A heat reflux pipe 102 and a heat circulation tank 103 are arranged on the surface of the cold recovery tank 101, including: A plurality of mass transfer tanks 201 are arranged above the cold recovery tank 101. A plurality of mass transfer bottles 202 are fixedly connected inside the mass transfer tanks 201. The mass transfer bottles 202 are internally connected in sequence. By introducing a gas flow at a set temperature into one of the mass transfer tanks 201 at the end, the corresponding mass transfer bottle 202 is heated A top plate 219 is fixedly connected to the top of the mass transfer tank 201. A plurality of adjustment holes 220 are evenly formed on the surface of the top plate 219. By adjusting the effective communication area between the adjustment holes 220 and the inside of the corresponding mass transfer tank 201, the temperature of the liquid raw material inside the corresponding mass transfer bottle 202 is adjusted Adjustment boxes 205 are arranged inside the mass transfer tanks 201. High corrosion-resistant air bags 206 are symmetrically arranged on the surface of the adjustment boxes 205. By adjusting the telescopic speed of the two high corrosion-resistant air bags 206, the speed of gaseous hydrofluoric acid entering the mass transfer bottle 202 is controlled An adjustment block 209 is arranged inside the adjustment box 205. By sliding the adjustment block 209 inside the adjustment box 205, the corresponding high corrosion-resistant air bag 206 on the surface of the adjustment box 205 is adjusted to expand and contract, so as to maintain the stability of the air pressure inside the corresponding mass transfer bottle 202 A rotating pipe 214 is arranged inside the mass transfer bottle 202. Stirring paddles 217 are arranged on the surface of the rotating pipe 214. The gaseous hydrofluoric acid pumped into the corresponding mass transfer bottle 202 by the high corrosion-resistant air bag 206 drives the stirring paddles 217 to stir the liquid raw material

[0025] In an embodiment of the present invention, according to different raw materials of hydrofluoric acid, multi-stage mass transfer is set, that is, a plurality of mass transfer bottles 202 are connected in sequence. One of the mass transfer bottles 202 located at the end is heated to a set temperature to generate sufficient gaseous hydrofluoric acid in the mass transfer bottle 202. The gaseous hydrofluoric acid enters the highly corrosion-resistant airbag 206 through a pipeline, and is pumped into the next-stage mass transfer bottle 202 through the compression deformation of the highly corrosion-resistant airbag 206, and mass transfer exchange is carried out with the raw materials inside the next-stage mass transfer bottle 202 through the rotating pipe 214. Among them, the air pressure intensity provided by the compression deformation of the highly corrosion-resistant airbag 206 makes the stirring paddle 217 rotate to stir the liquid raw materials and improve the mass transfer efficiency; After multi-stage mass transfer, when the purity of the gaseous hydrofluoric acid discharged from the last-stage mass transfer bottle 202 reaches the set value, it is first passed through a filtering device to remove impurities such as water and silicon tetrafluoride in the gaseous hydrofluoric acid, and then passed through a condensing device for collection; If the impurity concentration of the liquid raw materials inside the mass transfer bottle 202 reaches the waste liquid level, a group of mass transfer bottles 202 can be added between the last-stage mass transfer bottle 202 and the filtering device, and at the same time, the mass transfer bottle 202 whose internal liquid raw materials reach the waste liquid level is removed, so that the original second-stage mass transfer bottle 202 becomes the first-stage mass transfer bottle 202, and then it is filled forward level by level, and the added mass transfer bottle 202 is the last stage; The specific filling method is to pass a gas flow at a set temperature into the corresponding mass transfer box 201 to heat the corresponding mass transfer bottle 202 to the set temperature. The temperature of the first-stage mass transfer bottle 202 is the highest to provide gaseous hydrofluoric acid. To maintain better mass transfer efficiency and concentration difference driving force, the temperature difference between the gaseous hydrofluoric acid entering each stage and the liquid raw materials inside the corresponding mass transfer bottle 202 is controlled between 2 degrees Celsius and 5 degrees Celsius. During filling, it is only necessary to make the corresponding mass transfer box 201 where the mass transfer bottle 202 is located reach the corresponding temperature; If the number of mass transfer bottles 202 is limited, the purity of the raw materials can be made to reach the set value through multiple rounds of rectification, that is, during the rectification process, by dynamically replacing the mass transfer bottles 202, the purity of the gaseous hydrofluoric acid flowing out of the last-stage mass transfer bottle 202 is gradually increased. That is, if the purity of the condensed and collected hydrofluoric acid does not meet the standard, it is used as the liquid raw materials inside the added mass transfer bottle 202 until the purity of the hydrofluoric acid meets the standard.

[0026] It should be noted that the working principles and usage processes of the condensing device (not shown in the figure) and the filtering device (not shown in the figure) are well known in the prior art and will not be elaborated in detail here.

[0027] The mass transfer box 201 is arranged between the cold recovery box 101 and the hot reflux pipe 102. The upper surface of the mass transfer box 201 abuts against the bottom surface of the thermal circulation box 103. The mass transfer bottle 202 is fixedly connected inside the mass transfer box 201. The first one-way valve 203 and the second one-way valve 208 are symmetrically arranged on the surface of the mass transfer box 201. The first one-way valve 203 is installed in the first circular groove opened on the surface of the mass transfer box 201. The air outlet of the first one-way valve 203 is connected to the inlet of the mass transfer bottle 202 through a pipeline. The second one-way valve 208 is connected to the inside of the air inlet of the adjacent first one-way valve 203 through a pipeline. The rotating pipe 214 is rotatably connected to the inlet of the mass transfer bottle 202 through a first bearing. A plurality of branch pipes 215 are arranged in an annular array on the surface of the rotating pipe 214. The branch pipes 215 are fixedly connected in the second circular groove opened on the surface of the rotating pipe 214. Nozzles 216 are installed at the ends of the branch pipes 215. The stirring paddle 217 is fixedly connected to the surface of the rotating pipe 214.

[0028] Two porous plates 218 are fixedly connected inside the mass transfer bottle 202. The stirring paddle 217 is located between the two porous plates 218. The rotating pipe 214 is located in the avoidance groove opened on the surface of the porous plate 218.

[0029] In the embodiment of the present invention, the lower porous plate 218 is immersed in the liquid raw material, and the upper porous plate 218 is located above the liquid raw material. After the gaseous hydrofluoric acid enters the mass transfer bottle 202, it enters the inside of the rotating pipe 214 and then enters the inside of the branch pipes 215, and finally sprays out from the nozzles 216. After the sprayed gaseous hydrofluoric acid is cut by the micropores on the surface of the porous plate 218, it more fully undergoes mass transfer exchange with the liquid raw material inside the mass transfer bottle 202. At the same time, when the gaseous hydrofluoric acid sprays out from the nozzles 216, the nozzles 216 drive the rotating pipe 214 to rotate through the branch pipes 215 under the action of the reaction force, so that the stirring paddle 217 stirs the liquid raw material inside the mass transfer bottle 202, further improving the mass transfer efficiency between the gaseous hydrofluoric acid and the liquid raw material. The upper porous plate 218 is used to reduce foam, stabilize the liquid level and the splash of the liquid raw material, thereby facilitating the maintenance of the stability of the mass transfer efficiency.

[0030] The adjustment box 205 is fixedly connected to the inner wall of the mass transfer box 201. A first adjustment groove 210 is provided inside the adjustment box 205. The highly corrosion-resistant air bags 206 are fixedly connected to the bottom surface of the adjustment box 205. Electrically controlled telescopic rods 207 are arranged directly below the highly corrosion-resistant air bags 206. The electrically controlled telescopic rods 207 are installed inside the mass transfer box 201. A third one-way valve 212 and a fourth one-way valve 213 are respectively installed in the third circular grooves symmetrically opened on the surface of the highly corrosion-resistant air bag 206. The first adjustment groove 210 is internally connected to the air inlets of the two third one-way valves 212. The adjustment block 209 is slidably connected inside the first adjustment groove 210. A hydrophobic valve 204 is arranged inside the mass transfer box 201. The air inlet of the hydrophobic valve 204 is connected to the outlet of the mass transfer bottle 202 through a pipeline. The air outlet of the hydrophobic valve 204 is connected to the inside of the first adjustment groove 210 through a pipeline. The adjustment block 209 is always internally connected to the air outlet of the hydrophobic valve 204. A second adjustment groove 211 is provided inside the adjustment box 205. The second adjustment groove 211 is internally connected to the air inlet of the fourth one-way valve 213. The second adjustment groove 211 is internally connected to the air inlet of the second one-way valve 208 through a pipeline.

[0031] In the embodiment of the present invention, the steam trap 204 is made of a highly corrosion-resistant material and is used to prevent gaseous hydrofluoric acid from entraining the liquid raw materials in the mass transfer bottle 202, so as to ensure that the impurity content of the gaseous hydrofluoric acid decreases step by step. The gaseous hydrofluoric acid flowing out of the outlet of the mass transfer bottle 202 enters the inside of the adjustment box 205 through the steam trap 204 and the pipeline. The gaseous hydrofluoric acid entering the inside of the adjustment box 205 first enters the adjustment block 209 inside the first adjustment groove 210 and enters the corresponding highly corrosion-resistant airbag 206 through one of the third one-way valves 212, causing the highly corrosion-resistant airbag 206 to continuously expand. An inductor is installed at the end of the output shaft of the electric control telescopic rod 207 below the highly corrosion-resistant airbag 206. When the electric control telescopic rod 207 touches the inductor, the corresponding electric control telescopic rod 207 elongates, causing the corresponding highly corrosion-resistant airbag 206 to be compressed. The compression of the highly corrosion-resistant airbag 206 causes the gaseous hydrofluoric acid inside it to enter the inside of the second adjustment groove 211 through the fourth one-way valve 213 and enter the air inlet of the second one-way valve 208 through the pipeline, and then flow through the pipeline to the air inlet of the first one-way valve 203 corresponding to the next-stage mass transfer bottle 202. During this process, due to the increase in the internal air pressure of the highly corrosion-resistant airbag 206 in the process of compression deformation, the gaseous hydrofluoric acid entering the inside of the adjustment block 209 cannot continue to enter the highly corrosion-resistant airbag 206 undergoing compression deformation through the corresponding third one-way valve 212. The continuous entry of gaseous hydrofluoric acid into the inside of the adjustment block 209 causes the adjustment block 209 to move away from the highly corrosion-resistant airbag 206 undergoing compression deformation inside the first adjustment groove 210 until the adjustment block 209 is connected to the inside of the air inlet of the third one-way valve 212 on the surface of another highly corrosion-resistant airbag 206. At this time, the gaseous hydrofluoric acid enters the inside of another highly corrosion-resistant airbag 206 and causes the highly corrosion-resistant airbag 206 to undergo expansion deformation; The deformation speed of the highly corrosion-resistant airbag 206 is positively correlated with the air pressure pumped into the corresponding mass transfer bottle 202, and thus the stirring speed of the corresponding stirring paddle 217 can be regulated.

[0032] An adjustment plug 221 is slidably connected inside the mass transfer box 201. The bottom surface of the adjustment plug 221 abuts against the upper surface of the top plate 219. A driving motor 222 is installed on the surface of the mass transfer box 201. The output shaft of the driving motor 222 extends into the inside of the mass transfer box 201 through the fourth circular groove opened on the surface of the mass transfer box 201. The end of the output shaft of the driving motor 222 is fixedly connected to a first lead screw 225. The first lead screw 225 is threadedly connected to the adjustment plug 221 through the first threaded hole opened on the surface of the adjustment plug 221.

[0033] The bottom surface of the top plate 219 is fixedly connected to a flow guide plate 223. The surface of the flow guide plate 223 abuts against the inner wall of the mass transfer box 201, and the bottom surface of the flow guide plate 223 does not contact the inner bottom surface of the mass transfer box 201.

[0034] In the embodiment of the present invention, the hot air generated by the external heating device is introduced into the interior of the mass transfer box 201 above the top plate 219. The hot air flow entering the interior of the top plate 219 enters the interior of the mass transfer box 201 through the adjustment holes 220. Under the guidance of the flow guide plate 223, the hot air flow first passes through the surface of the mass transfer bottle 202 to heat the mass transfer bottle 202, so as to improve the response efficiency of the hot air flow to the temperature adjustment of the mass transfer bottle 202, and enable the temperature of the mass transfer bottle 202 to quickly change with the change of the flow rate of the hot air flow; By energizing and operating the drive motor 222, the drive motor 222 drives the first lead screw 225 to rotate. The rotation of the first lead screw 225 causes the adjustment plug 221 to move on the upper surface of the top plate 219, thereby changing the degree of blockage of the adjustment plug 221 to the adjustment holes 220, so as to adjust the flow rate of the hot air flow entering the interior of the mass transfer box 201 through the adjustment holes 220.

[0035] A plurality of first solenoid valves 301 are arranged on the surface of the mass transfer box 201 in a circular array. A four-way pipe 302 is arranged between every two adjacent first solenoid valves 301. Two of the pipe orifices of the four-way pipe 302 are respectively connected to the interior of one of the valve ports of the two adjacent first solenoid valves 301 through pipes. A collecting bottle 303 is arranged inside the cold recovery box 101. One of the pipe orifices of the four-way pipe 302 is connected to the interior of the collecting bottle 303 through a pipe, and a second solenoid valve 304 is installed at the last pipe orifice of the four-way pipe 302.

[0036] In the embodiment of the present invention, the outlet of the second one-way valve 208 corresponding to the mass transfer bottle 202 at the last stage is connected to the valve port of the adjacent second solenoid valve 304 through a pipe (not shown in the figure), and the second solenoid valve 304 is in an open state, and all the other first solenoid valves 301 and the second solenoid valve 304 are in a closed state, that is, the outlet of the second one-way valve 208 corresponding to the mass transfer bottle 202 at the last stage is connected to the interior of the corresponding four-way pipe 302 through the second solenoid valve 304, and further the second one-way valve 208 is connected to the interior of the corresponding collecting bottle 303; The gaseous hydrofluoric acid entering the interior of the collecting bottle 303 flows out through the pipe arranged at the bottom of the collecting bottle 303 to the external filtering device and condensing device. When it is necessary to add a mass transfer bottle 202, the added mass transfer box 201 is placed on one side of the original last-stage mass transfer box 201, so that the second one-way valve 208 on the surface of the added mass transfer box 201 is connected to the valve port of the adjacent second solenoid valve 304 through a pipe, the second solenoid valve 304 connected to the added second one-way valve 208 is in an open state, and the second solenoid valve 304 corresponding to the original last-stage mass transfer bottle 202 is closed, that is, the addition of the mass transfer bottle 202 is completed.

[0037] The surface of the heat reflux pipe 102 is provided with insertion slots 406 in an annular array. An insertion pipe 224 is fixedly connected inside the sixth circular groove opened on the surface of the mass transfer box 201. The upper surface of the heat reflux pipe 102 abuts against the inner top surface of the heat circulation box 103. The bottom surface of the heat reflux pipe 102 is provided with first communication slots 405 in an annular array. A flow equalizing plate 404 is fixedly connected inside the heat circulation box 103, and the surface of the flow equalizing plate 404 abuts against the surface of the heat reflux pipe 102.

[0038] Two adjustment air pipes 401 are arranged on the surface of the heat circulation box 103. The adjustment air pipes 401 are fixedly connected to the heat circulation box 103 through the fifth circular grooves opened on the surface of the heat circulation box 103. The inside of one of the adjustment air pipes 401 is communicated with the inside of the heat circulation box 103, and the inside of the other adjustment air pipe 401 is communicated with the inside of the heat reflux pipe 102. A moving plug 402 is slidably connected inside the adjustment air pipe 401. An electric push rod 403 is installed in the seventh circular groove opened on the upper surface of the adjustment air pipe 401, and the end of the output shaft of the electric push rod 403 is fixedly connected to the moving plug 402.

[0039] In the embodiment of the present invention, the mass transfer box 201 is placed on the upper surface of the cold recovery box 101, so that the insertion pipe 224 on the surface of the mass transfer box 201 is inserted into one of the insertion slots 406 on the surface of the heat reflux pipe 102, so that the inside of the mass transfer box 201 is communicated with the inside of the heat reflux pipe 102 through the insertion pipe 224, and the mass transfer box 201 is communicated with one of the first communication slots 405 on the bottom surface of the heat circulation box 103; After arranging a number of mass transfer boxes 201 in the above manner in sequence, the remaining first communication slots 405 and insertion slots 406 that are not communicated with the inside of the mass transfer box 201 are blocked. In this embodiment, the blocking method is to block them with a sealing plug, so that the hot air flow generated by the heating device is introduced into the air inlet pipe 501 through the air pump and the pipeline, and enters the inside of the heat circulation box 103 through the air inlet pipe 501. After being equalized by the flow equalizing plate 404, it enters the inside of the corresponding mass transfer box 201 through the unblocked first communication slot 405; When adjusting the blocking situation of the adjusting block 221 to the adjusting hole 220 to adjust the flow rate of the hot air flow entering the corresponding mass transfer box 201, in order to keep the air pressure inside the heat circulation box 103 stable, make the flow rate of the hot air flow entering the mass transfer box 201 be positively correlated with the effective cross-section of the air flow actually passing through the adjusting hole 220, that is, be positively correlated with the effective communication area between the adjusting hole 220 and the inside of the mass transfer box 201, so that the moving plug 402 inside the adjustment air pipe 401 moves under the telescopic drive of the electric push rod 403, thereby weakening the air pressure fluctuation inside the heat circulation box 103 and the heat reflux pipe 102, so as to improve the adjustment accuracy of the temperature inside the mass transfer box 201; The hot air flow entering the interior of the mass transfer box 201 returns from the insertion connection pipe 224 to the interior of the hot return pipe 102 and returns from the air outlet pipe 502 to the heating device to reduce heat loss; If the temperature of the mass transfer bottle 202 is gradually decreasing, the surface of the corresponding mass transfer box 201 can be cooled by ventilation, and then the mass transfer bottle 202 inside it can be cooled. The use of air cooling is well known in the prior art and will not be elaborated here in detail; It should be noted that: the hot return pipe 102 is fixed on the upper surface of the cold recovery box 101, and the hot return pipe 102 is fixedly connected to the hot circulation box 103 through a second reserved opening provided at the bottom surface of the hot circulation box 103, which is convenient for forming an air flow channel.

[0040] The connection method of the pipeline is to fix the end of the pipeline in the reserved opening by opening the reserved opening so that the pipeline is communicated with the interior of the reserved opening. This is well known in the prior art and will not be elaborated here in detail; The bottom end of the rotating pipe 214 is closed, which is convenient for gaseous hydrofluoric acid to enter the interior of the branch pipe 215 through the rotating pipe 214; The shape of the flow guide plate 223 is composed of a threaded sleeve and several blocking blocks fixed on the threaded sleeve through rectangular blocks. The shape and arrangement of the blocking blocks correspond to the adjustment holes 220, which is convenient for adjusting the blocking of the adjustment holes 220 by the blocking blocks 221. Avoidance holes are provided on the surface of the flow guide plate 223, which is convenient for the pipeline to pass through the flow guide plate 223; The working principles and usage processes of the heating equipment and the air pump are well known in the prior art and will not be elaborated here in detail; Ventilation holes are evenly provided on the upper surface of the adjustment air pipe 401 for balancing the air pressure inside the adjustment air pipe 401; The working principle and usage process of the sensor are well known in the prior art and will not be elaborated here in detail.

[0041] The above is the preferred implementation manner of the present invention. It should be pointed out that for those of ordinary skill in the art of the present technology, without departing from the principle described in the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. An electronic-grade hydrofluoric acid rectification heat exchange device, comprising a cold recovery box (101), wherein a heat reflux pipe (102) and a heat circulation box (103) are arranged on the surface of the cold recovery box (101), and is characterized in that, Including: Above the cold recovery box (101), a number of mass transfer boxes (201) are provided. Inside the mass transfer box (201), a number of mass transfer bottles (202) are fixedly connected. The mass transfer bottles (202) are internally connected in sequence. By introducing an air flow at a set temperature into one of the mass transfer boxes (201) located at the end, the corresponding mass transfer bottle (202) is heated; At the top of the mass transfer box (201), a top plate (219) is fixedly connected. On the surface of the top plate (219), a number of adjustment holes (220) are evenly opened. By adjusting the effective communication area between the adjustment holes (220) and the interior of the corresponding mass transfer box (201), the temperature of the liquid raw material inside the corresponding mass transfer bottle (202) is adjusted; Inside the mass transfer box (201), an adjustment box (205) is provided. On the surface of the adjustment box (205), highly corrosion-resistant air bags (206) are symmetrically arranged. By adjusting the telescopic speed of the two highly corrosion-resistant air bags (206), the speed of gaseous hydrofluoric acid entering the mass transfer bottle (202) is controlled; Inside the adjustment box (205), an adjustment block (209) is provided. By sliding the adjustment block (209) inside the adjustment box (205), the corresponding highly corrosion-resistant air bag (206) on the surface of the adjustment box (205) is adjusted to expand and contract, so as to maintain the stability of the air pressure inside the corresponding mass transfer bottle (202); Inside the mass transfer bottle (202), a rotating pipe (214) is provided. On the surface of the rotating pipe (214), stirring paddles (217) are provided. By pumping gaseous hydrofluoric acid into the corresponding mass transfer bottle (202) through the highly corrosion-resistant air bag (206), the stirring paddles (217) are driven to stir the liquid raw material.

2. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 1, wherein The mass transfer box (201) is arranged between the cold recovery box (101) and the heat reflux pipe (102). The upper surface of the mass transfer box (201) abuts against the bottom surface of the heat circulation box (103). The mass transfer bottle (202) is fixedly connected inside the mass transfer box (201). On the surface of the mass transfer box (201), a first one-way valve (203) and a second one-way valve (208) are symmetrically arranged. The first one-way valve (203) is installed in the first circular groove opened on the surface of the mass transfer box (201). The air outlet of the first one-way valve (203) is connected to the inlet of the mass transfer bottle (202) through a pipeline. The second one-way valve (208) is internally connected to the air inlet of the adjacent first one-way valve (203) through a pipeline. The rotating pipe (214) is rotatably connected to the inlet of the mass transfer bottle (202) through a first bearing. On the surface of the rotating pipe (214), a number of branch pipes (215) are arranged in an annular array. The branch pipes (215) are fixedly connected in the second circular groove opened on the surface of the rotating pipe (214). Nozzles (216) are installed at the ends of the branch pipes (215). The stirring paddles (217) are fixedly connected to the surface of the rotating pipe (214).

3. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 2, wherein Two porous plates (218) are fixedly connected inside the mass transfer bottle (202). The stirring paddle (217) is located between the two porous plates (218), and the rotating tube (214) is located in the avoidance groove formed on the surface of the porous plate (218).

4. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 3, characterized in that The adjustment box (205) is fixedly connected to the inner wall of the mass transfer box (201). A first adjustment groove (210) is formed inside the adjustment box (205). High corrosion-resistant air bags (206) are fixedly connected to the bottom surface of the adjustment box (205). Electrically controlled telescopic rods (207) are arranged directly below the high corrosion-resistant air bags (206). The electrically controlled telescopic rods (207) are installed inside the mass transfer box (201). A third one-way valve (212) and a fourth one-way valve (213) are respectively installed in the third circular grooves symmetrically formed on the surface of the high corrosion-resistant air bag (206). The first adjustment groove (210) is internally connected to the air inlets of the two third one-way valves (212). The adjustment block (209) is slidably connected inside the first adjustment groove (210). A hydrophobic valve (204) is arranged inside the mass transfer box (201). The air inlet of the hydrophobic valve (204) is connected to the outlet of the mass transfer bottle (202) through a pipeline. The air outlet of the hydrophobic valve (204) is internally connected to the first adjustment groove (210) through a pipeline. The adjustment block (209) is always internally connected to the air outlet of the hydrophobic valve (204). A second adjustment groove (211) is formed inside the adjustment box (205). The second adjustment groove (211) is internally connected to the air inlet of the fourth one-way valve (213). The second adjustment groove (211) is internally connected to the air inlet of the second one-way valve (208) through a pipeline.

5. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 4, wherein, An adjustment plug (221) is slidably connected inside the mass transfer box (201). The bottom surface of the adjustment plug (221) abuts against the upper surface of the top plate (219). A driving motor (222) is installed on the surface of the mass transfer box (201). The output shaft of the driving motor (222) extends into the mass transfer box (201) through the fourth circular groove formed on the surface of the mass transfer box (201). The end of the output shaft of the driving motor (222) is fixedly connected to a first lead screw (225). The first lead screw (225) is threadedly connected to the adjustment plug (221) through the first threaded hole formed on the surface of the adjustment plug (221).

6. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 5, wherein, A flow guide plate (223) is fixedly connected to the bottom surface of the top plate (219). The surface of the flow guide plate (223) abuts against the inner wall of the mass transfer box (201). The bottom surface of the flow guide plate (223) does not contact the inner bottom surface of the mass transfer box (201).

7. The rectification heat exchange device for electronic grade hydrofluoric acid according to claim 6, characterized in that, A plurality of first solenoid valves (301) are arranged on the surface of the mass transfer box (201) in an annular array. A four-way pipe (302) is arranged between two adjacent first solenoid valves (301). Two of the pipe orifices of the four-way pipe (302) are respectively connected to the inside of one valve orifice of two adjacent first solenoid valves (301) through pipes. A current collecting bottle (303) is arranged inside the cold recovery box (101). One of the pipe orifices of the four-way pipe (302) is connected to the inside of the current collecting bottle (303) through a pipe. A second solenoid valve (304) is installed at the last pipe orifice of the four-way pipe (302).

8. The electronic grade hydrofluoric acid rectification heat exchange device according to claim 7, wherein Insertion slots (406) are arranged on the surface of the heat reflux pipe (102) in an annular array. An insertion pipe (224) is fixedly connected inside the sixth circular groove opened on the surface of the mass transfer box (201). The upper surface of the heat reflux pipe (102) abuts against the inner top surface of the heat circulation box (103). First communication slots (405) are arranged on the bottom surface of the heat reflux pipe (102) in an annular array. A flow equalizing plate (404) is fixedly connected inside the heat circulation box (103). The surface of the flow equalizing plate (404) abuts against the surface of the heat reflux pipe (102).

9. The electronic-grade hydrofluoric acid rectification heat exchange device according to claim 8, wherein, Two regulating air pipes (401) are arranged on the surface of the heat circulation box (103). The regulating air pipes (401) are fixedly connected to the heat circulation box (103) through the fifth circular grooves opened on the surface of the heat circulation box (103). The inside of one of the regulating air pipes (401) is communicated with the inside of the heat circulation box (103). The inside of the other regulating air pipe (401) is communicated with the inside of the heat reflux pipe (102). A moving plug (402) is slidably connected inside the regulating air pipe (401). An electric push rod (403) is installed inside the seventh circular groove opened on the upper surface of the regulating air pipe (401). The end of the output shaft of the electric push rod (403) is fixedly connected to the moving plug (402).

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