An electronic-grade hydrofluoric acid distillation heat exchange device

Abstract

The present invention provides an electronic-grade hydrofluoric acid distillation heat exchange device, which relates to the field of heat exchange devices and comprises a cold recovery box, wherein a heat reflux pipe and a heat circulation box are arranged on the surface of the cold recovery box, wherein a plurality of mass transfer boxes are arranged above the cold recovery box, a plurality of mass transfer bottles are fixedly connected to the interior of the mass transfer boxes, a top plate is fixedly connected to the top of the mass transfer box, a plurality of adjustment holes are evenly opened on the surface of the top plate, an adjustment box is arranged inside each mass transfer box, a high-corrosion-resistant air bag is symmetrically arranged on the surface of the adjustment box, an adjustment block is arranged inside the adjustment box, a rotating tube is arranged inside the mass transfer bottle, and a stirring paddle is arranged on the surface of the rotating tube. The present invention improves the efficiency and stability of the hydrofluoric acid distillation heat exchange device through multi-stage mass transfer and temperature-controlled airflow adjustment, improves the adaptability of the device to production scale and different raw materials, and reduces energy consumption.

Description

Technical Field

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

[0002] Electronic grade hydrofluoric acid is a core material for semiconductor manufacturing, photovoltaic cells and precision electronic components cleaning. Its purity is required to reach above 99.999% (5N). In particular, the metal ions (such as Fe 3+ Cr 3+ ), concentrations of particulate matter and organic pollutants;

[0003] At present, the industry mainly uses multi-stage distillation towers combined with chemical adsorption to achieve purification. However, the relevant distillation towers usually rely on a single tower plate structure or packing type, and the number of mass transfer units (NTU) and the height of the mass transfer unit (HTU) are fixed. It is difficult to dynamically adjust the separation efficiency according to the impurity concentration in the raw materials. In addition, the tower plate spacing, feed position and reflux ratio of the relevant distillation towers usually need to be pre-set, which is not compatible with the differentiated processing requirements of multiple sources of raw materials such as fluorine-containing waste acid recovery liquid and industrial-grade HF crude product. The relevant process usually adopts uniform heating of the entire tower and drives the vapor-liquid equilibrium through temperature difference. However, high-purity purification requires maintaining a high temperature in the tower bottom (>100°C) and a low temperature at the tower top (<20°C), resulting in steam consumption accounting for a high proportion of production costs. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide an electronic-grade hydrofluoric acid distillation heat exchange device. Through multi-stage mass transfer and temperature-controlled airflow regulation, the efficiency and stability of the hydrofluoric acid distillation heat exchange device are improved, the adaptability of the device to production scale and different raw materials is improved, and energy consumption is reduced.

[0005] In order to solve the above technical problems, the technical solutions of the present invention are as follows:

[0006] An electronic-grade hydrofluoric acid distillation heat exchange device includes a cold recovery box, the surface of which is provided with a heat reflux pipe and a heat circulation box, comprising:

[0007] A plurality of mass transfer boxes are provided above the cold recovery box, and a mass transfer bottle is fixedly connected to the inside of each mass transfer box. The mass transfer bottles are connected to each other in sequence, and a set temperature air flow is introduced into the inside of one of the mass transfer boxes located at the end to heat the corresponding mass transfer bottle;

[0008] The top of the mass transfer box is fixedly connected to a top plate, and a plurality of adjustment holes are evenly opened on the surface of the top plate. By adjusting the effective communication area between the adjustment holes and the corresponding interior of the mass transfer box, the temperature of the liquid raw material inside the corresponding mass transfer bottle can be adjusted;

[0009] The mass transfer box is provided with an adjustment box inside, and the surface of the adjustment box is symmetrically provided with high corrosion-resistant air bags. By adjusting the expansion and contraction speed of the two high corrosion-resistant air bags, the speed at which the gaseous hydrofluoric acid enters the mass transfer bottle is regulated;

[0010] An adjusting block is provided inside the adjusting box, and the adjusting block slides inside the adjusting box to adjust the expansion and contraction of the corresponding high corrosion-resistant airbag on the surface of the adjusting box, so as to maintain the stability of the air pressure inside the corresponding mass transfer bottle;

[0011] A rotating tube is provided inside the mass transfer bottle, and a stirring paddle is provided on the surface of the rotating tube. Gaseous hydrofluoric acid corresponding to the interior of the mass transfer bottle is pumped into the mass transfer bottle through the high corrosion-resistant air bag to drive the stirring paddle to stir the liquid raw material.

[0012] Furthermore, the mass transfer box is arranged between the cold recovery box and the hot reflux pipe, the upper surface of the mass transfer box is in conflict with the bottom surface of the heat circulation box, the mass transfer bottle is fixedly connected to the inside of the mass transfer box, and a first one-way valve and a second one-way valve are symmetrically arranged on the surface of the mass transfer box. The first one-way valve is installed in a first circular groove opened on the surface of the mass transfer box, and the air outlet of the first one-way valve is connected to the inlet of the mass transfer bottle through a pipe. The second one-way valve is connected to the inside of the adjacent first one-way valve air inlet through a pipe. The rotating tube is rotatably connected to the inlet of the mass transfer bottle through a first bearing. The surface of the rotating tube is provided with a plurality of branch pipes in an annular array. The branch pipes are fixedly connected to the second circular groove opened on the surface of the rotating tube. The ends of the branch pipes are each installed with a nozzle, and the stirring paddle is fixedly connected to the surface of the rotating tube.

[0013] Furthermore, two porous plates are fixedly connected to the interior of the mass transfer bottle, the stirring paddle is located between the two porous plates, and the rotating tube is located in an avoidance groove opened on the surface of the porous plates.

[0014] Furthermore, the regulating box is fixedly connected to the inner wall of the mass transfer box, a first regulating groove is provided inside the regulating box, the high corrosion-resistant airbags are all fixedly connected to the bottom surface of the regulating box, an electrically-controlled telescopic rod is provided directly below the high corrosion-resistant airbags, the electrically-controlled telescopic rod is 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 provided on the surface of the high corrosion-resistant airbags, the first regulating groove is connected to the interior of the air inlets of the two third one-way valves, the regulating block is slidably connected to the interior of the first regulating groove, a hydrophobic valve is provided inside the mass transfer box, the air inlet of the hydrophobic valve is connected to the outlet of the mass transfer bottle through a pipe, the air outlet of the hydrophobic valve is connected to the interior of the first regulating groove through a pipe, the regulating block is always connected to the interior of the air outlet of the hydrophobic valve, a second regulating groove is provided inside the regulating box, the second regulating groove is connected to the interior of the air inlet of the fourth one-way valve, and the second regulating groove is connected to the interior of the air inlet of the second one-way valve through a pipe.

[0015] Furthermore, an adjusting block is slidably connected to the interior of the mass transfer box, the bottom surface of the adjusting block is in conflict with the upper surface of the top plate, a driving motor is installed on the surface of the mass transfer box, and the output shaft of the driving motor extends to the interior of the mass transfer box through a fourth circular groove opened on the surface of the mass transfer box, and the end of the output shaft of the driving motor is fixedly connected to a first screw rod, which is threadedly connected to the adjusting block through a first threaded hole opened on the surface of the adjusting block.

[0016] Furthermore, a guide plate is fixedly connected to the bottom surface of the top plate, the surface of the guide plate conflicts with the inner wall of the mass transfer box, and the bottom surface of the guide plate does not contact the inner bottom surface of the mass transfer box.

[0017] Furthermore, a plurality of first solenoid valves are provided in a circular array on the surface of the mass transfer box, and a four-way pipe is provided between two adjacent first solenoid valves, two of the pipe openings of the four-way pipe are respectively connected to the interior of one of the valve openings of the two adjacent first solenoid valves through a pipe, and a collecting bottle is provided inside the cold recovery box, one of the pipe openings of the four-way pipe is connected to the interior of the collecting bottle through a pipe, and the last pipe opening of the four-way pipe is installed with a second solenoid valve.

[0018] Furthermore, the surface of the heat return pipe is provided with plug-in grooves in a circular array, and a plug-in tube is fixedly connected to the sixth circular groove provided on the surface of the mass transfer box. The upper surface of the heat return pipe conflicts with the internal top surface of the heat circulation box. The bottom surface of the heat return pipe is provided with a first connecting groove in a circular array, and a flow equalizing plate is fixedly connected to the interior of the heat circulation box, and the surface of the flow equalizing plate conflicts with the surface of the heat return pipe.

[0019] Furthermore, two regulating air pipes are provided on the surface of the heat circulation box, and the regulating air pipes are fixedly connected to the heat circulation box through a fifth circular groove opened on the surface of the heat circulation box. The interior of one of the regulating air pipes is connected to the interior of the heat circulation box, and the interior of the other regulating air pipe is connected to the interior of the heat return pipe. A movable plug is slidably connected to the interior of the regulating air pipe, and an electric push rod is installed in the seventh circular groove opened on the upper surface of the regulating air pipe, and the end of the output shaft of the electric push rod is fixedly connected to the movable plug.

[0020] The above solution of the present invention includes at least the following beneficial effects:

[0021] The above-mentioned solution of the present invention effectively improves the mass transfer efficiency between gaseous hydrofluoric acid and liquid raw materials by setting internal connections between multiple mass transfer bottles and combining them with temperature-controlled airflow heating, optimizes the distillation process, and reduces energy consumption; uses a highly corrosion-resistant airbag and an electrically controlled telescopic rod to adjust the flow of hydrofluoric acid, which helps to accurately control the gas entry rate, thereby ensuring stable air pressure and effective stirring of the liquid raw materials; adopts a dynamic temperature adjustment method to make airflow and temperature control more precise, reduce heat loss, and enhance the capacity of the entire heat exchange device. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the overall structure provided by the present invention.

[0023] Figure 2 It is a schematic diagram of the movable plug in the present invention.

[0024] Figure 3 Schematic diagram of the mass transfer box in the present invention.

[0025] Figure 4 It is a schematic diagram of the heat return pipe in the present invention.

[0026] Figure 5 It is a schematic diagram of the highly corrosion-resistant airbag of the present invention.

[0027] Figure 6 Schematic diagram of the porous plate in the present invention.

[0028] Figure 7 It is a schematic diagram of the adjustment block in the present invention.

[0029] Figure 8 This invention Figure 5 Enlarged view of point A in the middle.

[0030] In the figure: 101, cold recovery box; 102, hot return pipe; 103, hot circulation box;

[0031] 201. Mass transfer box; 202. Mass transfer bottle; 203. First one-way valve; 204. Steam trap; 205. Adjustment box; 206. High-corrosion-resistant airbag; 207. Electric telescopic rod; 208. Second one-way valve; 209. Adjustment block; 210. First adjustment slot; 211. Second adjustment slot; 212. Third one-way valve; 213. Fourth one-way valve; 214. Rotating tube; 215. Branch pipe; 216. Sprinkler; 217. Stirring paddle; 218. Perforated plate; 219. Top plate; 220. Adjustment hole; 221. Adjustment block; 222. Drive motor; 223. Guide plate; 224. Plug-in tube; 225. First screw rod;

[0032] 301, first solenoid valve; 302, four-way pipe; 303, collecting bottle; 304, second solenoid valve;

[0033] 401, regulating air pipe; 402, movable plug; 403, electric push rod; 404, flow equalizing plate; 405, first connecting groove; 406, plug-in groove;

[0034] 501, air inlet pipe; 502, air outlet pipe. DETAILED DESCRIPTION

[0035] The following describes exemplary embodiments of the present disclosure in more detail with reference to the accompanying drawings. Although exemplary embodiments of the present disclosure are shown in the accompanying 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. Rather, these embodiments are provided to enable a more thorough understanding of the present disclosure and to fully convey the scope of the present disclosure to those skilled in the art.

[0036] like Figures 1 to 8 As shown, an embodiment of the present invention provides an electronic grade hydrofluoric acid distillation heat exchange device, including a cold recovery box 101, a surface of which is provided with a heat return pipe 102 and a heat circulation box 103, including:

[0037] A plurality of mass transfer boxes 201 are provided above the cold recovery box 101. Mass transfer bottles 202 are fixedly connected to the interior of the mass transfer boxes 201. The mass transfer bottles 202 are interconnected in sequence. A set temperature airflow is introduced into one of the mass transfer boxes 201 at the end to heat the corresponding mass transfer bottle 202.

[0038] A top plate 219 is fixedly connected to the top of the mass transfer box 201. A plurality of adjustment holes 220 are evenly opened on the surface of the top plate 219. 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 can be adjusted.

[0039] The mass transfer box 201 is provided with an adjustment box 205 inside. The surface of the adjustment box 205 is symmetrically provided with high corrosion-resistant air bags 206. By adjusting the expansion and contraction speed of the two high corrosion-resistant air bags 206, the speed of gaseous hydrofluoric acid entering the mass transfer bottle 202 is regulated.

[0040] An adjusting block 209 is provided inside the adjusting box 205. The adjusting block 209 slides inside the adjusting box 205 to adjust the expansion and contraction of the corresponding high corrosion-resistant airbag 206 on the surface of the adjusting box 205, so as to maintain the stability of the internal air pressure of the corresponding mass transfer bottle 202.

[0041] A rotating tube 214 is provided inside the mass transfer bottle 202, and a stirring paddle 217 is provided on the surface of the rotating tube 214. Gaseous hydrofluoric acid is pumped into the corresponding mass transfer bottle 202 through the high corrosion-resistant air bag 206 to drive the stirring paddle 217 to stir the liquid raw material.

[0042] In an embodiment of the present invention, a multi-stage mass transfer is provided depending on the raw material of the hydrofluoric acid. That is, a plurality of mass transfer bottles 202 are connected in sequence, and one of the mass transfer bottles 202 at the end is heated to a set temperature so that the mass transfer bottle 202 generates sufficient gaseous hydrofluoric acid. The gaseous hydrofluoric acid enters the highly corrosion-resistant airbag 206 through a pipeline, is compressed and deformed by the highly corrosion-resistant airbag 206, and is pumped into the mass transfer bottle 202 of the next stage. The gaseous hydrofluoric acid is then exchanged with the raw material inside the mass transfer bottle 202 of the next stage through the rotating tube 214. The air pressure provided by the compression deformation of the highly corrosion-resistant airbag 206 causes the stirring paddle 217 to rotate, thereby stirring the liquid raw material and improving the mass transfer efficiency.

[0043] After multiple stages of mass transfer, the gaseous hydrofluoric acid discharged from the last stage of mass transfer bottle 202 reaches the set value. It is first passed through a filter to remove impurities such as water and silicon tetrafluoride in the gaseous hydrofluoric acid, and then passed through a condenser for collection.

[0044] If the impurity concentration of the liquid raw material inside the mass transfer bottle 202 reaches the waste liquid level, a group of mass transfer bottles 202 can be added between the last mass transfer bottle 202 and the filtration device, and the mass transfer bottle 202 whose liquid raw material inside reaches the waste liquid level can be removed at the same time, so that the original second-stage mass transfer bottle 202 becomes the first-stage mass transfer bottle 202, and the additional mass transfer bottles 202 are added step by step.

[0045] The specific method of replenishment is to heat the corresponding mass transfer bottle 202 to the set temperature by introducing a set temperature airflow into the corresponding mass transfer box 201. The temperature of the first-stage mass transfer bottle 202 is the highest to provide gaseous hydrofluoric acid. To maintain optimal mass transfer efficiency and concentration driving force, the temperature difference between the gaseous hydrofluoric acid entering each stage and the liquid raw material inside the corresponding mass transfer bottle 202 is controlled between 2 degrees Celsius and 5 degrees Celsius. When replenishing, the mass transfer box 201 where the corresponding mass transfer bottle 202 is located is made to reach the corresponding temperature.

[0046] If the number of mass transfer bottles 202 is limited, the raw material purity can be brought to the set value through multiple rounds of distillation. That is, during the distillation process, the purity of the gaseous hydrofluoric acid flowing out of the last-stage mass transfer bottle 202 is gradually improved by dynamically replacing the mass transfer bottle 202. That is, if the purity of the condensed and collected hydrofluoric acid does not meet the standard, it will be used as the liquid raw material in the additional mass transfer bottle 202 until the hydrofluoric acid purity meets the standard.

[0047] It should be noted that the working principles and usage procedures 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 described in detail here.

[0048] 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 conflicts with the bottom surface of the heat circulation box 103. The mass transfer bottle 202 is fixedly connected to the interior of the mass transfer box 201. The surface of the mass transfer box 201 is symmetrically provided with a first one-way valve 203 and a second one-way valve 208. The first one-way valve 203 is installed in a first circular groove opened on the surface of the mass transfer box 201. The outlet of the first one-way valve 203 is connected to the inlet of the mass transfer bottle 202 through a pipe. The first one-way valve 208 is connected to the air inlet of the adjacent first one-way valve 203 through a pipeline. The rotating tube 214 is rotatably connected to the inlet of the mass transfer bottle 202 through a first bearing. The surface of the rotating tube 214 is provided with a plurality of branch pipes 215 in an annular array. The branch pipes 215 are fixedly connected to the second circular groove opened on the surface of the rotating tube 214. The ends of the branch pipes 215 are respectively installed with nozzles 216. The stirring paddle 217 is fixedly connected to the surface of the rotating tube 214.

[0049] Two porous plates 218 are fixedly connected to the interior of 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 an avoidance groove opened on the surface of the porous plates 218 .

[0050] In the embodiment of the present invention, the porous plate 218 at the bottom is immersed in the liquid raw material, and the porous plate 218 at the top is located above the liquid raw material. After the gaseous hydrofluoric acid enters the mass transfer bottle 202, it enters the interior of the rotating tube 214 and the interior of the branch pipe 215, and finally is ejected from the nozzle 216. After the ejected gaseous hydrofluoric acid passes through the micropores on the surface of the porous plate 218, it more fully exchanges mass with the liquid raw material in the mass transfer bottle 202. At the same time, when the gaseous hydrofluoric acid is ejected from the nozzle 216, the nozzle 216 drives the rotating tube 214 to rotate through the branch pipe 215 under the action of the reaction force, thereby causing the stirring paddle 217 to stir the liquid raw material in the mass transfer bottle 202, further improving the mass transfer efficiency between the gaseous hydrofluoric acid and the liquid raw material. The porous plate 218 at the top is used to reduce foam, stabilize the liquid level and splashing of the liquid raw material, and thus help maintain stable mass transfer efficiency.

[0051] The regulating box 205 is fixedly connected to the inner wall of the mass transfer box 201, and a first regulating groove 210 is provided inside the regulating box 205. The high corrosion resistant airbags 206 are fixedly connected to the bottom surface of the regulating box 205. An electric telescopic rod 207 is provided directly below the high corrosion resistant airbags 206. The electric telescopic rod 207 is installed inside the mass transfer box 201. The third circular groove symmetrically provided on the surface of the high corrosion resistant airbags 206 is respectively installed with a third one-way valve 212 and a fourth one-way valve 213. The first regulating groove 210 is connected to the air inlet of the two third one-way valves 212. The regulating block 209 slides Connected to the interior of the first regulating tank 210, a steam trap 204 is provided inside the mass transfer box 201. The air inlet of the steam trap 204 is connected to the outlet of the mass transfer bottle 202 through a pipeline. The air outlet of the steam trap 204 is connected to the interior of the first regulating tank 210 through a pipeline. The regulating block 209 is always connected to the interior of the air outlet of the steam trap 204. A second regulating tank 211 is provided inside the regulating box 205. The second regulating tank 211 is connected to the interior of the air inlet of the fourth one-way valve 213. The second regulating tank 211 is connected to the interior of the air inlet of the second one-way valve 208 through a pipeline.

[0052] In an 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 material in the mass transfer bottle 202 to ensure that the impurity content of the gaseous hydrofluoric acid is gradually reduced. The gaseous hydrofluoric acid flowing out of the outlet of the mass transfer bottle 202 enters the interior of the regulating box 205 through the steam trap 204 and the pipeline. The gaseous hydrofluoric acid entering the regulating box 205 first enters the regulating block 209 inside the first regulating tank 210, and enters the corresponding high-corrosion-resistant airbag 206 through one of the third one-way valves 212, so that the high-corrosion-resistant airbag 206 continues to expand. A sensor is installed at the output shaft end of the electric-controlled telescopic rod 207 below the high-corrosion-resistant airbag 206. When the electric-controlled telescopic rod 207 touches the sensor, the corresponding electric-controlled telescopic rod 207 is extended to compress the corresponding high-corrosion-resistant airbag 206. The compression of the high-corrosion-resistant airbag 206 causes the gaseous hydrofluoric acid inside it to pass through the fourth The one-way valve 213 enters the interior of the second regulating tank 211, and enters the air inlet of the second one-way valve 208 through the pipeline, and flows through the pipeline to the air inlet of the first one-way valve 203 corresponding to the next-level mass transfer bottle 202. During this process, due to the increase in the internal air pressure of the high-corrosion-resistant airbag 206 in the process of compression deformation, the gaseous hydrofluoric acid entering the regulating block 209 cannot continue to pass through the corresponding third one-way valve 212 to enter the interior of the high-corrosion-resistant airbag 206 that has undergone compression deformation. The gaseous hydrofluoric acid continues to enter the regulating block 209, causing the regulating block 209 to move inside the first regulating tank 210 away from the high-corrosion-resistant airbag 206 that has undergone compression deformation, until the regulating block 209 is connected to the interior of the third one-way valve 212 air inlet on the surface of the other high-corrosion-resistant airbag 206. At this time, the gaseous hydrofluoric acid enters the interior of the other high-corrosion-resistant airbag 206 and causes the high-corrosion-resistant airbag 206 to expand and deform;

[0053] The deformation speed of the high corrosion-resistant airbag 206 is positively correlated with the air pressure pumped into the corresponding mass transfer bottle 202 , thereby being able to regulate the stirring speed of the corresponding stirring paddle 217 .

[0054] An adjusting block 221 is slidably connected to the interior of the mass transfer box 201, and the bottom surface of the adjusting block 221 conflicts with the upper surface of the top plate 219. A driving motor 222 is installed on the surface of the mass transfer box 201, and the output shaft of the driving motor 222 extends to the interior of the mass transfer box 201 through a 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 screw rod 225, and the first screw rod 225 is threadedly connected to the adjusting block 221 through a first threaded hole opened on the surface of the adjusting block 221.

[0055] The bottom surface of the top plate 219 is fixedly connected to a guide plate 223 . The surface of the guide plate 223 contacts the inner wall of the mass transfer box 201 , and the bottom surface of the guide plate 223 does not contact the inner bottom surface of the mass transfer box 201 .

[0056] In the embodiment of the present invention, hot air generated by the external heating device is passed into the interior of the mass transfer box 201 and into the top of the top plate 219. The hot air flow entering the top plate 219 enters the interior of the mass transfer box 201 through the regulating hole 220. After being guided by the guide plate 223, the hot air flow first passes over the surface of the mass transfer bottle 202, heating the mass transfer bottle 202. This improves the response efficiency of the hot air flow in regulating the temperature of the mass transfer bottle 202, allowing the temperature of the mass transfer bottle 202 to change rapidly with changes in the flow rate of the hot air flow.

[0057] By energizing the drive motor 222, the drive motor 222 drives the first screw rod 225 to rotate. The rotation of the first screw rod 225 causes the adjustment block 221 to move on the upper surface of the top plate 219, thereby changing the degree of blockage of the adjustment hole 220 by the adjustment block 221, thereby adjusting the flow rate of the hot air flow entering the mass transfer box 201 through the adjustment hole 220.

[0058] The surface of the mass transfer box 201 is provided with a plurality of first solenoid valves 301 in a circular array, and a four-way pipe 302 is provided between each adjacent first solenoid valve 301. Two of the pipe openings of the four-way pipe 302 are connected to the interior of one of the valve openings of the two adjacent first solenoid valves 301 through a pipe. A collecting bottle 303 is provided inside the cold recovery box 101, and one of the pipe openings of the four-way pipe 302 is connected to the interior of the collecting bottle 303 through a pipe. The last pipe opening of the four-way pipe 302 is installed with a second solenoid valve 304.

[0059] In the embodiment of the present invention, the gas outlet of the second one-way valve 208 corresponding to the last-stage mass transfer bottle 202 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. All other first solenoid valves 301 and second solenoid valves 304 are in a closed state. That is, the gas outlet of the second one-way valve 208 corresponding to the last-stage mass transfer bottle 202 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.

[0060] The gaseous hydrofluoric acid entering the collecting bottle 303 flows to the external filtering equipment and condensing equipment through the pipeline arranged at the bottom of the collecting bottle 303. When it is necessary to add a mass transfer bottle 202, the added mass transfer box 201 is placed on the 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 the pipeline, so that the second solenoid valve 304 connected to the added second one-way valve 208 is in the open state, and the second solenoid valve 304 corresponding to the original last-stage mass transfer bottle 202 is closed, thus completing the addition of the mass transfer bottle 202.

[0061] The surface of the heat return pipe 102 is provided with a plug-in groove 406 in a circular array, and the plug-in tube 224 is fixedly connected to the sixth circular groove provided on the surface of the mass transfer box 201. The upper surface of the heat return pipe 102 conflicts with the internal top surface of the heat circulation box 103. The bottom surface of the heat return pipe 102 is provided with a first connecting groove 405 in a circular array. The interior of the heat circulation box 103 is fixedly connected with a flow equalizing plate 404, and the surface of the flow equalizing plate 404 conflicts with the surface of the heat return pipe 102.

[0062] Two regulating air pipes 401 are provided 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 groove opened on the surface of the heat circulation box 103. The interior of one regulating air pipe 401 is connected to the interior of the heat circulation box 103, and the interior of the other regulating air pipe 401 is connected to the interior of the heat return pipe 102. A movable plug 402 is slidably connected to the interior of the regulating air pipe 401. An electric push rod 403 is installed in the seventh circular groove opened on the upper surface of the regulating air pipe 401, and the end of the output shaft of the electric push rod 403 is fixedly connected to the movable plug 402.

[0063] In this embodiment of the present invention, the mass transfer box 201 is placed on the upper surface of the cold recovery box 101, and the plug-in tube 224 on the surface of the mass transfer box 201 is inserted into one of the plug-in grooves 406 on the surface of the hot return pipe 102. The interior of the mass transfer box 201 is connected to the interior of the hot return pipe 102 through the plug-in tube 224, and the mass transfer box 201 is connected to the interior of one of the first connecting grooves 405 on the bottom surface of the thermal circulation box 103.

[0064] After several mass transfer boxes 201 are sequentially arranged in the above manner, the remaining first communication slots 405 and plugging slots 406 that are not connected to the interior of the mass transfer box 201 are blocked. In this embodiment, the blocking method is to use a sealing plug to block the hot air generated by the heating equipment through the air pump and the pipeline into the air inlet pipe 501, and then enter the interior of the thermal circulation box 103 through the air inlet pipe 501. After being evenly distributed by the flow equalizing plate 404, the hot air enters the interior of the corresponding mass transfer box 201 through the unblocked first communication slots 405;

[0065] When adjusting the blockage of the regulating hole 220 by the regulating block 221 to adjust the flow rate of the hot airflow entering the corresponding mass transfer box 201, in order to maintain a stable air pressure inside the thermal circulation box 103, the flow rate of the hot airflow entering the mass transfer box 201 is positively correlated with the effective cross-sectional area of ​​the airflow actually passing through the regulating hole 220, that is, the effective communication area between the regulating hole 220 and the interior of the mass transfer box 201. The movable plug 402 inside the regulating air pipe 401 is moved by the extension and contraction of the electric push rod 403, thereby reducing the air pressure fluctuations inside the thermal circulation box 103 and the heat return pipe 102, thereby improving the regulation accuracy of the temperature inside the mass transfer box 201.

[0066] The hot air flow entering the mass transfer box 201 flows back through the plug-in tube 224 to the inside of the heat return pipe 102 and then flows back through the outlet pipe 502 to the heating device to reduce heat loss.

[0067] If the temperature of the mass transfer bottle 202 is set to gradually decrease, air cooling can be used to cool the surface of the corresponding mass transfer box 201, thereby cooling the mass transfer bottle 202 inside it. The use of air cooling is well known in the prior art and will not be described in detail here.

[0068] It should be noted that the heat return pipe 102 is fixed on the upper surface of the cold recovery box 101 and is fixedly connected to the heat circulation box 103 through a second reserved opening opened on the bottom surface of the heat circulation box 103 to form an air flow channel.

[0069] The connection method of the pipe is to fix the end of the pipe in the reserved opening by opening a reserved opening so that the pipe is connected to the inside of the reserved opening. This is well known in the prior art and will not be described in detail here.

[0070] The bottom end of the rotating tube 214 is closed, which facilitates the gaseous hydrofluoric acid to enter the interior of the branch pipe 215 through the rotating tube 214;

[0071] The guide plate 223 is formed by a threaded sleeve and a plurality of blocking blocks fixed to the threaded sleeve by rectangular blocks. The shape and arrangement of the blocking blocks correspond to the adjustment hole 220, making it easy to adjust the blockage of the adjustment hole 220 by the blocking block 221. The surface of the guide plate 223 is provided with an avoidance hole to facilitate the passage of the pipe through the guide plate 223.

[0072] The working principle and use process of the heating device and the air pump are well known in the prior art and will not be described in detail here;

[0073] The upper surface of the regulating air pipe 401 is evenly provided with vent holes for balancing the air pressure inside the regulating air pipe 401;

[0074] The working principle and usage process of the sensor are well known in the prior art and will not be described in detail here.

[0075] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. An electronic grade hydrofluoric acid distillation heat exchange device, comprising a cold recovery box (101), wherein a heat return pipe (102) and a heat circulation box (103) are provided on the surface of the cold recovery box (101), characterized in that: include: A plurality of mass transfer boxes (201) are provided above the cold recovery box (101), and a mass transfer bottle (202) is fixedly connected to the interior of the mass transfer box (201). The mass transfer bottles (202) are interconnected in sequence, and a set temperature airflow is introduced into the interior of one of the mass transfer boxes (201) located at the end to heat the corresponding mass transfer bottle (202); A top plate (219) is fixedly connected to the top of the mass transfer box (201), and a plurality of adjustment holes (220) are evenly opened on the surface of the top plate (219). 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) can be adjusted; The mass transfer box (201) is provided with an adjustment box (205) inside, and the surface of the adjustment box (205) is symmetrically provided with high corrosion-resistant air bags (206). By adjusting the expansion and contraction speed of the two high corrosion-resistant air bags (206), the speed at which the gaseous hydrofluoric acid enters the mass transfer bottle (202) is regulated; An adjusting block (209) is provided inside the adjusting box (205), and the adjusting block (209) slides inside the adjusting box (205) to adjust the expansion and contraction of the corresponding high corrosion-resistant airbag (206) on the surface of the adjusting box (205) to maintain the stability of the internal air pressure of the corresponding mass transfer bottle (202); A rotating tube (214) is provided inside the mass transfer bottle (202), and a stirring paddle (217) is provided on the surface of the rotating tube (214). Gaseous hydrofluoric acid corresponding to the interior of the mass transfer bottle (202) is pumped into the high corrosion-resistant air bag (206) to drive the stirring paddle (217) to stir the liquid raw material.

2. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 1, characterized in that: The mass transfer box (201) is arranged between the cold recovery box (101) and the heat return pipe (102), the upper surface of the mass transfer box (201) is in conflict with the bottom surface of the heat circulation box (103), the mass transfer bottle (202) is fixedly connected to the inside of the mass transfer box (201), and the surface of the mass transfer box (201) is symmetrically provided with a first one-way valve (203) and a second one-way valve (208), the first one-way valve (203) is installed in a first circular groove opened on the surface of the mass transfer box (201), and the gas outlet of the first one-way valve (203) is connected to the mass transfer bottle (208) through a pipeline. 2), 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 tube (214) is rotatably connected to the inlet of the mass transfer bottle (202) through a first bearing, the surface of the rotating tube (214) is provided with a plurality of branch pipes (215) in an annular array, the branch pipes (215) are fixedly connected to the second circular groove opened on the surface of the rotating tube (214), the ends of the branch pipes (215) are each installed with a nozzle (216), and the stirring paddle (217) is fixedly connected to the surface of the rotating tube (214).

3. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 2, characterized in that: Two porous plates (218) are fixedly connected to the interior of 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 an avoidance groove opened on the surface of the porous plates (218).

4. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 3, characterized in that: The regulating box (205) is fixedly connected to the inner wall of the mass transfer box (201), and a first regulating groove (210) is provided inside the regulating box (205). The high corrosion resistant airbags (206) are fixedly connected to the bottom surface of the regulating box (205), and an electric telescopic rod (207) is provided directly below the high corrosion resistant airbags (206). The electric telescopic rod (207) is 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 groove symmetrically provided on the surface of the high corrosion resistant airbag (206). The first regulating groove (210) is connected to the inside of the air inlet of the two third one-way valves (212). The regulating block (209) slides Connected to the interior of the first regulating tank (210), a steam trap (204) is provided inside the mass transfer box (201), the air inlet of the steam trap (204) is connected to the outlet of the mass transfer bottle (202) through a pipeline, the air outlet of the steam trap (204) is connected to the interior of the first regulating tank (210) through a pipeline, the regulating block (209) is always connected to the interior of the air outlet of the steam trap (204), a second regulating tank (211) is provided inside the regulating box (205), the second regulating tank (211) is connected to the interior of the air inlet of the fourth one-way valve (213), and the second regulating tank (211) is connected to the interior of the air inlet of the second one-way valve (208) through a pipeline.

5. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 4, characterized in that: The mass transfer box (201) is internally slidably connected to an adjusting block (221), the bottom surface of the adjusting block (221) is in conflict with the upper surface of the top plate (219), and a driving motor (222) is installed on the surface of the mass transfer box (201), and the output shaft of the driving motor (222) extends to the interior of the mass transfer box (201) through a fourth circular groove opened on the surface of the mass transfer box (201), and the end of the output shaft of the driving motor (222) is fixedly connected to a first screw rod (225), and the first screw rod (225) is threadedly connected to the adjusting block (221) through a first threaded hole opened on the surface of the adjusting block (221).

6. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 5, characterized in that: The bottom surface of the top plate (219) is fixedly connected to a guide plate (223), the surface of the guide plate (223) is in conflict with the inner wall of the mass transfer box (201), and the bottom surface of the guide plate (223) does not contact the inner bottom surface of the mass transfer box (201).

7. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 6, characterized in that: The surface of the mass transfer box (201) is provided with a plurality of first solenoid valves (301) in a ring array, a four-way pipe (302) is provided between two adjacent first solenoid valves (301), two of the pipe openings of the four-way pipe (302) are respectively connected to the interior of one of the valve openings of the two adjacent first solenoid valves (301) through a pipe, a collecting bottle (303) is provided inside the cold recovery box (101), one of the pipe openings 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 opening of the four-way pipe (302).

8. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 7, characterized in that: The surface of the heat return pipe (102) is provided with a plug-in groove (406) in an annular array, and a plug-in pipe (224) is fixedly connected to the sixth circular groove provided on the surface of the mass transfer box (201). The upper surface of the heat return pipe (102) is in conflict with the internal top surface of the heat circulation box (103). The bottom surface of the heat return pipe (102) is provided with a first connecting groove (405) in an annular array. A flow equalizing plate (404) is fixedly connected to the interior of the heat circulation box (103), and the surface of the flow equalizing plate (404) is in conflict with the surface of the heat return pipe (102).

9. The electronic-grade hydrofluoric acid distillation heat exchange device according to claim 8, characterized in that: Two regulating air pipes (401) are provided on the surface of the heat circulation box (103), and the regulating air pipes (401) are fixedly connected to the heat circulation box (103) through a fifth circular groove opened on the surface of the heat circulation box (103), the interior of one of the regulating air pipes (401) is connected to the interior of the heat circulation box (103), and the interior of the other regulating air pipe (401) is connected to the interior of the heat return pipe (102), and the interior of the regulating air pipe (401) is slidably connected to a movable plug (402), and an electric push rod (403) is installed in the seventh circular groove opened on the upper surface of the regulating air pipe (401), and the end of the output shaft of the electric push rod (403) is fixedly connected to the movable plug (402).

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