A continuous production equipment for electronic grade sulfuric acid
By adopting multiple absorption and gas-liquid reverse contact design of mixing barrels and mixed spray towers in electronic-grade sulfuric acid production equipment, the problem of low fusion efficiency of sulfur trioxide gas and ultrapure water under normal pressure is solved, and high-efficiency sulfuric acid is achieved Production reduces the exhaust gas treatment load.
Patent Information
- Application Number
- CN202411092049.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-09
- Publication Date
- 2025-01-07
- Estimated Expiration
- 2044-08-09
AI Technical Summary
The existing electronic-grade sulfuric acid production equipment has low fusion efficiency of sulfur trioxide gas and ultrapure water at normal pressure, resulting in low production efficiency of high-purity sulfuric acid.
An electronic-grade sulfuric acid continuous production equipment was designed, using a mixing barrel and a mixed spray tower. Through multiple absorption mechanisms and gas-liquid reverse contact methods, the contact area and contact time of sulfur trioxide gas and ultrapure water are improved, and water is used. The interaction between pressure and air pressure increases the fusion pressure and improves absorption efficiency through structures such as stirring and reducer plates.
The fusion efficiency of sulfur trioxide gas and ultrapure water is significantly improved, the sulfur trioxide content in the waste gas is reduced, the workload of the waste gas treatment mechanism is reduced, and the resource utilization rate is improved.
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Figure CN118877839B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of sulfuric acid production equipment, in particular to a continuous production equipment for electronic-grade sulfuric acid. Background Art
[0002] Electronic grade sulfuric acid, commonly known as electronic grade pure sulfuric acid or high purity sulfuric acid, is a high purity chemical. Electronic grade sulfuric acid is also widely used in the manufacture and maintenance of other precision electronic equipment, such as liquid crystal displays, photovoltaic cells, etc. Its importance lies not only in its chemical properties, but also in its purity and reliability. These properties directly affect the performance and life of modern electronic products, and thus it plays a vital role in the electronics industry and semiconductor manufacturing. The production processes of electronic grade sulfuric acid mainly include distillation and gas absorption. The gas absorption method is to pass sulfur trioxide gas into ultrapure water, so that ultrapure water absorbs sulfur trioxide gas to form high purity sulfuric acid liquid. At present, when ultrapure water absorbs sulfur trioxide gas, sulfur trioxide gas is passed into a mixing tank filled with ultrapure water under normal pressure, and then sulfur trioxide gas is fused with ultrapure water by stirring and atomizing. However, under normal pressure, sulfur trioxide gas and ultrapure water merge slowly, resulting in low production efficiency of high purity sulfuric acid.
[0003] The invention patent with patent number CN117886279B discloses an electronic grade sulfuric acid production equipment, including: a primary absorption mechanism, a secondary absorption mechanism, a discharge mechanism, and a mixing mechanism. The primary absorption mechanism includes a mixing barrel body and an axial flow cover and an axial flow fan blade arranged inside the mixing barrel body. The secondary absorption mechanism includes a circulating barrel body and a first circulating air pump connected to the circulating barrel body. The discharge mechanism includes a discharge pipe and a sealing plate arranged inside the discharge pipe. The mixing mechanism includes a second air outlet pipe arranged inside the mixing barrel body and a diffuser cover arranged at the end of the second air outlet pipe. By circulating sulfur trioxide gas, the circulated sulfur trioxide gas enters the top of the second chamber, pushing the ultrapure water inside the second chamber to move toward the inside of the first chamber. Under the reaction force of the ultrapure water, the air pressure inside the second chamber increases, thereby increasing the pressure of the fusion of ultrapure water and sulfur trioxide gas inside the second chamber. This invention patent uses two circulating air pumps to make sulfur trioxide gas merge and absorb with ultrapure water multiple times in the circulating barrel and the mixing barrel, and uses the interaction between air pressure and water pressure to increase the absorption rate of sulfur trioxide gas by ultrapure water.
[0004] However, the technical means used in the above invention to improve the absorption rate of sulfur trioxide gas by ultrapure water is still relatively weak. In addition to the above technical means, the following methods can be used to promote the efficient absorption of sulfur trioxide gas by ultrapure water: 1. Step-by-step feeding, slowly introducing sulfur trioxide gas into ultrapure water in batches, so that the absorption is more efficient and uniform; 2. Improving the design of the absorption tower, the contact area between sulfur trioxide gas and ultrapure water can be increased by reverse gas-liquid contact, thereby improving the fusion efficiency; 3. Controlling the gas flow rate, by controlling the flow rate of sulfur trioxide gas, so that it is slowly and evenly introduced into ultrapure water, the absorption efficiency can be improved and the content of sulfur trioxide in the waste gas can be reduced; 4. Stirring or oscillating, by stirring or oscillating the solution, the contact area and contact time between gas and water can be increased, thereby improving the fusion rate. For this reason, the present invention combines and optimizes the above technical means to provide an electronic grade sulfuric acid continuous production equipment. Summary of the invention
[0005] The purpose of the present invention is to solve the problems existing in the above-mentioned background technology, and the present invention provides a continuous production equipment for electronic grade sulfuric acid.
[0006] The present invention achieves the above-mentioned purpose through the following technical scheme: Provide an electronic grade sulfuric acid continuous production equipment, including a mixing barrel and a mixing spray tower, wherein the mixing barrel and the mixing spray tower are jointly provided with an absorption mechanism for multiple fusion of sulfur trioxide gas and ultrapure water; wherein the mixing barrel is provided with a primary absorption mechanism, wherein the primary absorption mechanism comprises a double-layer gas-liquid box, wherein the gas transmission layer of the upper layer of the double-layer gas-liquid box is connected with a gas transmission component for transporting sulfur trioxide gas to ultrapure water, and the water sprinkling layer of the lower layer of the double-layer gas-liquid box is connected with a water absorption component for sucking ultrapure water into the interior, when the gas pressure in the mixing barrel increases, the ultrapure water is squeezed into the water sprinkling layer and sprayed out, and the double-layer gas-liquid box is connected with a first stirring component, and the first stirring component scatters the water droplets sprayed by the water sprinkling layer while stirring the ultrapure water to increase the contact area between gas and liquid; the mixing spray tower is divided into an upper part A spray layer and a lower mixing layer, the mixing layer is connected to the mixing barrel through an air supply pipe, a secondary absorption mechanism is arranged in the mixing layer, the secondary absorption mechanism is arranged to slow down the flow rate of sulfur trioxide gas so that it is slowly and evenly passed into ultrapure water to improve the absorption rate, the secondary absorption mechanism includes an air supply reduction box, the air supply reduction box is provided with a spiral baffle for slowing down the flow rate of sulfur trioxide gas, the bottom of the air supply reduction box is connected to a plurality of exhaust pipes, and a second stirring component is arranged on one side of the exhaust pipe; a circulating water supply system connecting the mixing layer and the spray layer is arranged on one side of the mixing spray tower, a tertiary absorption mechanism is arranged in the spray layer, the tertiary absorption mechanism is arranged to increase the contact area between sulfur trioxide gas and ultrapure water by reverse contact between gas and liquid, the tertiary absorption mechanism includes a spray component connected to the circulating water supply system and a guide component for making gas and liquid fully contact.
[0007] Furthermore, the gas delivery component includes two first connecting columns symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box, one end of two of the four first connecting columns located on the same side is fixedly connected to the air supply pipe, one end of the two air supply pipes are connected to the gas delivery layer, and the other ends of the two air supply pipes are connected to an annular tube, and a plurality of air outlets are evenly arranged at equal angles on the bottom of the annular tube; the outer wall of the water sprinkling layer is connected to the water absorption component, and the water absorption component includes two second connecting columns symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box, one end of two of the four second connecting columns located on the same side is fixedly connected to the water absorption pipe, one end of the two water absorption pipes are connected to the water sprinkling layer, and the other ends of the two water absorption pipes are immersed under the water surface of the ultrapure water in the mixing barrel; four nozzles connected to the water sprinkling layer are installed at equal angles on the bottom of the double-layer gas-liquid box.
[0008] Furthermore, the double-layer gas-liquid box is an annular box and a sealed bearing is installed in the middle gap, and the double-layer gas-liquid box is connected and installed on the inner top of the mixing barrel through a fixed column; the first stirring assembly includes a first motor fixedly installed on the top surface of the mixing barrel, and the output end of the first motor is fixedly connected to a first stirring shaft, the first stirring shaft passes through the sealed bearing and is connected to the inner ring of the sealed bearing, and a plurality of first stirring blades are fixedly installed on the first stirring shaft below the ultrapure water surface, and an impact fan for scattering water droplets is fixedly installed on the first stirring shaft near the nozzle, and the impact fan includes four blades arranged at equal angles and inclined, and a plurality of raised impact bumps are provided on the fan surfaces on both sides of each blade.
[0009] Furthermore, the secondary absorption mechanism also includes a mounting plate installed on the inner wall of the mixing layer, the air transmission reduction box is installed on the mounting plate, the air transmission pipe passes through the mixing layer and is connected to the air transmission reduction box, one end of the air transmission pipe is connected to the inner circle of the spiral baffle; six exhaust pipes are equiangularly connected and installed at the bottom of the air transmission reduction box, one end of the exhaust pipe is connected to the outer circle of the spiral baffle, the exhaust pipe is trumpet-shaped and a plurality of exhaust holes are evenly arranged on the pipe wall at the other end; the second stirring assembly includes a second motor installed at the bottom of the air transmission reduction box, the output end of the second motor is fixedly connected to a second stirring shaft, and a plurality of second stirring blades are installed on the second stirring shaft.
[0010] Furthermore, a partition for separating the spray layer and the mixing layer is connected and installed on the inner wall of the mixing spray tower, a plurality of through holes are opened at equal angles on the partition, a mounting box is connected to the bottom of the partition, a telescopic cylinder is installed in the mounting box, a closing component for closing the through holes is connected to one end of the telescopic rod of the telescopic cylinder, the closing component includes a top plate installed at one end of the telescopic rod of the telescopic cylinder, connecting rods are connected to the top plate at equal angles, and a sealing plug matching the position and number of the through holes is connected to one end of the connecting rod.
[0011] Furthermore, the circulating water supply system includes a water supply pipe connected to the bottom of the mixing spray tower, a water pump is connected to one side of the water supply pipe, the output end of the water pump is connected to a water supply pipe, a first water branch pipe and a second water branch pipe are connected to the side wall of the water supply pipe, the other ends of the first water branch pipe and the second water branch pipe both pass through the side wall of the mixing spray tower and are connected to the spray assembly; valves are provided on the water supply pipe, the first water branch pipe and the second water branch pipe.
[0012] Furthermore, the spray assembly includes a spray pipe and an atomizing nozzle, and the atomizing nozzle is evenly distributed at the bottom of the spray pipe.
[0013] Furthermore, the guide assembly is connected and installed on the inner wall of the spray layer, and the guide assembly includes a guide ring. The guide ring is truncated cone-shaped and the top diameter is larger than the bottom diameter. A plurality of guide grooves are provided at equal angles on the inner surface of the guide ring. The bottom of the guide ring is connected and installed with an upwardly protruding arc-shaped guide plate, and a plurality of guide holes are provided on the guide plate.
[0014] Furthermore, an air pump is installed on the gas supply pipe, and a first solenoid valve is installed at one end of the gas supply pipe close to the top of the mixing barrel; an air intake pipe is connected through the outer wall of the top of the mixing barrel, the air intake pipe is connected to the gas supply layer, and a second solenoid valve is installed on the air intake pipe; a first pressure gauge for detecting the air pressure is installed on the outer wall of the mixing barrel, and a second pressure gauge for detecting the air pressure in the mixing layer is installed on the outer wall of the mixing spray tower.
[0015] Furthermore, an activated carbon plate is provided above the second water distribution pipe near the top of the mixing spray tower, a wire mesh demister is provided between the second water distribution pipe and the first water distribution pipe, a filling layer is provided between the first water distribution pipe and the partition, and the guide assembly is installed below the filling layer.
[0016] Compared with the prior art, the present invention has the following beneficial effects:
[0017] 1. In the present invention, an absorption mechanism for fusing sulfur trioxide gas and ultrapure water multiple times is jointly provided in the mixing barrel and the mixing spray tower; on the one hand, sulfur trioxide gas is directly introduced into ultrapure water, and the pressure of fusing sulfur trioxide gas and ultrapure water is increased under the interaction of water pressure and air pressure; on the other hand, the primary absorption mechanism squeezes ultrapure water into the water sprinkling layer and sprays it out after the air pressure in the mixing barrel increases, and utilizes the first stirring component to scatter the water droplets sprayed by the water sprinkling layer while stirring the ultrapure water, so as to increase the contact area between gas and liquid, thereby improving the fusion efficiency of ultrapure water and sulfur trioxide gas.
[0018] 2. A secondary absorption mechanism is provided in the mixing layer. The secondary absorption mechanism is configured to slow down the flow rate of sulfur trioxide gas so that it can be slowly and evenly passed into ultrapure water to improve the absorption rate. The designed spiral baffle and trumpet-shaped exhaust pipe allow sulfur trioxide gas to be slowly and evenly passed into ultrapure water, thereby improving the absorption fusion efficiency of the two.
[0019] 3. A tertiary absorption mechanism is provided in the spray layer. The tertiary absorption mechanism is configured to increase the contact area between sulfur trioxide gas and ultrapure water by means of gas-liquid reverse contact. The guide component increases the contact area between the sulfur trioxide gas and the ultrapure water sprayed down during the rising process, thereby improving the fusion efficiency of ultrapure water and sulfur trioxide gas.
[0020] 4. After the multi-stage efficient absorption of sulfur trioxide gas by ultrapure water, the sulfur trioxide content in the sulfur trioxide gas is lower, so that the sulfur trioxide content in the discharged waste gas is lower, which reduces the workload of the waste gas treatment agency and reduces the waste of resources. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a schematic diagram of the overall structure of the present invention;
[0022] Figure 2 is a cross-sectional view of the present invention;
[0023] Figure 3 It is a schematic diagram of the internal structure of the mixing barrel in the present invention;
[0024] Figure 4 A top view of the mixing barrel of the present invention;
[0025] Figure 5 for Figure 4 Sectional view of AA in the middle;
[0026] Figure 6 is a schematic diagram of an impact fan in the present invention;
[0027] Figure 7 It is a schematic diagram of the internal structure of the mixing spray tower in the present invention;
[0028] Figure 8 is a schematic diagram of the secondary absorption structure of the present invention;
[0029] Fig. 9 is a schematic diagram of the secondary absorption structure of the present invention;
[0030] Fig.10 An exploded view of the partition and the closure assembly of the present invention;
[0031] Fig.11 It is a schematic diagram of the flow guide component in the present invention.
[0032] In the figure: 1-mixing barrel, 2-mixing spray tower, 3-primary absorption mechanism, 4-spraying layer, 5-mixing layer, 6-air delivery pipe, 7-secondary absorption mechanism, 8-circulating water delivery system, 9-tertiary absorption mechanism, 10-partition, 11-through port, 12-installation box, 13-telescopic cylinder, 14-closing assembly, 15-air pump, 16-first solenoid valve, 17-intake pipe, 18-second solenoid valve, 19-first pressure gauge, 20-second pressure gauge, 21-activated carbon plate, 22-wire mesh demister, 23-filling layer;
[0033] 31-double-layer gas-liquid box, 32-gas delivery component, 33-water absorption component, 34-first stirring component, 35-sealed bearing, 36-fixed column, 311-gas delivery layer, 312-water sprinkling layer, 313-sprinkler, 321-first connecting column, 322-air delivery pipe, 323-annular pipe, 331-second connecting column, 332-water absorption pipe, 341-first motor, 342-first stirring shaft, 343-first stirring blade, 344-impact fan, 3231-air outlet, 3441-fan blade, 34411-impact convex point;
[0034] 71-air transmission reduction box, 72-exhaust pipe, 73-second stirring assembly, 74-mounting plate, 711-spiral baffle, 721-exhaust hole, 731-second motor, 732-second stirring shaft, 733-second stirring blade;
[0035] 81- water delivery pipe, 82- water pump, 83- water delivery pipe, 84- first water distribution pipe, 85- second water distribution pipe, 86- valve;
[0036] 91-spray assembly, 92-guide assembly, 911-spray pipe, 912-atomizing nozzle, 921-guide ring, 922-guide plate, 9211-guide groove, 9221-guide hole;
[0037] 141 - top plate, 142 - connecting rod, 143 - sealing plug. DETAILED DESCRIPTION
[0038] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0039] In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.
[0040] Combination Figures 1 to 11The electronic grade sulfuric acid continuous production equipment shown in the figure comprises a mixing barrel 1 and a mixing spray tower 2, wherein the mixing barrel 1 and the mixing spray tower 2 are jointly provided with an absorption mechanism for fusing sulfur trioxide gas with ultrapure water for multiple times; wherein the mixing barrel 1 is provided with a primary absorption mechanism 3, the primary absorption mechanism 3 comprises a double-layer gas-liquid box 31, the gas transmission layer 311 of the upper layer of the double-layer gas-liquid box 31 is connected with a gas transmission component 32 for transporting sulfur trioxide gas to ultrapure water, the water sprinkling layer 312 of the lower layer of the double-layer gas-liquid box 31 is connected with a water absorption component 33 for sucking ultrapure water into the interior, when the gas pressure in the mixing barrel 1 increases, the ultrapure water is squeezed into the water sprinkling layer 312 and sprayed out, the double-layer gas-liquid box 31 is connected with a first stirring component 34, the first stirring component 34 scatters the water droplets sprayed by the water sprinkling layer 312 while stirring the ultrapure water to increase the contact area between gas and liquid; the mixing spray tower 2 is divided into an upper spray layer 4 and a lower spray layer 5. The mixing layer 5 is connected to the mixing barrel 1 through the gas pipe 6. The mixing layer 5 is provided with a secondary absorption mechanism 7. The secondary absorption mechanism 7 is configured to slow down the flow rate of sulfur trioxide gas so that it is slowly and evenly passed into the ultrapure water to improve the absorption rate. The secondary absorption mechanism 7 includes a gas transmission reduction box 71. The gas transmission reduction box 71 is provided with a spiral baffle 711 for slowing down the flow rate of sulfur trioxide gas. The bottom of the gas transmission reduction box 71 is connected to a plurality of exhaust pipes 72. A second stirring component 73 is provided on one side of the exhaust pipe 72; a circulating water supply system 8 connecting the mixing layer 5 and the spray layer 4 is provided on one side of the mixing spray tower 2. A tertiary absorption mechanism 9 is provided in the spray layer 4. The tertiary absorption mechanism 9 is configured to increase the contact area between sulfur trioxide gas and ultrapure water by reverse contact between gas and liquid. The tertiary absorption mechanism 9 includes a spray component 91 connected to the circulating water supply system 8 and a flow guide component 92 for fully contacting gas and liquid;
[0041] Reference Figure 1-6As shown, the gas delivery component 32 includes two first connecting columns 321 symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box 31, one end of two first connecting columns 321 located on the same side among the four first connecting columns 321 is fixedly connected to the gas supply pipe 322, one end of the two gas supply pipes 322 are both connected to the gas delivery layer 311, and the other ends of the two gas supply pipes 322 are connected with an annular tube 323, and a plurality of gas outlets 3231 are evenly arranged at equal angles at the bottom of the annular tube 323; a water absorption component 33 is connected to the outer wall of the water sprinkling layer 312, and the water absorption component 33 includes two second connecting columns 331 symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box 31, one end of two second connecting columns 331 located on the same side among the four second connecting columns 331 is fixedly connected to the water absorption pipe 332, one end of the two water absorption pipes 332 are both connected to the water sprinkling layer 312, and the other ends of the two water absorption pipes 332 are both immersed under the water surface of the ultrapure water in the mixing barrel 1; Four nozzles 313 connected to the watering layer 312 are installed at equal angles at the bottom of the double-layer gas-liquid box 31; the double-layer gas-liquid box 31 is an annular box and a sealed bearing 35 is installed in the middle gap, and the double-layer gas-liquid box 31 is connected and installed on the inner top of the mixing barrel 1 through a fixing column 36; the first stirring component 34 includes a first motor 341 fixedly installed on the top surface of the mixing barrel 1, and the output end of the first motor 341 is fixedly connected to a first stirring shaft 342, and the first stirring shaft 342 passes through the sealed bearing 35 and is connected to the inner ring of the sealed bearing 35. A plurality of first stirring blades 343 are fixedly installed on the first stirring shaft 342 located below the ultrapure water surface, and an impact fan 344 for scattering water droplets is fixedly installed on the first stirring shaft 342 near the nozzle 313. The impact fan 344 includes four blades 3441 arranged at equal angles and inclined, and a plurality of raised impact bumps 34411 are provided on the fan surfaces on both sides of each blade 3441;
[0042] An air pump 15 is installed on the air delivery pipe 6, and a first solenoid valve 16 is installed at one end of the air delivery pipe 6 close to the top of the mixing barrel 1; an air inlet pipe 17 is connected through the outer wall of the top of the mixing barrel 1, and the air inlet pipe 17 is connected to the air delivery layer 311, and a second solenoid valve 18 is installed on the air inlet pipe 17; a first pressure gauge 19 for detecting air pressure is installed on the outer wall of the mixing barrel 1, and a second pressure gauge 20 for detecting air pressure in the mixing layer 5 is installed on the outer wall of the mixing spray tower 2;
[0043] Embodiment 1:
[0044] The sulfur trioxide gas is transported to the gas transmission layer 311 of the upper layer of the double-layer gas-liquid box 31 through the air inlet pipe 17, and then transported to the annular tube 323 through the air supply pipe 322, and discharged from the multiple uniformly arranged gas outlets 3231 at the bottom of the annular tube 323, and merges with the ultrapure water during the rising process, wherein the water level of the ultrapure water is lower than the impact fan 344, and the first stirring component 34 is started during the absorption and fusion process of the two, and under the action of the sealed bearing 35, the first motor 341 drives the first stirring shaft 342 and the first stirring blade 343 to rotate and stir; directly When sulfur trioxide gas is introduced into ultrapure water, the interaction between water pressure and air pressure increases the fusion pressure of sulfur trioxide gas and ultrapure water, thereby accelerating the fusion efficiency of ultrapure water and sulfur trioxide gas; sulfur trioxide gas that has not been fused with ultrapure water rises to the inner top of mixing barrel 1, and with the continuous input of sulfur dioxide gas, the air pressure in mixing barrel 1 continues to increase, thereby increasing the fusion pressure of sulfur trioxide gas and ultrapure water, further increasing the absorption rate of sulfur trioxide gas by ultrapure water; and with the increase of air pressure, the sulfur trioxide gas above the liquid surface of ultrapure water The gas squeezes the ultrapure water in the mixing barrel 1, and then the ultrapure water enters the water sprinkling layer 312 through the water suction pipe 332, and flows downward through the nozzle 313. In the process of flowing downward, the first stirring shaft 342 drives the impact fan 344 to rotate continuously, and the blades 3441 of the impact fan 344 will scatter the falling water droplets, and the multiple impact bumps 34411 set on the blades 3441 make the water droplets easier to break and disperse, thereby increasing the contact area between the ultrapure water and the sulfur trioxide gas, and improving the fusion efficiency of the two. Detection: when the air pressure in the mixing barrel 1 reaches a set higher value, the second solenoid valve 18 is closed to suspend the delivery of sulfur trioxide gas, and the first solenoid valve 16 is opened to start the air pump 15 to extract the sulfur trioxide gas in the mixing barrel 1 and send it to the mixing layer 5 of the mixing spray tower 2 through the gas pipe 6 to be merged with the ultrapure water again; when the air pressure in the mixing barrel 1 drops to a preset value, the second solenoid valve 18 is opened to continue to deliver sulfur trioxide gas, and the first solenoid valve 16 is closed, so that the ultrapure water in the mixing barrel 1 continues to absorb sulfur dioxide gas.
[0045] Reference Figure 2 and Figure 7-10As shown, the secondary absorption mechanism 7 also includes a mounting plate 74 mounted on the inner wall of the mixing layer 5, an air delivery reduction box 71 is mounted on the mounting plate 74, an air delivery pipe 6 penetrates the mixing layer 5 and is connected to the air delivery reduction box 71, and one end of the air delivery pipe 6 is connected to the inner circle of the spiral baffle 711; six exhaust pipes 72 are connected and mounted at equal angles at the bottom of the air delivery reduction box 71, one end of the exhaust pipe 72 is connected to the outer circle of the spiral baffle 711, the exhaust pipe 72 is trumpet-shaped, and a plurality of exhaust holes 721 are evenly arranged on the pipe wall at the other end; the second stirring assembly 73 includes a second motor 731 mounted on the bottom of the air delivery reduction box 71, the output end of the second motor 731 is fixedly connected to a second stirring shaft 732, and a plurality of second stirring blades 733 are mounted on the second stirring shaft 732;
[0046] A partition 10 for separating the spray layer 4 and the mixing layer 5 is connected and installed on the inner wall of the mixing spray tower 2, and a plurality of through holes 11 are opened at equal angles on the partition 10. A mounting box 12 is connected and installed at the bottom of the partition 10. A telescopic cylinder 13 is installed in the mounting box 12. A closing component 14 for closing the through hole 11 is connected and installed at one end of the telescopic rod of the telescopic cylinder 13. The closing component 14 includes a top plate 141 installed at one end of the telescopic rod of the telescopic cylinder 13. A connecting rod 142 is connected and installed at equal angles on the top plate 141. A sealing plug 143 matching the position and number of the through hole 11 is connected and installed at one end of the connecting rod 142.
[0047] Embodiment 2:
[0048] The sulfur trioxide gas is transported from the mixing barrel 1 to the gas reduction box 71 through the air pump 15 and the gas pipe 6, and the gas outlet end of the gas pipe 6 is connected to the middle position of the top of the gas reduction box 71, so that one end of the gas pipe 6 is connected to the inner circle of the spiral baffle 711, thereby, the sulfur trioxide gas gradually moves from the inner circle of the spiral baffle 711 to the outer circle. When reaching the outer circle, the gas enters a plurality of trumpet-shaped exhaust pipes 72 and is slowly and evenly transported into the ultrapure water through the exhaust holes 721 thereon, wherein the liquid level of the ultrapure water in the mixing layer 5 is lower than the position of the gas reduction box 71; then the second stirring component 73 is started, and the second stirring shaft 732 and the second motor 731 are driven to move. The second stirring blade 733 rotates to increase the contact area and contact time between the sulfur trioxide gas and the ultrapure water, thereby improving the absorption and fusion efficiency of the two; as the sulfur trioxide gas and the ultrapure water fuse and rise, the air pressure in the mixed layer 5 continues to increase, and under the interaction of water pressure and air pressure, the fusion pressure of the sulfur trioxide gas and the ultrapure water is increased, thereby improving the fusion efficiency of the two; and through the detection of the second pressure gauge 20, when the air pressure in the mixed layer 5 reaches a set higher value, the telescopic cylinder 13 is started, and its telescopic rod pushes the top plate 141 upward to drive the connecting rod 142 and the sealing plug 143 upward, thereby, the sulfur trioxide gas rises and enters the spray layer 4 through the through-hole 11.
[0049] Reference Figure 1-2 , Figure 7 and Fig.11 As shown, the circulating water delivery system 8 includes a water delivery pipe 81 connected to the bottom of the mixing spray tower 2, a water pump 82 is connected to one side of the water delivery pipe 81, and a water delivery pipe 83 is connected to the output end of the water pump 82. The side wall of the water delivery pipe 83 is connected to a first water distribution pipe 84 and a second water distribution pipe 85. The other ends of the first water distribution pipe 84 and the second water distribution pipe 85 penetrate the side wall of the mixing spray tower 2 and are connected to the spray assembly 91; valves 86 are provided on the water delivery pipe 81, the first water distribution pipe 84 and the second water distribution pipe 85; the spray assembly 91 includes a spray pipe 911 and an atomizing nozzle 912, and the atomizing nozzle 912 is evenly distributed at the bottom of the spray pipe 911; the inner wall of the spray layer 4 A flow guide assembly 92 is installed on the upper connection, and the flow guide assembly 92 includes a flow guide ring 921, which is truncated and has a top diameter larger than a bottom diameter. A plurality of flow guide grooves 9211 are provided at equal angles on the inner surface of the flow guide ring 921, and an arc-shaped flow guide plate 922 protruding upward is connected to the bottom of the flow guide ring 921, and a plurality of flow guide holes 9221 are provided on the flow guide plate 922; an activated carbon plate 21 is provided above the second water distribution pipe 85 near the top of the mixing spray tower 2, a wire mesh demister 22 is provided between the second water distribution pipe 85 and the first water distribution pipe 84, a filling layer 23 is provided between the first water distribution pipe 84 and the partition 10, and the flow guide assembly 92 is installed below the filling layer 23;
[0050] Embodiment three:
[0051] The sulfur trioxide gas rises to the spray layer 4 through the through hole 11 on the partition 10, and while starting the telescopic cylinder 13, the water pump 82 in the circulating water supply system 8 is started and the valve 86 is opened, and the ultrapure water inside the mixing layer 5 is transported to the first water branch pipe 84 and the second water branch pipe 85 through the water supply pipe 81 and the water supply pipe 83, and then the water flows into the spray pipe 911 of the spray assembly 91 and is sprayed downward through the atomizing nozzle 912. At this time, the sulfur trioxide gas encounters the ultrapure water spraying downward during the rising process, and the two are in reverse contact, which increases the contact area and improves the fusion efficiency; the wire mesh demister 22 is used to remove the foam in the gas, and the filling layer 23 is composed of porcelain balls, plastic balls or ceramic fillers, which helps to increase the gas-liquid contact area and improve the mass transfer efficiency; and when the spray water reaches the filling layer 23, it will continue to flow downward, and when the liquid stays below, it will flow along the guide ring 921 The liquid flows along the guide groove 9211 provided on the guide ring 921, so that the liquid can be diverted on the guide ring 921, thereby avoiding the liquid from concentrating on the guide ring 921, and the guide plate 922 with an arc-shaped convex surface also increases the contact area between the sulfur dioxide gas and the ultrapure water, thereby improving the fusion rate of the two; the spray water falls and then falls into the mixing layer 5 through the through-hole 11 on the partition 10, thereby circulating and transporting; and after the sulfur trioxide gas is efficiently absorbed by the ultrapure water for many times, the sulfur trioxide content therein is extremely low, thereby reducing the workload of the exhaust gas treatment mechanism, and the pollution to the environment is greatly reduced after filtering through the activated carbon plate 21 at the top of the mixed spray tower 2; when the air pressure in the mixing layer 5 is reduced to the preset value, the water delivery operation of the water pump 82 is suspended, and the through-hole 11 is closed by the telescopic cylinder 13.
[0052] In summary, the above three embodiments can be regarded as a method of introducing sulfur trioxide gas into ultrapure water in batches by using the step-by-step feeding method through the detection of two pressure gauges, that is:
[0053] First, sulfur trioxide gas is input into the mixing barrel 1 to make it blend with ultrapure water, and the unblended gas rises. The air pressure in the mixing barrel 1 increases with the continuous input of sulfur trioxide gas. When the air pressure reaches the preset value of the first pressure gauge 19, on the one hand, the continuous input of sulfur trioxide gas is suspended, and on the other hand, the gas is transported to the mixing spray tower 2 through the air pump 15. When the air pressure in the mixing barrel 1 drops to the set value, the sulfur trioxide gas is continuously transported to the mixing barrel 1. Secondly, the mixing layer 5 in the mixing spray tower 2 is filled with sulfur trioxide gas. The input sulfur trioxide gas is mixed with ultrapure water, and the unmixed gas rises, and the air pressure in the mixing layer 5 increases. When the air pressure therein reaches the set value of the second pressure gauge 20, the through-hole 11 is opened to allow the sulfur trioxide gas to rise to the spray layer 4, and continue to be mixed with ultrapure water by gas-liquid reverse contact. When the air pressure in the mixing layer 5 drops to the set value of the second pressure gauge 20, the through-hole 11 is closed to allow the sulfur trioxide gas in the mixing layer 5 to continue to be mixed with ultrapure water; thereby making the absorption of the two more efficient and uniform.
[0054] In order to prevent corrosion, the mechanical components in the above mixing barrel 1 and the mixing spray tower 2 can be made of corrosion-resistant materials, or anti-corrosion coatings such as polymer coatings or special corrosion-resistant coatings can be applied on the surface of the components. These coatings can form a protective film on the surface to reduce the corrosion effects on the basic materials; in addition, an industrial automation controller can be used to operate and monitor the entire reaction process, thereby improving the operating efficiency of the entire process and improving the safety of production.
[0055] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.
[0056] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.
Claims
1. An electronic grade sulfuric acid continuous production device, comprising a mixing barrel (1) and a mixing spray tower (2), characterized in that: The mixing barrel (1) and the mixing spray tower (2) are jointly provided with an absorption mechanism for multiple fusion of sulfur trioxide gas and ultrapure water; wherein the mixing barrel (1) is provided with a primary absorption mechanism (3), the primary absorption mechanism (3) comprising a double-layer gas-liquid box (31), the upper gas transmission layer (311) of the double-layer gas-liquid box (31) being connected to a gas transmission component (32) for transporting sulfur trioxide gas to ultrapure water, and the lower water sprinkling layer (312) of the double-layer gas-liquid box (31) being connected to a water sprinkling component (32) for transporting ultrapure water to the upper gas transmission layer (311) of the double-layer gas-liquid box (31) being connected to a water sprinkling component (32) for transporting sulfur trioxide gas to the ultrapure water. The water absorbing component (33) is sucked in, and when the air pressure in the mixing barrel (1) increases, the ultrapure water is squeezed into the water sprinkling layer (312) and sprayed out. The double-layer gas-liquid box (31) is connected to a first stirring component (34). The first stirring component (34) stirs the ultrapure water while scattering the water droplets sprayed by the water sprinkling layer (312) to increase the contact area between the gas and the liquid. The mixing spray tower (2) is divided into an upper spray layer (4) and a lower mixing layer (5). The mixing layer (5) is connected to the air supply pipe (6). The mixing layer (5) is connected to the mixing barrel (1), and a secondary absorption mechanism (7) is provided in the mixing layer (5). The secondary absorption mechanism (7) is configured to slow down the flow rate of sulfur trioxide gas so that it is slowly and evenly introduced into the ultrapure water to improve the absorption rate. The secondary absorption mechanism (7) comprises a gas transmission reduction box (71), and a spiral baffle (711) is provided in the gas transmission reduction box (71) for slowing down the flow rate of sulfur trioxide gas. The bottom of the gas transmission reduction box (71) is connected to a plurality of exhaust pipes (72), and one side of the exhaust pipe (72) is provided with a A second stirring assembly (73) is provided; a circulating water supply system (8) connecting the mixing layer (5) and the spray layer (4) is provided on one side of the mixing spray tower (2); a tertiary absorption mechanism (9) is provided in the spray layer (4); the tertiary absorption mechanism (9) is configured to increase the contact area between sulfur trioxide gas and ultrapure water by reverse contact between gas and liquid; the tertiary absorption mechanism (9) comprises a spray assembly (91) connected to the circulating water supply system (8) and a flow guide assembly (92) for achieving sufficient contact between gas and liquid; The gas delivery component (32) comprises two first connecting columns (321) symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box (31); one end of two of the four first connecting columns (321) located on the same side are fixedly connected to an air supply pipe (322); one end of the two air supply pipes (322) are connected to the inside of the gas delivery layer (311); the other ends of the two air supply pipes (322) are connected to an annular pipe (323); a plurality of air outlets (3231) are evenly arranged at equal angles at the bottom of the annular pipe (323); the outer wall of the water sprinkling layer (312) is connected to the water absorption component (323); The water absorption component (33) comprises two second connection columns (331) symmetrically distributed on both sides of the outer surface of the double-layer gas-liquid box (31); one end of two second connection columns (331) located on the same side of the four second connection columns (331) are fixedly connected to a water absorption pipe (332); one end of the two water absorption pipes (332) are connected to the water sprinkling layer (312); the other ends of the two water absorption pipes (332) are immersed under the water surface of the ultrapure water in the mixing barrel (1); four nozzles (313) connected to the water sprinkling layer (312) are installed at equal angles on the bottom of the double-layer gas-liquid box (31); The secondary absorption mechanism (7) further comprises a mounting plate (74) mounted on the inner wall of the mixing layer (5), the mounting plate (74) being mounted on the gas transmission reduction box (71), the gas transmission pipe (6) penetrating the mixing layer (5) and being connected to the gas transmission reduction box (71), one end of the gas transmission pipe (6) being connected to the inner circle of the spiral baffle (711); six exhaust pipes (72) being equiangularly connected and mounted on the bottom of the gas transmission reduction box (71), one end of the exhaust pipe (72) being connected to the outer circle of the spiral baffle (711), the exhaust pipe (72) being trumpet-shaped and having a plurality of exhaust holes (721) uniformly arranged on the pipe wall at the other end; the second stirring assembly (73) comprising a second motor (731) mounted on the bottom of the gas transmission reduction box (71), the output end of the second motor (731) being fixedly connected to a second stirring shaft (732), and a plurality of second stirring blades (733) being mounted on the second stirring shaft (732).
2. The electronic grade sulfuric acid continuous production equipment according to claim 1, characterized in that: The double-layer gas-liquid box (31) is an annular box and a sealed bearing (35) is installed in a gap in the middle thereof, and the double-layer gas-liquid box (31) is connected and installed on the inner top of the mixing barrel (1) via a fixing column (36); the first stirring assembly (34) comprises a first motor (341) fixedly installed on the top surface of the mixing barrel (1), the output end of the first motor (341) is fixedly connected to a first stirring shaft (342), and the first stirring shaft (342) passes through the sealed bearing (35) and is connected to the first stirring shaft (342). The inner ring of the sealing bearing (35) is connected, and a plurality of first stirring blades (343) are fixedly installed on the first stirring shaft (342) located below the ultrapure water surface. An impact fan (344) for scattering water droplets is fixedly installed on the first stirring shaft (342) close to the nozzle (313), and the impact fan (344) includes four blades (3441) arranged at equal angles and inclined, and a plurality of raised impact bumps (34411) are provided on the fan surfaces on both sides of each blade (3441).
3. The electronic grade sulfuric acid continuous production equipment according to claim 2, characterized in that: A partition (10) for separating the spray layer (4) and the mixing layer (5) is connected and installed on the inner wall of the mixing spray tower (2); a plurality of through holes (11) are opened at equal angles on the partition (10); a mounting box (12) is connected and installed on the bottom of the partition (10); a telescopic cylinder (13) is installed in the mounting box (12); a closing component (14) for closing the through holes (11) is connected and installed at one end of the telescopic rod of the telescopic cylinder (13); the closing component (14) comprises a top plate (141) installed at one end of the telescopic rod of the telescopic cylinder (13); a connecting rod (142) is connected and installed at equal angles on the top plate (141); a sealing plug (143) matching the position and number of the through holes (11) is connected and installed at one end of the connecting rod (142).
4. The electronic grade sulfuric acid continuous production equipment according to claim 3, characterized in that: The circulating water supply system (8) comprises a water supply pipe (81) connected to the bottom of the mixing spray tower (2); a water pump (82) is connected to one side of the water supply pipe (81); an output end of the water pump (82) is connected to a water supply pipe (83); a first water distribution pipe (84) and a second water distribution pipe (85) are connected to the side wall of the water distribution pipe (83); the other ends of the first water distribution pipe (84) and the second water distribution pipe (85) both pass through the side wall of the mixing spray tower (2) and are connected to the spray assembly (91); valves (86) are provided on the water supply pipe (81), the first water distribution pipe (84) and the second water distribution pipe (85).
5. The continuous production equipment for electronic grade sulfuric acid according to claim 4, characterized in that: The spray assembly (91) comprises a spray pipe (911) and atomizing nozzles (912); the atomizing nozzles (912) are evenly distributed at the bottom of the spray pipe (911).
6. The electronic grade sulfuric acid continuous production equipment according to claim 5, characterized in that: The guide assembly (92) is connected and installed on the inner wall of the spray layer (4), and the guide assembly (92) comprises a guide ring (921), the guide ring (921) is truncated and has a top diameter greater than a bottom diameter, a plurality of guide grooves (9211) are provided at equal angles on the inner surface of the guide ring (921), and an upwardly protruding arc-shaped guide plate (922) is connected and installed on the bottom of the guide ring (921), and a plurality of guide holes (9221) are provided on the arc-shaped guide plate (922).
7. The continuous production equipment for electronic grade sulfuric acid according to claim 6, characterized in that: An air pump (15) is installed on the air delivery pipe (6), and a first solenoid valve (16) is installed at one end of the air delivery pipe (6) close to the top of the mixing barrel (1); an air intake pipe (17) is connected to the outer wall of the top of the mixing barrel (1), the air intake pipe (17) is connected to the air delivery layer (311), and a second solenoid valve (18) is installed on the air intake pipe (17); a first pressure gauge (19) for detecting air pressure is installed on the outer wall of the mixing barrel (1), and a second pressure gauge (20) for detecting air pressure in the mixing layer (5) is installed on the outer wall of the mixing spray tower (2).
8. The continuous production equipment for electronic grade sulfuric acid according to claim 7, characterized in that: An activated carbon plate (21) is provided above the second water distribution pipe (85) near the top of the mixing spray tower (2), a wire mesh demister (22) is provided between the second water distribution pipe (85) and the first water distribution pipe (84), a filling layer (23) is provided between the first water distribution pipe (84) and the partition plate (10), and the guide assembly (92) is installed below the filling layer (23).
Citation Information
Patent Citations
An electronic grade sulfuric acid production equipment
CN117886279B
Electronic-grade sulfuric acid production equipment
CN117886279A
Drying absorption tower for sulfuric acid production
CN220276639U