Evaporation purification equipment and method of high-purity electronic-grade hydrochloric acid

Abstract

The application discloses an evaporation and purification device and method for high-purity electronic-grade hydrochloric acid, and relates to the technical field of hydrochloric acid evaporation and purification. The device comprises a tower body, a filler, a liquid distributor and an isolation and guide mechanism. The acid mist droplets in the high-temperature hydrochloric acid mixed steam are sequentially subjected to cyclone primary capture and wave baffling secondary capture before entering the filler area through the cooperation of the spiral guide mechanism, the capture sheet and the dynamic trap, so that the probability of the entrained droplets entering the upper rectification area is reduced, thereby reducing the impurities such as metal ions and particulate matters from entering the subsequent condensation process with the steam. Through the cooperation of the collection cavity, the guide pipe and the reflux pipe, the captured impurity-containing droplets can be timely introduced into the waste liquid area and separated from the purified steam, so that the captured liquid is prevented from participating in evaporation again or being secondarily entrained by high-speed steam. Through the cooperation of the flow detector, the driving member, the upper capture plate and the lower capture plate, the control system can dynamically adjust the through-flow gap of the wave capture cavity according to the capture liquid load, so that the capture liquid efficiency is ensured.

Description

Technical Field

[0001] This invention relates to the field of hydrochloric acid evaporation and purification technology, specifically to an evaporation and purification device and method for high-purity electronic-grade hydrochloric acid. Background Technology

[0002] High-purity electronic-grade hydrochloric acid evaporation and purification equipment is an acid purification device used in the preparation process of wet electronic chemicals. It is mainly suitable for evaporating, separating, condensing, and improving the purity of industrial hydrochloric acid or pretreated hydrochloric acid. This equipment uses controlled heating of the hydrochloric acid raw material, causing volatile components such as hydrogen chloride and water to escape from the raw liquid in gaseous form, while metal ions, particulate matter, and high-boiling-point impurities are mainly retained in the liquid residue. Subsequently, the generated hydrochloric acid vapor is further purified and condensed for recovery, thereby obtaining high-purity electronic-grade hydrochloric acid that meets the requirements for use.

[0003] In existing high-purity electronic-grade hydrochloric acid evaporation and purification equipment, the acid liquid at the bottom of the tower has a high impurity content. Direct discharge would result in the waste of volatile hydrochloric acid components and increase the burden of waste liquid treatment. If it is heated and reused, acid mist droplets with high concentration of impurities are easily generated and enter the packing zone and condenser with the steam, affecting the purity and stability of the finished hydrochloric acid. The existing structure is difficult to collect, isolate and discharge the high-impurity entrained droplets while recovering the volatile components in the acid liquid at the bottom of the tower. Summary of the Invention

[0004] The purpose of this invention is to provide an evaporation and purification device and method for high-purity electronic-grade hydrochloric acid, so as to solve the problem of difficult bottom waste liquid treatment in the prior art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: an evaporation and purification device for high-purity electronic-grade hydrochloric acid, comprising a tower body and an isolation and guide mechanism, wherein the tower body is provided with several sets of packing materials and a liquid distributor is installed at the top of the tower body; The isolation and discharge mechanism includes a cylinder and several sets of dynamic traps. The cylinder is installed inside the tower through connectors. An isolation component is installed at the bottom of the cylinder. The isolation component is connected to the tower and the bottom of the tower forms a waste liquid zone. An exhaust chamber is formed between the outer wall of the cylinder and the inner wall of the tower. Several sets of driving components are installed on the cylinder, and a reflux component is installed on the isolation component. The dynamic trap includes a lower trap plate and an upper trap plate. The lower trap plate is mounted on the cylinder, and the upper trap plate is slidably mounted on the cylinder. The upper trap plate is connected to the drive component, and a wave trapping chamber is formed between the upper trap plate and the lower trap plate. The reflux component passes through the lower trap plate and communicates with the waste liquid area. The wave trapping chamber is connected with the exhaust chamber.

[0006] The evaporation and purification equipment is connected to an external control cabinet, which contains a control system for operating the entire evaporation and purification equipment.

[0007] After being processed by the isolation and discharge mechanism, the hydrochloric acid vapor continues upward along the exhaust chamber into the areas containing several groups of packing materials, where it comes into contact with the hydrochloric acid liquid film distributed below the distributor, causing the hydrochloric acid in the packing to vaporize upon heating. Finally, the high-purity vaporized hydrochloric acid is discharged from the exhaust port at the top of the tower and then enters an external condenser for condensation and recovery via pipeline. The waste liquid containing metallic impurities and high-boiling-point impurities accumulated in the waste liquid area at the bottom of the tower is discharged into the waste liquid tank through the drain port, completing the purification process.

[0008] Furthermore, the isolation assembly includes an outer ramp ring and an inner ramp ring. The outer ramp ring is installed on the inner wall of the tower body, and the inner ramp ring is installed at the bottom of the cylinder. A liquid collection slit is provided between the outer ramp ring and the inner ramp ring. The inner wall of the inner ramp ring forms a swirl chamber. Several spiral blades are arranged circumferentially on the inner wall of the inner ramp ring. The spiral blades form a spiral guide mechanism. The outer ramp ring and the inner ramp ring form a waste liquid zone between themselves and the bottom of the tower body. The waste liquid zone is connected to the swirl chamber. The reflux assembly passes through the isolation assembly and is connected to the waste liquid zone.

[0009] The outer and inner slope rings together form a funnel-shaped liquid collection and discharge structure.

[0010] The high-temperature hydrochloric acid mixed vapor then enters the swirl chamber formed on the inner wall of the inner inclined ring. Because the inner wall of the inner inclined ring is circumferentially equipped with several spiral blades, which constitute a spiral guiding mechanism, the mixed vapor is guided by the spiral blades as it passes through the swirl chamber, causing it to rotate and rise. During this upward rotation, acid mist droplets, metal impurity droplets, and particulate matter entrained in the mixed vapor are deflected outwards due to inertia and collide with the inner wall of the cylinder and the collecting plates installed on it, thus achieving a primary centrifugal collection effect. The droplets captured by the inner wall of the cylinder and the collecting plates flow back down the inner wall of the cylinder into the waste liquid area.

[0011] Inside the tower, unvaporized liquid falling from the packing material flows downwards along the inner wall of the tower, the surface of the packing material, and the outer side of the cylinder. When the falling liquid reaches the isolation component, the outer and inner ramp rings together form a funnel-shaped liquid collection and discharge structure, which guides and collects the falling liquid. The falling liquid converges at the collection slit and falls downwards into the waste liquid area. The converged liquid continuously falls at the collection slit, forming a liquid curtain. This liquid curtain creates a liquid seal to isolate the upward-rising steam in the waste liquid area, preventing the high-temperature steam rising from the waste liquid area from directly entering the exhaust chamber through the collection slit. Instead, it is forced to enter the swirl chamber formed by the inner wall of the inner ramp ring. This ensures that the return liquid from above can smoothly return to the waste liquid area while preventing unpurified steam from escaping by bypassing the isolation and discharge mechanism.

[0012] Furthermore, the lower trapping plate is provided with several gradient-arranged lower trapping toothed rings, and several collection grooves are opened on the several lower trapping toothed rings. The bottom of the collection groove is provided with a drop outlet. The lower trapping plate is provided with a collection chamber. The drop outlet is connected to the collection chamber. A connection port is provided on one side of the collection chamber. The collection chamber is connected to the return assembly through the connection port.

[0013] Furthermore, the upper trapping plate is provided with several upper trapping toothed rings arranged in a gradient, and the upper trapping toothed rings and the lower trapping toothed rings form a dynamically adjustable wave trapping cavity.

[0014] The driving component can be a telescopic rod, whose output shaft drives the upper capture plate to move up and down, thereby adjusting the size of the wave capture chamber.

[0015] After primary swirl trapping, the mixed steam enters the wave trapping chamber of the dynamic trap through several strip-shaped openings on the cylinder. After entering the wave trapping chamber, the mixed steam continuously changes its flow direction between the upper and lower trapping toothed rings, forming a multi-stage baffle flow. During the baffle process, the residual droplets in the mixed steam collide with the surfaces of the upper and lower trapping toothed rings due to inertia, and coalesce on the surface of the trapping toothed rings to form larger droplets.

[0016] The droplets captured by the lower collecting toothed ring flow along its surface into the collecting tank, and then enter the collection chamber inside the lower collecting plate through the drop outlet at the bottom of the collecting tank. The impurity-containing droplets collected in the collection chamber are sequentially guided into the waste liquid area through the connection port, the guide pipe, and the return pipe, thereby completing the recovery of high-impurity droplets and preventing these droplets from continuing to enter the upper packing area and subsequent condenser with the purified steam, thus reducing the impurity content of the finished hydrochloric acid and completing the two-stage wave baffle collection treatment.

[0017] Furthermore, the reflux assembly includes a reflux pipe with several guide pipes installed on it. The guide pipes are connected to the collection chamber through a connection port. The reflux pipe passes through the outer inclined ring and is connected to the waste liquid area. A flow detector is installed inside the guide pipe.

[0018] A flow detector is used to detect the flow rate of waste liquid in the drainage pipe.

[0019] During the evaporation and purification process, the flow detector monitors the waste liquid flow rate in the corresponding guide pipe in real time. The control system determines the liquid capture load of the corresponding dynamic collector based on the waste liquid flow rate. During normal operation, the upper and lower capture plates maintain a preset distance, allowing the wave-like capture chamber to function as both a deflector for liquid capture and a stabilizing ventilator. When the waste liquid flow rate in a certain guide pipe gradually increases, it indicates that the entrained liquid captured by the corresponding wave-like capture chamber is increasing. The control system then controls the drive component to move the upper capture plate closer to the lower capture plate, reducing the flow gap in the wave-like capture chamber, thus enhancing the steam deflection degree and appropriately reducing the input of steam and hydrochloric acid raw materials, thereby improving the capture effect of acid mist droplets.

[0020] Furthermore, the inner wall of the cylinder forms a collection chamber, which is connected to the swirl chamber. Several strip-shaped openings are provided inside the cylinder, and the collection chamber is connected to the wave collection cavity through the strip-shaped openings. Several collection plates are installed on the inner wall of the cylinder.

[0021] Furthermore, the top of the tower is equipped with an exhaust port, which is connected to an external condenser through a pipe. The tower is also equipped with a feed inlet, through which a liquid distributor is connected to an external raw material tank. The bottom of the tower is equipped with an air inlet and a liquid outlet, with the air inlet connected to an evaporator through a pipe and the liquid outlet connected to a waste liquid tank through a pipe.

[0022] During the purification process, the control system first controls the external raw material tank to supply the hydrochloric acid raw material to be purified to the liquid distributor at the top of the tower. After being evenly distributed by the liquid distributor, the hydrochloric acid raw material flows downward along several sets of packing materials, forming a liquid film on the surface of the packing materials. At the same time, the high-temperature steam generated by the external evaporator enters the lower part of the tower through the air inlet at the bottom of the tower and enters the waste liquid zone. The high-temperature steam heats the acid liquid accumulated in the waste liquid zone, causing the volatile hydrochloric acid components in the waste liquid zone to continue to vaporize, while metal ions, particulate matter and high-boiling-point impurities are mainly retained in the waste liquid zone and are finally discharged into the waste liquid tank through the drain outlet.

[0023] A method for evaporating and purifying high-purity electronic-grade hydrochloric acid, comprising the following steps: S1. The hydrochloric acid raw material to be purified is conveyed to the distributor through the feed port. The distributor distributes the hydrochloric acid raw material onto several sets of packing in the tower body, so that the hydrochloric acid raw material flows downward along the packing. S2. Start the external evaporator to allow high-temperature steam to enter the waste liquid zone at the bottom of the tower through the air inlet and heat the acid liquid in the waste liquid zone, so that the volatile hydrochloric acid components in the waste liquid zone continue to vaporize. S3. High-temperature hydrochloric acid mixed vapor enters the swirl chamber and forms a rotating upward airflow under the action of the spiral blades, causing the impurity droplets in the mixed vapor to deflect towards the inner wall of the cylinder, and are then initially captured by the inner wall of the cylinder and the collecting blades. S4. The mixed steam after primary capture enters the wave capture chamber through the strip-shaped inlet and flows between the upper and lower capture toothed rings, causing the residual acid mist droplets to collide and coalesce before entering the collection chamber through the convergence tank and the drop outlet. It is then guided into the waste liquid area through the guide pipe and the return pipe. The control system adjusts the position of the upper capture plate according to the waste liquid flow rate in the guide pipe to change the flow gap of the wave capture chamber. S5. After being treated by the isolation and discharge mechanism, the hydrochloric acid vapor enters the exhaust chamber and continues to pass through several sets of packing for gas-liquid mass transfer. It is then discharged from the exhaust port at the top of the tower and enters the external condenser for condensation and recovery. The waste liquid containing impurities accumulated in the waste liquid area is discharged to the waste liquid tank through the drain port.

[0024] Compared with the prior art, the beneficial effects of the present invention are: 1. Through the cooperation of the spiral guide mechanism, the trapping plate and the dynamic trap, the acid mist droplets in the high-temperature hydrochloric acid mixed vapor undergo primary swirling trapping and secondary wave baffle trapping before entering the packing zone. This reduces the probability of entrained droplets entering the upper distillation zone, thereby reducing the amount of impurities such as metal ions and particulate matter that enter the subsequent condensation process with the vapor, and improving the purification effect of electronic-grade hydrochloric acid.

[0025] 2. Through the cooperation of the collection chamber, the guide pipe and the return pipe, the captured droplets containing impurities can be introduced into the waste liquid area in a timely manner and separated from the purification steam, so as to avoid the collected liquid from participating in evaporation again or being entrained by high-speed steam.

[0026] 3. Through the cooperation of the flow detector, drive unit, upper collection plate and lower collection plate, the control system can dynamically adjust the flow gap of the wave collection chamber according to the liquid collection load, so as to ensure the liquid collection efficiency and enable the equipment to adapt to the operating conditions under different evaporation loads.

[0027] 4. Through the cooperation of the outer slope ring, the inner slope ring and the liquid collection gap, the upper return liquid is gathered to form a continuous liquid curtain, which isolates the rising steam in the waste liquid area, guides the steam through the swirl chamber into the isolation and discharge mechanism, reduces steam leakage, improves steam utilization, and further ensures the purification effect of hydrochloric acid steam. Attached Figure Description

[0028] Figure 1 This is a perspective view of the evaporation and purification equipment of the present invention; Figure 2 This is a cross-sectional view of the evaporation and purification equipment of the present invention; Figure 3 This is a partial cross-sectional view of the evaporation and purification equipment of the present invention; Figure 4 This is a cross-sectional view of the isolation guide mechanism of the present invention; Figure 5 This is a cross-sectional view of the cylindrical body of the present invention; Figure 6 This is a cross-sectional view of the dynamic trapping device of the present invention; Figure 7 For the present invention Figure 6 A magnified view of a portion of region A in the middle; Figure 8 This is a perspective view of the trapping plate of the present invention.

[0029] In the diagram: 1. Tower body; 2. Packing; 3. Liquid distributor; 4. Waste liquid zone; 5. Isolation and drainage mechanism; 6. Exhaust chamber; 51. Reflux assembly; 52. Isolation assembly; 53. Shell; 54. Dynamic collector; 55. Drive unit; 11. Feed inlet; 12. Exhaust port; 13. Air inlet; 14. Liquid outlet; 511. Reflux pipe; 512. Drainage pipe; 521. Outer inclined ring; 522. Inner inclined ring 523. Slope ring; 524. Spiral blade; 525. Liquid collection slot; 531. Swirling chamber; 532. Strip-shaped opening; 533. Collection plate; 541. Upper collection plate; 542. Lower collection plate; 543. Wave collection cavity; 5411. Upper collection toothed ring; 5421. Collection cavity; 5422. Drop outlet; 5423. Converging trough; 5424. Connecting port; 5425. Lower collection toothed ring. Detailed Implementation

[0030] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] like Figures 1-2 and Figures 4-8 The first embodiment of the present invention illustrates an evaporation purification device and method for high-purity electronic-grade hydrochloric acid, comprising a tower body 1 and an isolation and drainage mechanism 5. The tower body 1 contains several sets of packing materials 2, and a liquid distributor 3 is installed at the top of the tower body 1. The isolation and drainage mechanism 5 includes a cylinder 53 and several sets of dynamic collectors 54. The cylinder 53 is installed inside the tower body 1 via connectors. An isolation component 52 is installed at the bottom of the cylinder 53, and the isolation component 52 is connected to the tower body 1. The isolation component 52 and the bottom of the tower body 1 form a waste liquid zone 4. An exhaust system is formed between the outer wall of the cylinder 53 and the inner wall of the tower body 1. Chamber 6 has several sets of drive components 55 mounted on the cylinder 53, and a reflux component 51 mounted on the isolation assembly 52. ​​The dynamic collector 54 includes a lower collecting plate 542 and an upper collecting plate 541. The lower collecting plate 542 is mounted on the cylinder 53, and the upper collecting plate 541 is slidably mounted on the cylinder 53. The upper collecting plate 541 is connected to the drive components 55, and a wave collecting chamber 543 is formed between the upper collecting plate 541 and the lower collecting plate 542. The reflux component 51 passes through the lower collecting plate 542 and communicates with the waste liquid zone 4. The wave collecting chamber 543 communicates with the exhaust chamber 6. The evaporation and purification equipment is externally connected to a control cabinet, which contains a control system for operating the entire evaporation and purification equipment.

[0032] The top of the tower body 1 is provided with an exhaust port 12, which is connected to an external condenser through a pipe. The tower body 1 is provided with a feed inlet 11, and the liquid distributor 3 is connected to an external raw material tank through the feed inlet 11. The bottom of the tower body 1 is provided with an air inlet 13 and a liquid outlet 14. The air inlet 13 is connected to an evaporator through a pipe, and the liquid outlet 14 is connected to a waste liquid tank through a pipe.

[0033] During the purification process, the control system first controls the external raw material tank to supply the hydrochloric acid raw material to be purified to the liquid distributor 3 at the top of the tower body 1. After being evenly distributed by the liquid distributor 3, the hydrochloric acid raw material flows downward along several sets of packing 2, forming a liquid film on the surface of the packing 2. At the same time, the high-temperature steam generated by the external evaporator enters the lower part of the tower body 1 through the air inlet 13 at the bottom of the tower body 1 and enters the waste liquid zone 4. The high-temperature steam heats the acid liquid accumulated in the waste liquid zone 4, causing the volatile hydrochloric acid components in the waste liquid zone 4 to continue to vaporize, while metal ions, particulate matter and high-boiling-point impurities are mainly retained in the waste liquid zone 4 and are finally discharged into the waste liquid tank through the drain outlet 14.

[0034] The isolation assembly 52 includes an outer ramp ring 521 and an inner ramp ring 522. The outer ramp ring 521 is installed on the inner wall of the tower body 1, and the inner ramp ring 522 is installed at the bottom of the cylinder 53. A liquid collection slit 524 is provided between the outer ramp ring 521 and the inner ramp ring 522. The inner wall of the inner ramp ring 522 forms a swirl chamber 525. A number of spiral blades 523 are arranged circumferentially on the inner wall of the inner ramp ring 522. The number of spiral blades 523 forms a spiral guide mechanism. The outer ramp ring 521 and the inner ramp ring 522 form a waste liquid zone 4 between themselves and the bottom of the tower body 1. The waste liquid zone 4 is connected to the swirl chamber 525. The reflux assembly 51 passes through the isolation assembly 52 and is connected to the waste liquid zone 4.

[0035] The outer slope ring 521 and the inner slope ring 522 form a liquid collection and discharge structure with a funnel-shaped cross-section.

[0036] The high-temperature hydrochloric acid mixed vapor then enters the swirl chamber 525 formed on the inner wall of the inner inclined ring 522. Because the inner wall of the inner inclined ring 522 is circumferentially equipped with several spiral blades 523, which constitute a spiral guide mechanism, the mixed vapor, upon passing through the swirl chamber 525, is guided by the spiral blades 523 and generates a rotating upward motion. During the upward rotation of the mixed vapor, acid mist droplets, metal impurity droplets, and particulate matter entrained in the mixed vapor are deflected outward due to inertia and collide with the inner wall of the cylinder 53 and the collecting plates 532 installed on the inner wall of the cylinder 53, thereby achieving a primary centrifugal collection effect. The droplets captured by the inner wall of the cylinder 53 and the collecting plates 532 flow downwards along the inner wall of the cylinder 53 back into the waste liquid area 4.

[0037] Inside the tower body 1, unvaporized liquid falling from the packing 2 flows downwards along the inner wall of the tower body 1, the surface of the packing 2, and the outer side of the cylinder 53. When the falling liquid reaches the isolation component 52, the outer slope ring 521 and the inner slope ring 522 together form a funnel-shaped liquid collection and discharge structure, which can guide and collect the falling liquid. The falling liquid converges at the collection slit 524 and falls downwards into the waste liquid zone 4. The converged liquid continuously falls at the collection slit 524 to form a liquid curtain. The liquid curtain forms a liquid seal to isolate the upward steam in the waste liquid zone 4, making it difficult for the high-temperature steam rising in the waste liquid zone 4 to directly enter the exhaust chamber 6 from the collection slit 524. Instead, it is forced to enter the swirl chamber 525 formed by the inner wall of the inner slope ring 522. Thus, while ensuring that the return liquid from above can smoothly return to the waste liquid zone 4, it prevents unpurified steam from escaping by bypassing the isolation and discharge mechanism 5.

[0038] The lower collecting plate 542 is provided with a number of lower collecting toothed rings 5425 arranged in a gradient. A number of collecting grooves 5423 are opened on the lower collecting toothed rings 5425. A drop outlet 5422 is provided at the bottom of the collecting groove 5423. A collection chamber 5421 is provided inside the lower collecting plate 542. The drop outlet 5422 is connected to the collection chamber 5421. A connection port 5424 is provided on one side of the collection chamber 5421. The collection chamber 5421 is connected to the return assembly 51 through the connection port 5424.

[0039] The upper trapping plate 541 is provided with several upper trapping toothed rings 5411 arranged in a gradient. The upper trapping toothed rings 5411 and the lower trapping toothed rings 5425 form a dynamically adjustable wave trapping cavity 543. The driving component 55 can be a telescopic rod. The output shaft of the telescopic rod drives the upper trapping plate 541 to move up and down, thereby adjusting the size of the wave trapping cavity 543.

[0040] After primary swirl trapping, the mixed steam enters the wave trapping chamber 543 of the dynamic trapping device 54 through several strip-shaped openings 531 provided on the cylinder 53. After entering the wave trapping chamber 543, the mixed steam continuously changes its flow direction between the upper trapping toothed ring 5411 and the lower trapping toothed ring 5425, forming a multi-stage baffle flow. During the baffle process, the residual droplets in the mixed steam collide with the surfaces of the upper trapping toothed ring 5411 and the lower trapping toothed ring 5425 due to inertia, and coalesce on the surface of the trapping toothed rings to form larger droplets.

[0041] The droplets captured by the lower collecting toothed ring 5425 flow along the surface of the lower collecting toothed ring 5425 into the collecting tank 5423, and then enter the collection chamber 5421 inside the lower collecting plate 542 through the drop outlet 5422 at the bottom of the collecting tank 5423. The droplets containing impurities collected in the collection chamber 5421 are sequentially introduced into the waste liquid zone 4 through the connection port 5424, the guide pipe 512 and the return pipe 511, thereby completing the recovery of high impurity droplets and preventing these droplets from continuing to enter the upper packing zone 2 and the subsequent condenser with the purified steam, thereby reducing the impurity content of the finished hydrochloric acid and completing the two-stage wave baffle collection treatment.

[0042] The inner wall of the cylinder 53 forms a collection chamber 533, which is connected to the swirl chamber 525. Several strip-shaped openings 531 are provided inside the cylinder 53. The collection chamber 533 is connected to the wave collection cavity 543 through the strip-shaped openings 531. Several collection plates 532 are installed on the inner wall of the cylinder 53.

[0043] like Figure 3 The second embodiment of the present invention provides a reflux assembly 51 for the evaporation and purification of high-purity electronic-grade hydrochloric acid, which differs from that in the first embodiment. The reflux assembly 51 includes a reflux pipe 511, on which several guide pipes 512 are installed. The guide pipes 512 are connected to a collection chamber 5421 via a connection port 5424. The reflux pipe 511 passes through an outer inclined ring 521 and is connected to a waste liquid zone 4. A flow detector is installed inside the guide pipe 512. The flow detector is used to detect the flow rate of the waste liquid in the guide pipe 512. The impurity-containing liquid captured in the collection chamber 5421 is introduced into the reflux pipe 511 through the guide pipes 512 and discharged into the waste liquid zone 4 through the reflux pipe 511. Simultaneously, the flow detector provides feedback on the captured liquid flow rate to promptly discharge the high-impurity entrained liquid, reducing its secondary entrainment into the upper packing zone with hydrochloric acid vapor and improving the stability of the evaporation and purification process.

[0044] During the evaporation and purification process, the flow detector monitors the waste liquid flow rate in the corresponding guide pipe 512 in real time, and the control system determines the liquid capture load of the corresponding dynamic collector 54 based on the waste liquid flow rate. During normal operation, the upper collector plate 541 and the lower collector plate 542 maintain a preset distance, so that the wave collection chamber 543 has both the functions of deflecting and capturing liquid and stabilizing ventilation. When the waste liquid flow rate in a certain guide pipe 512 gradually increases, it indicates that the entrained liquid captured by the corresponding wave collection chamber 543 has increased. The control system controls the drive component 55 to move the upper collector plate 541 closer to the lower collector plate 542, reducing the flow gap of the wave collection chamber 543, enhancing the steam deflection degree, and appropriately reducing the input of steam and hydrochloric acid raw materials, thereby improving the capture effect of acid mist droplets.

[0045] A method for evaporating and purifying high-purity electronic-grade hydrochloric acid, comprising the following steps: S1. The hydrochloric acid raw material to be purified is conveyed to the distributor 3 through the feed port 11. The distributor 3 distributes the hydrochloric acid raw material onto several sets of packing 2 in the tower body 1, so that the hydrochloric acid raw material flows downward along the packing 2. S2. Start the external evaporator so that high-temperature steam enters the waste liquid zone 4 at the bottom of the tower body 1 through the air inlet 13 and heats the acid liquid in the waste liquid zone 4 so that the volatile hydrochloric acid components in the waste liquid zone 4 continue to vaporize. S3. High-temperature hydrochloric acid mixed vapor enters the swirl chamber 525 and forms a rotating upward airflow under the action of the spiral blade 523, causing the impurity droplets in the mixed vapor to deflect towards the inner wall of the cylinder 53, and are then initially captured by the inner wall of the cylinder 53 and the collecting blade 532. S4. The mixed steam after primary capture enters the wave capture chamber 543 through the strip-shaped inlet 531, and flows between the upper capture toothed ring 5411 and the lower capture toothed ring 5425, causing the residual acid mist droplets to collide and coalesce before entering the collection chamber 5421 through the collection tank 5423 and the drop outlet 5422, and then being introduced into the waste liquid zone 4 through the guide pipe 512 and the return pipe 511; the control system controls the drive component 55 to adjust the position of the upper capture plate 541 according to the waste liquid flow rate in the guide pipe 512, so as to change the flow gap of the wave capture chamber 543; S5. After being processed by the isolation and discharge mechanism 5, the hydrochloric acid vapor enters the exhaust chamber 6 and continues to pass through several sets of packing 2 for gas-liquid mass transfer. It is then discharged from the exhaust port 12 at the top of the tower body 1 and enters the external condenser for condensation and recovery. The waste liquid containing impurities accumulated in the waste liquid area 4 is discharged to the waste liquid tank through the drain port 14.

[0046] The working principle of this invention is as follows: During the purification operation, the control system first controls the external raw material tank to supply the hydrochloric acid raw material to be purified to the liquid distributor 3 at the top of the tower body 1. After being evenly distributed by the liquid distributor 3, the hydrochloric acid raw material flows downward along several sets of packing 2, forming a liquid film on the surface of the packing 2. At the same time, the high-temperature steam generated by the external evaporator enters the lower part of the tower body 1 through the air inlet 13 at the bottom of the tower body 1 and enters the waste liquid zone 4. The high-temperature steam heats the acid liquid accumulated in the waste liquid zone 4, so that the volatile hydrochloric acid components in the waste liquid zone 4 continue to vaporize, while metal ions, particulate matter and high-boiling-point impurities are mainly retained in the waste liquid zone 4 and are finally discharged into the waste liquid tank through the drain outlet 14.

[0047] The high-temperature hydrochloric acid mixed vapor then enters the swirl chamber 525 formed on the inner wall of the inner inclined ring 522. Because the inner wall of the inner inclined ring 522 is circumferentially equipped with several spiral blades 523, which constitute a spiral guide mechanism, the mixed vapor, upon passing through the swirl chamber 525, is guided by the spiral blades 523 and generates a rotating upward motion. During the upward rotation of the mixed vapor, acid mist droplets, metal impurity droplets, and particulate matter entrained in the mixed vapor are deflected outward due to inertia and collide with the inner wall of the cylinder 53 and the collecting plates 532 installed on the inner wall of the cylinder 53, thereby achieving a primary centrifugal collection effect. The droplets captured by the inner wall of the cylinder 53 and the collecting plates 532 flow downwards along the inner wall of the cylinder 53 back into the waste liquid area 4.

[0048] After primary swirl trapping, the mixed steam enters the wave trapping chamber 543 of the dynamic trapping device 54 through several strip-shaped openings 531 provided on the cylinder 53. After entering the wave trapping chamber 543, the mixed steam continuously changes its flow direction between the upper trapping toothed ring 5411 and the lower trapping toothed ring 5425, forming a multi-stage baffle flow. During the baffle process, the residual droplets in the mixed steam collide with the surfaces of the upper trapping toothed ring 5411 and the lower trapping toothed ring 5425 due to inertia, and coalesce on the surface of the trapping toothed rings to form larger droplets.

[0049] The droplets captured by the lower collecting toothed ring 5425 flow along the surface of the lower collecting toothed ring 5425 into the collecting tank 5423, and then enter the collection chamber 5421 inside the lower collecting plate 542 through the drop outlet 5422 at the bottom of the collecting tank 5423. The droplets containing impurities collected in the collection chamber 5421 are sequentially introduced into the waste liquid zone 4 through the connection port 5424, the guide pipe 512 and the return pipe 511, thereby completing the recovery of high impurity droplets and preventing these droplets from continuing to enter the upper packing zone 2 and the subsequent condenser with the purified steam, thereby reducing the impurity content of the finished hydrochloric acid and completing the two-stage wave baffle collection treatment.

[0050] Inside the tower body 1, unvaporized liquid falling from the packing 2 flows downwards along the inner wall of the tower body 1, the surface of the packing 2, and the outer side of the cylinder 53. When the falling liquid reaches the isolation component 52, the outer slope ring 521 and the inner slope ring 522 together form a funnel-shaped liquid collection and discharge structure, which can guide and collect the falling liquid. The falling liquid converges at the collection slit 524 and falls downwards into the waste liquid zone 4. The converged liquid continuously falls at the collection slit 524 to form a liquid curtain. The liquid curtain forms a liquid seal to isolate the upward steam in the waste liquid zone 4, making it difficult for the high-temperature steam rising in the waste liquid zone 4 to directly enter the exhaust chamber 6 from the collection slit 524. Instead, it is forced to enter the swirl chamber 525 formed by the inner wall of the inner slope ring 522. Thus, while ensuring that the return liquid from above can smoothly return to the waste liquid zone 4, it prevents unpurified steam from escaping by bypassing the isolation and discharge mechanism 5.

[0051] During the evaporation and purification process, the flow detector monitors the waste liquid flow rate in the corresponding guide pipe 512 in real time, and the control system determines the liquid capture load of the corresponding dynamic collector 54 based on the waste liquid flow rate. During normal operation, the upper collector plate 541 and the lower collector plate 542 maintain a preset distance, so that the wave collection chamber 543 has both the functions of deflecting and capturing liquid and stabilizing ventilation. When the waste liquid flow rate in a certain guide pipe 512 gradually increases, it indicates that the entrained liquid captured by the corresponding wave collection chamber 543 has increased. The control system controls the drive component 55 to move the upper collector plate 541 closer to the lower collector plate 542, reducing the flow gap of the wave collection chamber 543, enhancing the steam deflection degree, and appropriately reducing the input of steam and hydrochloric acid raw materials, thereby improving the capture effect of acid mist droplets.

[0052] After being processed by the isolation and discharge mechanism 5, the hydrochloric acid vapor continues upward along the exhaust chamber 6 into the area where several groups of packing 2 are located, and comes into contact with the hydrochloric acid liquid film distributed under the liquid distributor 3, causing the hydrochloric acid in the packing 2 to vaporize upon heating. Finally, the vaporized hydrochloric acid with higher purity is discharged from the exhaust port 12 at the top of the tower body 1 and enters the external condenser through a pipeline for condensation and recovery. The waste liquid containing metal impurities and high-boiling-point impurities accumulated in the waste liquid area 4 at the bottom of the tower body 1 is discharged into the waste liquid tank through the drain port 14, completing the purification process.

[0053] It will be apparent to those skilled in the art that the present 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 its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

Claims

1. An evaporation and purification device for high-purity electronic-grade hydrochloric acid, characterized in that: The evaporation and purification equipment includes a tower body (1) and an isolation and guide mechanism (5). The tower body (1) is provided with several sets of packing materials (2), and a liquid distributor (3) is installed at the top of the tower body (1). The isolation and drainage mechanism (5) includes a cylinder (53) and several sets of dynamic traps (54). The cylinder (53) is installed inside the tower body (1) through a connector. An isolation component (52) is installed at the bottom of the cylinder (53). The isolation component (52) is connected to the tower body (1). The isolation component (52) and the bottom of the tower body (1) form a waste liquid zone (4). An exhaust chamber (6) is formed between the outer wall of the cylinder (53) and the inner wall of the tower body (1). Several sets of driving components (55) are installed on the cylinder (53). A return component (51) is installed on the isolation component (52). The dynamic trap (54) includes a lower trap plate (542) and an upper trap plate (541). The lower trap plate (542) is mounted on the cylinder (53), and the upper trap plate (541) is slidably mounted on the cylinder (53). The upper trap plate (541) is connected to the drive component (55). The upper trap plate (541) and the lower trap plate (542) form a wave trapping chamber (543). The reflux assembly (51) passes through the lower trap plate (542) and communicates with the waste liquid area (4). The wave trapping chamber (543) is connected with the exhaust chamber (6). The isolation component (52) includes an outer ramp ring (521) and an inner ramp ring (522). The outer ramp ring (521) is installed on the inner wall of the tower body (1), and the inner ramp ring (522) is installed at the bottom of the cylinder (53). A liquid collection slit (524) is provided between the outer ramp ring (521) and the inner ramp ring (522). The inner wall of the inner ramp ring (522) forms a swirl chamber (525). A plurality of spiral blades (523) are arranged circumferentially on the inner wall of the inner ramp ring (522). The plurality of spiral blades (523) form a spiral guide mechanism. The outer ramp ring (521) and the inner ramp ring (522) form a waste liquid area (4) between themselves and the bottom of the tower body (1). The waste liquid area (4) is connected to the swirl chamber (525). The reflux component (51) passes through the isolation component (52) and is connected to the waste liquid area (4).

2. The evaporation and purification equipment for high-purity electronic-grade hydrochloric acid according to claim 1, characterized in that: The lower trapping plate (542) is provided with a plurality of gradient-arranged lower trapping toothed rings (5425), and a plurality of gathering grooves (5423) are provided on the plurality of lower trapping toothed rings (5425). The bottom of the gathering grooves (5423) is provided with a drop outlet (5422). The lower trapping plate (542) is provided with a collection chamber (5421). The drop outlet (5422) is connected to the collection chamber (5421). A connection port (5424) is provided on one side of the collection chamber (5421). The collection chamber (5421) is connected to the return assembly (51) through the connection port (5424).

3. The evaporation and purification equipment for high-purity electronic-grade hydrochloric acid according to claim 2, characterized in that: The upper trapping plate (541) is provided with a plurality of upper trapping toothed rings (5411) arranged in a gradient, and the plurality of upper trapping toothed rings (5411) and the plurality of lower trapping toothed rings (5425) form a dynamically adjustable wave trapping cavity (543).

4. The evaporation and purification equipment for high-purity electronic-grade hydrochloric acid according to claim 3, characterized in that: The reflux assembly (51) includes a reflux pipe (511), on which a plurality of guide pipes (512) are installed. The guide pipes (512) are connected to the collection chamber (5421) through the connection port (5424). The reflux pipe (511) passes through the outer slope ring (521) and is connected to the waste liquid area (4). A flow detector is installed inside the guide pipes (512).

5. The evaporation and purification equipment for high-purity electronic-grade hydrochloric acid according to claim 4, characterized in that: The inner wall of the cylinder (53) forms a collection chamber (533), which is connected to the swirl chamber (525). The cylinder (53) has several strip-shaped openings (531) inside. The collection chamber (533) is connected to the wave collection cavity (543) through the strip-shaped openings (531). The inner wall of the cylinder (53) is equipped with several collection plates (532).

6. The evaporation and purification equipment for high-purity electronic-grade hydrochloric acid according to claim 5, characterized in that: The tower body (1) is provided with an exhaust port (12) at the top, which is connected to an external condenser through a pipe. The tower body (1) is provided with a feed inlet (11), and the liquid distributor (3) is connected to an external raw material tank through the feed inlet (11). The tower body (1) is provided with an air inlet (13) and a liquid outlet (14) at the bottom. The air inlet (13) is connected to an evaporator through a pipe, and the liquid outlet (14) is connected to a waste liquid tank through a pipe.

7. A method for evaporating and purifying high-purity electronic-grade hydrochloric acid, characterized in that: Using the evaporation and purification equipment for high-purity electronic-grade hydrochloric acid as described in claim 6, the evaporation and purification method includes the following steps: S1. The hydrochloric acid raw material to be purified is conveyed to the distributor (3) through the feed inlet (11). The distributor (3) distributes the hydrochloric acid raw material to several sets of packing (2) in the tower body (1), so that the hydrochloric acid raw material flows downward along the packing (2). S2. Start the external evaporator so that high-temperature steam enters the waste liquid zone (4) at the bottom of the tower body (1) through the air inlet (13) and heats the acid liquid in the waste liquid zone (4) so ​​that the volatile hydrochloric acid components in the waste liquid zone (4) continue to vaporize. S3. High-temperature hydrochloric acid mixed steam enters the swirl chamber (525) and forms a rotating upward airflow under the action of the spiral blade (523), causing the impurity droplets in the mixed steam to deflect towards the inner wall of the cylinder (53), and are then initially captured by the inner wall of the cylinder (53) and the collecting blade (532); S4. The mixed steam after primary capture enters the wave capture chamber (543) through the strip-shaped inlet (531) and flows between the upper capture toothed ring (5411) and the lower capture toothed ring (5425), causing the residual acid mist droplets to collide and coalesce before entering the collection chamber (5421) through the collection tank (5423) and the drop outlet (5422), and then being introduced into the waste liquid area (4) through the guide pipe (512) and the return pipe (511); the control system adjusts the position of the upper capture plate (541) according to the waste liquid flow rate in the guide pipe (512) to change the flow gap of the wave capture chamber (543); S5. After being processed by the isolation and discharge mechanism (5), the hydrochloric acid vapor enters the exhaust chamber (6) and continues to pass through several sets of packing (2) for gas-liquid mass transfer. Then it is discharged from the exhaust port (12) at the top of the tower body (1) and enters the external condenser for condensation and recovery. The waste liquid containing impurities accumulated in the waste liquid area (4) is discharged to the waste liquid tank through the drain port (14).

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