An electronic grade hydrochloric acid preparation device and method thereof

Abstract

The application relates to the technical field of hydrochloric acid preparation, in particular to an electronic-grade hydrochloric acid preparation device and a method thereof. The device comprises a stand, a mounting seat fixedly arranged at the bottom of the stand, vertically-arranged telescopic columns arranged at the upper and lower ends of the stand, and a plurality of adsorption structures evenly distributed on the outer side of the stand. The adsorption structures are evenly divided into a first adsorption cylinder and a second adsorption cylinder, and the first adsorption cylinder and the second adsorption cylinder are staggered. When the telescopic column is elongated, the sliding column slides upwards along the vertical groove, and under the abutment of the first abutment block, the sliding column enters the inclined groove. The sliding column continues to slide upwards, abuts against the inclined groove, and makes the connecting sleeve rotate by one station as a whole, so that each adsorption structure alternately bears higher working pressure, the working state of each adsorption structure is stable and uniform, and the device can effectively work for a long time.

Description

Technical Field

[0001] This invention relates to the field of hydrochloric acid preparation technology, and in particular to an electronic-grade hydrochloric acid preparation apparatus and method. Background Technology

[0002] Hydrochloric acid is an aqueous solution of hydrogen chloride and is a common chemical. Depending on its application, hydrochloric acid can be classified into industrial grade, electronic grade, and reagent grade. Electronic grade hydrochloric acid refers to products that can be used in pharmaceuticals, chemicals, semiconductors, and large-scale integrated circuits. Electronic grade hydrochloric acid represents a high-end, high-performance product, requiring a purity of over 99.999% and extremely low levels of organic impurities such as ferric chloride complexes. Removing ferric chloride complexes is particularly important in the preparation of electronic grade hydrochloric acid.

[0003] The prior art discloses a purification device and process for electronic-grade hydrochloric acid, with publication number CN116161621B. The device includes a hydrochloric acid feeding mechanism, a hydrochloric acid adsorption mechanism, and a hydrochloric acid distillation mechanism arranged sequentially. The hydrochloric acid adsorption mechanism includes exchange columns and a rinsing assembly. The exchange columns are arranged in a circular array around a vertical column, which is filled with adsorption resin. Each exchange column has pipe connectors at both ends, which are connected to the rinsing assembly via water pipes. Each exchange column is equipped with a hydrochloric acid connector, one of which connects to the hydrochloric acid feeding mechanism, and the other connects to the hydrochloric acid distillation mechanism. The purification device proposed in this invention can achieve automated adsorption and removal of iron-chlorine complexes from industrial hydrochloric acid, with high adsorption efficiency. It can also rapidly rinse and regenerate the resin in the exchange columns, thus meeting the requirements for large-scale, efficient purification of electronic-grade hydrochloric acid.

[0004] However, in the process of using the above technical solution, since the exchange column in the hydrochloric acid adsorption mechanism flows through the hydrochloric acid solution and the rinsing liquid in sequence, and the flow path is fixed, the exchange column near the hydrochloric acid inlet is always in a saturated working state under long-term operation, and is more prone to wear and tear, while the exchange column near the drain outlet has a lower working pressure and is relatively less prone to wear and tear. The uneven working state of the exchange column leads to differences in the service life of the exchange column, and replacement often results in waste. Moreover, since the pipeline position is fixed, multiple pipelines need to be set on one exchange column to meet the adsorption and rinsing steps, and the structure is relatively complicated. Summary of the Invention

[0005] The purpose of this invention is to solve the problems in the background art by providing an electronic-grade hydrochloric acid preparation apparatus and method.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] An electronic-grade hydrochloric acid preparation apparatus includes a column with a mounting base fixedly installed at its bottom and vertically extending telescopic columns installed at both the top and bottom ends of the column; several adsorption structures evenly distributed on the outer side of the column, the adsorption structures being evenly divided into a first adsorption cylinder and a second adsorption cylinder, the first and second adsorption cylinders being alternately distributed; an upper connecting seat located at the top of the adsorption structures, the bottom of the upper connecting seat being fixedly connected to the telescopic columns at the top of the column, and the bottom of the upper connecting seat being fixedly connected to multiple female connectors that mate with the adsorption structures; and a lower connecting seat located at the bottom of the adsorption structures, the top of the lower connecting seat being fixedly connected to the telescopic columns at the bottom of the column, and the top of the lower connecting seat also being fixedly connected to multiple female connectors that mate with the adsorption structures. The upper and lower connecting seats are equipped with... The lower connecting seat is equipped with a connecting pipe, and a hydrochloric acid discharge connector, a rinsing fluid discharge connector, a hydrochloric acid feed connector, and a rinsing fluid inlet connector. Multiple adsorption cylinders of type one are connected in series via the connecting pipe to form a type one adsorption system. The two ends of the type one adsorption system are connected to the hydrochloric acid feed connector and the hydrochloric acid discharge connector respectively via female connectors. Multiple adsorption cylinders of type two are connected in series via the connecting pipe to form a type two adsorption system. The two ends of the type two adsorption system are connected to the rinsing fluid inlet connector and the rinsing fluid discharge connector respectively via female connectors. A connecting sleeve is used to install multiple adsorption structures, and the connecting sleeve is rotatably connected to the outer wall of the column. An angle transmission device is also included to drive the connecting sleeve to rotate. The angle transmission device is installed on the upper connecting seat, and each time the upper connecting seat is lifted upwards, the angle transmission device drives the connecting sleeve to rotate one position.

[0008] In the aforementioned electronic-grade hydrochloric acid preparation apparatus, the angle transmission device includes multiple vertically arranged slide bars. The upper end of each slide bar is fixedly connected to the bottom of the upper connecting seat, and the lower end of each slide bar is fixedly connected to a sliding column. The inner side of the connecting sleeve has multiple vertically arranged grooves. The angle from an adjacent groove to the center of the connecting sleeve is one station. The angle from an adjacent adsorption structure to the center of the column is the same as the angle from an adjacent groove to the center of the connecting sleeve. The inner wall of the connecting sleeve also has multiple inclined grooves. The sliding column is slidably connected to the inner walls of the grooves and the inclined grooves. The inclined groove is located between two adjacent grooves. The upper end of the inclined groove is connected to the upper end of one of the grooves, and the lower end of the inclined groove is connected to the middle of another groove.

[0009] In the above-mentioned electronic-grade hydrochloric acid preparation apparatus, a first abutment block is fixedly connected to the middle of the side of each vertical trough away from the inclined trough, and a second abutment block is fixedly connected to the inner side of the upper end of each inclined trough.

[0010] In the above-mentioned electronic-grade hydrochloric acid preparation device, the adsorption structure includes a cylindrical body, the interior of which is filled with adsorption resin, and sub-connectors are fixedly connected to both the upper and lower ends of the cylindrical body. A mounting frame is fixedly connected to the outer wall of the cylindrical body, and the mounting frame is fixedly connected to the outer wall of the connecting sleeve.

[0011] In the aforementioned electronic-grade hydrochloric acid preparation apparatus, the lower end of the female connector has a slot adapted to the female connector. The female connector is inserted into the slot. A sealing airbag is fixedly connected to the inner wall of the slot. Multiple gas guide tubes are installed on the female connector. One end of each gas guide tube is connected to the inside of the sealing airbag. Main gas pipes are installed inside both the upper and lower connecting seats. The other end of each gas guide tube is connected to the inside of the main gas pipe. Gas connectors are fixedly connected to both the upper and lower connecting seats. One end of each gas connector is connected to the main gas pipe. An annular protrusion is fixedly connected to the outer wall of the female connector. The annular protrusion serves to limit the movement of the cylinder.

[0012] In the above-mentioned electronic-grade hydrochloric acid preparation device, a rubber gasket is fixedly connected to the inner wall of the slot, and the rubber gasket serves to seal between the female connector and the female connector.

[0013] In the above-mentioned electronic-grade hydrochloric acid preparation device, a bearing sleeve is fixedly connected to the bottom of the connecting sleeve, and the connecting sleeve is rotatably connected to the outer wall of the column through the bearing sleeve.

[0014] In the above-mentioned electronic-grade hydrochloric acid preparation device, the upper connecting seat and the lower connecting seat are both composed of an inner ring plate, an outer ring plate and a number of connecting rods. The outer side of the inner ring plate is fixedly connected to the inner side of the outer ring plate through a number of connecting rods.

[0015] A method for preparing electronic-grade hydrochloric acid, using the aforementioned electronic-grade hydrochloric acid preparation apparatus, specifically includes the following steps:

[0016] S1. Select industrial-grade hydrochloric acid. Connect the industrial-grade hydrochloric acid to the hydrochloric acid feed connector through the feed pipe, connect the hydrochloric acid discharge connector to the discharge pipe, connect the rinsing fluid inlet connector to the rinsing pipe, and connect the rinsing fluid discharge directly to the drain pipe. Use ultrapure water as the rinsing fluid.

[0017] S2. Industrial-grade hydrochloric acid flows through a No. 2 adsorption system formed by multiple No. 2 adsorption cylinders and connecting pipes. The adsorption resin inside the No. 2 adsorption cylinder adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. The hydrochloric acid liquid after adsorption is discharged from the hydrochloric acid discharge joint.

[0018] S3. Extend the telescopic columns at both ends of the column so that the female and male connectors on the upper and lower connecting seats are separated from the adsorption structure. When the telescopic column is fully extended, the connecting sleeve rotates one position under the transmission of the angle transmission device. At this time, the No. 1 adsorption system formed by multiple No. 1 adsorption cylinders and connecting pipes will be connected to the hydrochloric acid feed connector and the hydrochloric acid discharge connector, while the No. 2 adsorption system formed by multiple No. 2 adsorption cylinders and connecting pipes will be connected to the flushing liquid feed connector and the flushing liquid discharge connector.

[0019] S4. The rinsing solution flows through the No. 2 adsorption system, which is formed by multiple No. 2 adsorption cylinders and connecting pipes, to wash off the adsorption resin inside the No. 2 adsorption cylinders for later use. At this time, industrial-grade hydrochloric acid can be introduced through the No. 1 adsorption system, which is formed by multiple No. 1 adsorption cylinders and connecting pipes. The adsorption resin inside the No. 1 adsorption cylinder adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. This process is repeated to purify the industrial-grade hydrochloric acid. Moreover, after each transmission by the angle transmission device, the arrangement order of the No. 1 adsorption cylinders and the No. 2 adsorption cylinders inside the No. 2 adsorption system will change.

[0020] S5. The purified industrial-grade hydrochloric acid is sent to the hydrochloric acid distillation unit, and electronic-grade salt is obtained after distillation.

[0021] Compared with existing technologies, the advantages of this electronic-grade hydrochloric acid preparation apparatus and method are as follows:

[0022] 1. Through the connecting sleeve, when the telescopic column is extended, the sliding column will slide upward along the vertical groove. At this time, the upper connecting seat and the lower connecting seat are disengaged from the adsorption structure. Then, under the abutment of the first contact block, the sliding column will enter the inclined groove. The sliding column continues to slide upward and abuts the inclined groove, causing the connecting sleeve to rotate one position. This allows each adsorption structure to alternately bear a high working pressure. The working state of each adsorption structure is stable, uniform and stable, ensuring that the device works effectively for a long time.

[0023] 2. During adsorption and rinsing operations, the adsorption structure can be easily switched simply by extending and shortening the telescopic column. That is, the No. 1 adsorption cylinder, which was originally connected to the rinsing liquid drain and inlet connectors, is rotated to be connected to the hydrochloric acid discharge and inlet connectors, and the No. 2 adsorption cylinder is connected to the rinsing liquid drain and inlet connectors. After the telescopic column is repeatedly extended and shortened, the No. 1 and No. 2 adsorption cylinders will rotate regularly. The structure is compact and the operation is convenient.

[0024] 3. After the adsorption structure is connected to the female connector, air is injected into the main air pipe through the air connector, causing the sealing airbag to expand. This allows the sealing airbag to fit snugly against the female connector, preventing hydrochloric acid from evaporating or leaking to the outside during adsorption. Attached Figure Description

[0025] Figure 1 This is a three-dimensional structural schematic diagram of the present invention;

[0026] Figure 2 This is a three-dimensional structural diagram of the present invention from another perspective;

[0027] Figure 3 This is a cross-sectional structural schematic diagram of the present invention;

[0028] Figure 4 This is a schematic diagram of the structure of the present invention after the adsorption cylinder has been removed;

[0029] Figure 5 This is a schematic diagram of the adsorption cylinder of the present invention;

[0030] Figure 6 This is a schematic diagram of the upper connecting seat of the present invention;

[0031] Figure 7 This is a schematic diagram of the connecting sleeve of the present invention;

[0032] Figure 8 This is the invention Figure 7 Enlarged structural diagram at point D;

[0033] Figure 9 This is the invention Figure 3 Enlarged schematic diagram of the structure at point C.

[0034] In the diagram: 1. Column; 2. Mounting base; 3. Upper connecting base; 4. Lower connecting base; 5. Connecting sleeve; 6. Adsorption structure; 6A. No. 1 adsorption cylinder; 6B. No. 2 adsorption cylinder; 7. Female connector; 8. Connecting pipe; 9. Telescopic column; 10. Sliding bar; 11. Sliding column; 12. Vertical groove; 13. Inclined groove; 14. First contact block; 15. Second contact block; 16. Cylinder body; 17. Adsorption resin; 18. Sub-connector; 19. Mounting frame; 20. Bearing sleeve; 21. Slot; 22. Sealing airbag; 23. Air guide pipe; 24. Main air pipe; 25. Air connector; 26. Annular protrusion; 27. Rubber pad; 28. Inner ring plate; 29. ​​Outer ring plate; 30. Connecting rod; 31. Hydrochloric acid discharge connector; 32. Rinsing fluid discharge connector; 33. Hydrochloric acid feed connector; 34. Rinsing fluid inlet connector. Detailed Implementation

[0035] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0036] In the description of this invention, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0037] Reference Figures 1-9 An electronic-grade hydrochloric acid preparation apparatus for purifying industrial-grade hydrochloric acid includes a column 1 with a mounting base 2 fixedly installed at its bottom and vertically arranged telescopic columns 9 installed at both the top and bottom of the column 1; several adsorption structures 6 evenly distributed on the outside of the column 1, the adsorption structures 6 being evenly divided into adsorption cylinder 6A and adsorption cylinder 6B, with adsorption cylinder 6A and adsorption cylinder 6B alternating; an upper connecting seat 3 located at the top of the adsorption structures 6, the bottom of the upper connecting seat 3 being fixedly connected to the telescopic columns 9 at the top of the column 1, and the bottom of the upper connecting seat 3 being fixedly connected to multiple female connectors 7 that mate with the adsorption structures 6; and a lower connecting seat 4 located at the bottom of the adsorption structures 6, the top of the lower connecting seat 4 being fixedly connected to the telescopic columns 9 at the bottom of the column 1, and the top of the lower connecting seat 4 also being fixedly connected to multiple female connectors 7 that mate with the adsorption structures 6. Each of the four bases is equipped with a connecting pipe 8. The lower connecting base 4 is equipped with a hydrochloric acid discharge connector 31, a rinsing fluid discharge connector 32, a hydrochloric acid feed connector 33, and a rinsing fluid inlet connector 34. Multiple adsorption cylinders 6A are connected in series through the connecting pipes 8 to form an adsorption system. The two ends of the adsorption system are connected to the hydrochloric acid feed connector 33 and the hydrochloric acid discharge connector 31 through female connectors 7, respectively. Multiple adsorption cylinders 6B are connected in series through the connecting pipes 8 to form an adsorption system. The two ends of the adsorption system are connected to the rinsing fluid inlet connector 34 and the rinsing fluid discharge connector 32 through female connectors 7, respectively. A connecting sleeve 5 is used to install multiple adsorption structures 6. The connecting sleeve 5 is rotatably connected to the outer wall of the column 1. An angle transmission device is used to drive the connecting sleeve 5 to rotate. The angle transmission device is installed on the upper connecting base 3. Each time the upper connecting base 3 is lifted upward, the angle transmission device will drive the connecting sleeve 5 to rotate one position.

[0038] Based on one feasible solution of the above technical solution, the angle transmission device includes multiple vertically arranged slide bars 10. The upper end of the slide bar 10 is fixedly connected to the bottom of the upper connecting seat 3, and the lower end of the slide bar 10 is fixedly connected to a sliding column 11. Multiple vertically arranged vertical grooves 12 are opened on the inner side of the connecting sleeve 5. The angle from the adjacent vertical groove 12 to the center of the connecting sleeve 5 is one station. The angle from the adjacent adsorption structure 6 to the center of the column 1 is the same as the angle from the adjacent vertical groove 12 to the center of the connecting sleeve 5. Multiple inclined grooves 13 are also opened on the inner wall of the connecting sleeve 5. The sliding column 11 is slidably connected to the inner wall of the vertical groove 12 and the inclined groove 13. The inclined groove 13 is located between two adjacent vertical grooves 12, and the upper end of the inclined groove 13 is connected to one of them. The upper ends of the vertical grooves 12 are connected, and the lower end of the inclined groove 13 is connected to the middle of another vertical groove 12. A first abutment block 14 is fixedly connected to the middle of the side of each vertical groove 12 away from the inclined groove 13, and a second abutment block 15 is fixedly connected to the inner side of the upper end of each inclined groove 13. The first abutment block 14 and the second abutment block 15 are both made of elastic material. In the initial state, the sliding column 11 will be at the bottom of the vertical groove 12. Whenever the telescopic column 9 extends, the sliding column 11 will slide upward along the vertical groove 12. At this time, the upper connecting seat 3 and the lower connecting seat 4 will disengage from the adsorption structure 6. Then, under the abutment of the first abutment block 14, the sliding column 11 will enter the inclined groove 13 and continue to slide upward. Column 11 abuts against inclined groove 13, causing connecting sleeve 5 to rotate one position. This means that adsorption cylinder 6A, originally connected to flushing fluid drain connector 32 and flushing fluid inlet connector 34, rotates to connect with hydrochloric acid discharge connector 31 and hydrochloric acid inlet connector 33, while adsorption cylinder 6B connects to flushing fluid drain connector 32 and flushing fluid inlet connector 34. After repeated extension and retraction of telescopic column 9, adsorption cylinders 6A and 6B will rotate regularly, alternately connecting with flushing fluid drain connector 32 and flushing fluid inlet connector 34. Each time the angle transmission device passes through, the arrangement order of adsorption cylinders 6A and 6B within the adsorption system will change. The arrangement of adsorption cylinders 6A is varied. For example, adsorption cylinder 6A1 is divided into adsorption cylinder 6A2, adsorption cylinder 6A3, ... adsorption cylinder 6An. After rotating one station, adsorption cylinder 6B will replace adsorption cylinder 6A. After rotating another station, adsorption cylinder 6A will replace adsorption cylinder 6B. However, the order of adsorption cylinders 6A is adsorption cylinder 6A2, adsorption cylinder 6A3, ... adsorption cylinder 6An, adsorption cylinder 6A1. This allows each adsorption structure 6 to alternately bear a high working pressure. The working state of each adsorption structure 6 is stable, uniform, and consistent, ensuring that the device works effectively for a long time. The overall structure of the device is compact and easy to operate.

[0039] Based on one feasible solution of the above technical solution, the adsorption structure 6 includes a cylinder 16, the inside of the cylinder 16 is filled with adsorption resin 17, the upper and lower ends of the cylinder 16 are fixedly connected with sub-connectors 18, the outer wall of the cylinder 16 is fixedly connected with a mounting bracket 19, and the mounting bracket 19 is fixedly connected to the outer wall of the connecting sleeve 5.

[0040] Based on one feasible solution of the above technical solution, the lower end of the female connector 7 is provided with a slot 21 that is adapted to the female connector 18. The female connector 18 is inserted into the slot 21. A sealing airbag 22 is fixedly connected to the inner wall of the slot 21. Multiple air guide tubes 23 are installed on the female connector 7. One end of the air guide tube 23 is connected to the inside of the sealing airbag 22. The upper connecting seat 3 and the lower connecting seat 4 are both equipped with main air pipes 24. The other end of the air guide tube 23 is connected to the inside of the main air pipe 24. The upper connecting seat 3 and the lower connecting seat 4 are both equipped with main air pipes 24. Each connector 4 is fixedly connected with an air connector 25. One end of the air connector 25 is connected to the main air pipe 24. The outer wall of the sub-connector 18 is fixedly connected with an annular protrusion 26, which serves to limit the position of the cylinder 16. After the adsorption structure 6 is connected to the female connector 7, air is injected into the main air pipe 24 through the air connector 25, causing the sealing air bag 22 to expand. This allows the sealing air bag 22 to fit with the sub-connector 18, preventing hydrochloric acid from evaporating and leaking to the outside during adsorption.

[0041] Based on one feasible solution of the above technical solution, a rubber pad 27 is fixedly connected to the inner wall of the slot 21, and the rubber pad 27 plays the role of sealing between the female connector 7 and the female connector 18.

[0042] Based on one feasible solution of the above technical solution, a bearing sleeve 20 is fixedly connected to the bottom of the connecting sleeve 5, and the connecting sleeve 5 is rotatably connected to the outer wall of the column 1 through the provided bearing sleeve 20.

[0043] Based on one feasible solution of the above technical solution, the upper connecting seat 3 and the lower connecting seat 4 are both composed of an inner ring piece 28, an outer ring piece 29 and a number of connecting rods 30. The outer side of the inner ring piece 28 is fixedly connected to the inner side of the outer ring piece 29 through a number of connecting rods 30. The mounting seat 2 extends to the outside through the inner ring piece 28.

[0044] A method for preparing electronic-grade hydrochloric acid, using the aforementioned electronic-grade hydrochloric acid preparation apparatus, specifically includes the following steps:

[0045] S1. Select industrial-grade hydrochloric acid, connect the industrial-grade hydrochloric acid to the hydrochloric acid feed connector 33 through the feed pipe, connect the hydrochloric acid discharge connector 31 to the discharge pipe, connect the rinsing liquid inlet connector 34 to the rinsing pipe, and connect the rinsing liquid discharge connector 32 to the drain pipe. Use ultrapure water as the rinsing liquid.

[0046] S2. Industrial-grade hydrochloric acid flows through a No. 2 adsorption system formed by multiple No. 2 adsorption cylinders 6B and connecting pipes 8. The adsorption resin 17 inside the No. 2 adsorption cylinder 6B adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. The hydrochloric acid liquid after adsorption is discharged from the hydrochloric acid discharge joint 31.

[0047] S3. The telescopic columns 9 at both ends of the extended column 1 are extended so that the female connector 7 and the female connector 18 on the upper connecting seat 3 and the lower connecting seat 4 are separated from the adsorption structure 6. When the telescopic column 9 is fully extended, under the transmission of the angle transmission device, the connecting sleeve 5 is rotated one position. At this time, the first adsorption system formed by multiple first adsorption cylinders 6A and connecting pipes 8 will be connected to the hydrochloric acid feed connector 33 and the hydrochloric acid discharge connector 31, while the second adsorption system formed by multiple second adsorption cylinders 6B and connecting pipes 8 will be connected to the rinsing liquid inlet connector 34 and the rinsing liquid outlet connector 32.

[0048] S4. The rinsing liquid flows through the No. 2 adsorption system formed by multiple No. 2 adsorption cylinders 6B and connecting pipe 8, and washes off the adsorption resin 17 inside the No. 2 adsorption cylinder 6B for later use. At this time, industrial-grade hydrochloric acid can be introduced and flows through the No. 1 adsorption system formed by multiple No. 1 adsorption cylinders 6A and connecting pipe 8. The adsorption resin 17 inside the No. 1 adsorption cylinder 6A adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. This process is repeated to purify the industrial-grade hydrochloric acid. Moreover, after each transmission by the angle transmission device, the arrangement order of the No. 1 adsorption cylinder 6A and the No. 2 adsorption cylinder 6B inside the adsorption system will change.

[0049] S5. The purified industrial-grade hydrochloric acid is sent to the hydrochloric acid distillation unit, and electronic-grade salt is obtained after distillation.

[0050] To further clarify, the aforementioned fixed connection should be interpreted broadly unless otherwise explicitly specified and limited. For example, it may be welding, gluing, or integral molding, or other conventional methods well known to those skilled in the art.

[0051] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. An apparatus for preparing electronic-grade hydrochloric acid, characterized in that, include: The column (1) has a mounting base (2) fixedly installed at its bottom, and vertical telescopic columns (9) are installed at both the upper and lower ends of the column (1). Several adsorption structures (6) are evenly distributed on the outside of the column (1). The adsorption structures (6) are evenly divided into adsorption cylinder No. 1 (6A) and adsorption cylinder No. 2 (6B). The adsorption cylinder No. 1 (6A) and adsorption cylinder No. 2 (6B) are distributed alternately. Upper connecting seat (3), the upper connecting seat (3) is located at the top of the adsorption structure (6), the bottom of the upper connecting seat (3) is fixedly connected to the telescopic column (9) at the top of the column (1), and the bottom of the upper connecting seat (3) is fixedly connected to a plurality of female connectors (7) that cooperate with the adsorption structure (6). The lower connecting seat (4) is located at the bottom of the adsorption structure (6). The top of the lower connecting seat (4) is fixedly connected to the telescopic column (9) at the bottom of the column (1). The top of the lower connecting seat (4) is also fixedly connected to multiple female connectors (7) that cooperate with the adsorption structure (6). Both the upper connecting seat (3) and the lower connecting seat (4) are equipped with connecting pipes (8). The lower connecting seat (4) is equipped with a hydrochloric acid discharge connector (31), a rinsing liquid discharge connector (32), a hydrochloric acid feed connector (33), and a rinsing liquid feed connector. The liquid inlet connector (34) is used to connect multiple No. 1 adsorption cylinders (6A) in series through the set connecting pipe (8) to form a No. 1 adsorption system. The two ends of the No. 1 adsorption system are connected to the hydrochloric acid inlet connector (33) and the hydrochloric acid outlet connector (31) respectively through the set female connector (7). The multiple No. 2 adsorption cylinders (6B) are connected in series through the set connecting pipe (8) to form a No. 2 adsorption system. The two ends of the No. 2 adsorption system are connected to the rinsing liquid inlet connector (34) and the rinsing liquid outlet connector (32) respectively through the set female connector (7). A connecting sleeve (5) is used to install multiple adsorption structures (6), and the connecting sleeve (5) is rotatably connected to the outer wall of the column (1); An angle transmission device is provided to drive the connecting sleeve (5) to rotate. The angle transmission device is installed on the upper connecting seat (3). Each time the upper connecting seat (3) is lifted upward, the angle transmission device will drive the connecting sleeve (5) to rotate one position.

2. The electronic-grade hydrochloric acid preparation apparatus according to claim 1, characterized in that: The angle transmission device includes multiple vertically arranged slide bars (10). The upper end of the slide bar (10) is fixedly connected to the bottom of the upper connecting seat (3). The lower end of the slide bar (10) is fixedly connected to a slide column (11). The inner side of the connecting sleeve (5) is provided with multiple vertically arranged vertical grooves (12). The angle from the adjacent vertical groove (12) to the center of the connecting sleeve (5) is one station. The angle from the adjacent adsorption structure (6) to the center of the column (1) is the same as the angle from the adjacent vertical groove (12) to the center of the connecting sleeve (5). The inner wall of the connecting sleeve (5) is also provided with multiple inclined grooves (13). The slide column (11) is slidably connected to the inner wall of the vertical groove (12) and the inclined groove (13). The inclined groove (13) is located between two adjacent vertical grooves (12). The upper end of the inclined groove (13) is connected to the upper end of one of the vertical grooves (12). The lower end of the inclined groove (13) is connected to the middle of the other vertical groove (12).

3. The electronic-grade hydrochloric acid preparation apparatus according to claim 2, characterized in that: Each vertical groove (12) has a first abutment block (14) fixedly connected to the middle of the side away from the inclined groove (13), and a second abutment block (15) fixedly connected to the inner side of the upper end of each inclined groove (13).

4. The electronic-grade hydrochloric acid preparation apparatus according to claim 3, characterized in that: The adsorption structure (6) includes a cylinder (16), the inside of which is filled with adsorption resin (17). Sub-connectors (18) are fixedly connected to both the upper and lower ends of the cylinder (16). An installation frame (19) is fixedly connected to the outer wall of the cylinder (16), and the installation frame (19) is fixedly connected to the outer wall of the connecting sleeve (5).

5. The electronic-grade hydrochloric acid preparation apparatus according to claim 4, characterized in that: The lower end of the female connector (7) is provided with a slot (21) that is compatible with the female connector (18). The female connector (18) is inserted into the slot (21). A sealing airbag (22) is fixedly connected to the inner wall of the slot (21). Multiple air guide tubes (23) are installed on the female connector (7). One end of the air guide tube (23) is connected to the inside of the sealing airbag (22). The upper connecting seat (3) and the lower connecting seat (4) are both equipped with main air pipes (24). The other end of the air guide tube (23) is connected to the inside of the main air pipe (24). Air connectors (25) are fixedly connected to the upper connecting seat (3) and the lower connecting seat (4). One end of the air connector (25) is connected to the main air pipe (24). An annular protrusion (26) is fixedly connected to the outer wall of the female connector (18). The annular protrusion (26) serves to limit the position of the cylinder (16).

6. The electronic-grade hydrochloric acid preparation apparatus according to claim 5, characterized in that: A rubber pad (27) is fixedly connected to the inner wall of the slot (21), and the rubber pad (27) serves to seal between the female connector (7) and the female connector (18).

7. The electronic-grade hydrochloric acid preparation apparatus according to claim 1, characterized in that: The bottom of the connecting sleeve (5) is fixedly connected to a bearing sleeve (20), and the connecting sleeve (5) is rotatably connected to the outer wall of the column (1) through the bearing sleeve (20).

8. The electronic-grade hydrochloric acid preparation apparatus according to claim 1, characterized in that: The upper connecting seat (3) and the lower connecting seat (4) are both composed of an inner ring plate (28), an outer ring plate (29) and several connecting rods (30). The outer side of the inner ring plate (28) is fixedly connected to the inner side of the outer ring plate (29) through several connecting rods (30).

9. A method for preparing electronic-grade hydrochloric acid, characterized in that, The electronic-grade hydrochloric acid preparation apparatus as described in any one of claims 1-8 specifically includes the following steps: S1. Select industrial-grade hydrochloric acid, connect the industrial-grade hydrochloric acid to the hydrochloric acid feed connector (33) through the feed pipe, connect the hydrochloric acid discharge connector (31) to the drain pipe, connect the rinsing liquid inlet connector (34) to the rinsing pipe, connect the rinsing liquid discharge connector (32) to the drain pipe, and use ultrapure water as the rinsing liquid. S2. Industrial-grade hydrochloric acid flows through a No. 2 adsorption system formed by multiple No. 2 adsorption cylinders (6B) and connecting pipes (8). The adsorption resin (17) inside the No. 2 adsorption cylinder (6B) adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. The hydrochloric acid liquid after adsorption is discharged from the hydrochloric acid discharge joint (31). S3. Extend the telescopic columns (9) at both ends of the column (1) so that the female connector (7) and the female connector (18) on the upper connecting seat (3) and the lower connecting seat (4) are separated from the adsorption structure (6). When the telescopic column (9) is fully extended, under the transmission of the angle transmission device, the connecting sleeve (5) rotates one position. At this time, the No. 1 adsorption system formed by multiple No. 1 adsorption cylinders (6A) and connecting pipes (8) will dock with the hydrochloric acid feed connector (33) and the hydrochloric acid discharge connector (31), while the No. 2 adsorption system formed by multiple No. 2 adsorption cylinders (6B) and connecting pipes (8) will dock with the rinsing liquid feed connector (34) and the rinsing liquid discharge connector (32). S4. The rinsing liquid flows through the No. 2 adsorption system formed by multiple No. 2 adsorption cylinders (6B) and connecting pipes (8) to wash off the adsorption resin (17) inside the No. 2 adsorption cylinder (6B) for later use. At this time, industrial-grade hydrochloric acid is introduced and flows through the No. 1 adsorption system formed by multiple No. 1 adsorption cylinders (6A) and connecting pipes (8). The adsorption resin (17) inside the No. 1 adsorption cylinder (6A) adsorbs organic impurities such as iron-chlorine complexes in the hydrochloric acid. This process is repeated to purify the industrial-grade hydrochloric acid. Moreover, after each transmission by the angle transmission device, the arrangement order of the No. 1 adsorption cylinder (6A) inside the adsorption system and the No. 2 adsorption cylinder (6B) inside the No. 2 adsorption system will change. S5. The purified industrial-grade hydrochloric acid is sent to the hydrochloric acid distillation unit, and electronic-grade hydrochloric acid is obtained after distillation.

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