A distillation column and method for the distillation of electronic grade sulfuric acid

Abstract

The application discloses a kind of for semiconductor electronic grade sulfuric acid rectifying tower and rectification method, it is related to sulfuric acid rectification technical field, sulfuric acid rectifying tower includes tower body, extraction device, adjusting device and heater, heater and tower body pipeline intercommunication;Tower body is equipped with working cavity, several adjusting devices are equipped in working cavity, and extraction outlet is equipped in working cavity one side, extraction device and extraction outlet pipeline intercommunication, adjusting device includes separation component, baffle and deflection component, separation component and baffle are connected, and baffle and deflection component are connected, and deflection component is used to drive separation component rotation, separation component includes fixed packing and deflection packing, fixed packing axis and deflection packing axis are collinear, baffle is placed in working cavity, fixed packing is sleeved on baffle, baffle and deflection packing are rotatably connected, deflection component and deflection packing are connected, and deflection component adjusts replacement gap between fixed packing and deflection packing.

Description

Technical Field

[0001] This invention relates to the field of sulfuric acid distillation technology, specifically to a distillation column and distillation method for semiconductor electronic-grade sulfuric acid. Background Technology

[0002] High-purity sulfuric acid is used in semiconductor manufacturing as a cleaning agent and etching agent; it is also called electronic-grade sulfuric acid.

[0003] Currently, common industrial-grade sulfuric acid generally contains a significant amount of impurities, such as metal impurity ions and organic matter. Therefore, in the production of electronic-grade sulfuric acid, it is necessary to purify the industrial sulfuric acid to remove impurities and improve its purity level. However, current sulfuric acid production processes often employ fixed packing materials, resulting in fixed gaps for component replacement. Due to fluctuations in the feed material and reflux liquid, the accumulated liquid phase flows rapidly downwards under gravity, leading to insufficient replacement time for the rising gaseous components. This reduces the accuracy of gas-phase purification and the efficiency of liquid-phase recovery.

[0004] Furthermore, conventional distillation equipment cannot adaptively adjust to ensure distillation quality during fluctuations in incoming materials. Summary of the Invention

[0005] The purpose of this invention is to provide a semiconductor electronic-grade sulfuric acid distillation column and distillation method to solve the problem in the prior art where the packing gap for component replacement is fixed and cannot adapt to liquid phase fluctuations.

[0006] To achieve the above objectives, the present invention provides the following technical solution: A sulfuric acid distillation column includes a column body, a dispensing device, a regulating device, and a heater, with the heater and column body connected by pipelines. The tower body is equipped with a working chamber, which contains several adjusting devices. A extraction outlet is located on one side of the working chamber, and the extraction device and the extraction outlet pipeline are connected. The regulating device includes a separation component, a partition, and a deflection component. The separation component is connected to the partition, and the deflection component is connected to the partition. The deflection component is used to drive the separation component to rotate. The separation assembly includes stationary packing and deflecting packing, with the axes of the stationary packing and the deflecting packing collinear. The partition is placed inside the working chamber, and a fixed packing is fitted on the partition. The partition and the deflecting packing are rotatably connected. The deflecting assembly is connected to the deflecting packing, and the deflecting assembly adjusts the displacement gap between the fixed packing and the deflecting packing.

[0007] The tower body serves as the main load-bearing foundation, providing space for sulfuric acid distillation through the working chamber. Sulfuric acid vapor is generated by the heater and flows upward along the working chamber. The reflux liquid enters the working chamber and flows downward together with the raw material liquid, where it is replaced by sulfuric acid vapor at the regulating device. Excess sulfuric acid molecules in the liquid phase vaporize and enter the gas phase, while excess water vapor molecules in the vapor enter the liquid phase. This causes the water-absorbing solid-liquid liquid phase to continuously flow downward, while the purified sulfuric acid vapor continuously flows upward. Multiple regulating devices are installed to gradually purify the sulfuric acid vapor, making it easier to extract it from the outlet and ensuring its purity. A baffle plate is installed inside the working chamber to install the fixed packing and limit the installation of the deflecting packing. Both the fixed and deflecting packings adopt a comb-shaped design. During the rotation of the deflecting packings driven by the deflection assembly, they can insert into each other. The fixed and deflecting packings can be two semi-cylinders. When there is a large amount of downward flowing liquid phase, there is also a large amount of excess sulfuric acid in the liquid phase. Driven by the deflection assembly on the baffle plate, the deflecting packings rotate, and part of the deflecting packings inserts into the fixed packings, reducing the displacement gap between the fixed and deflecting packings. This reduces the instantaneous flow cross-section, thereby reducing the flow velocity. At the same time, it increases the contact area and improves the displacement efficiency.

[0008] Furthermore, the fixed packing is arranged in an arc shape, and several replacement grooves are provided on both sides of the fixed packing, with the axes of the several replacement grooves arranged collinearly; Several partition grooves are provided on both sides of the deflecting packing; A return channel is provided on one side of the working chamber; The replacement groove axis and the partition groove axis are set in the same line, the replacement groove and the partition groove are arranged in an alternating manner, and the replacement groove and the partition groove are set with openings at opposite ends.

[0009] Both the fixed packing and the deflecting packing are arranged in an arc shape to facilitate the adjustment of the displacement gap. The fixed packing cooperates with the displacement grooves on both sides and the partition grooves of the deflecting packing. When the deflecting packing rotates, the partition groove on one side and the adjacent displacement groove are inserted into each other in an alternating manner, creating a gap between the walls. The displacement groove at this point is the first displacement stroke, and the other side is the second displacement stroke. The displacement gap at this time includes the part where the displacement groove and the partition groove cooperate, as well as the remaining length of the displacement groove and the partition groove. As the insertion depth increases, the displacement gap becomes smaller and smaller, and the filtration effect on the gas phase and the recovery efficiency of the liquid phase become better and better.

[0010] Furthermore, the separation component also includes several replacement plates, the lower ends of which are arranged at an angle and the replacement plates are arc-shaped. Several compensation grooves are provided on one side of the deflection packing, and the compensation grooves are arranged vertically. The partition is arranged in a ring shape, and a rib is provided on the inner side of the partition. The axis of the supplement plate and the axis of the partition groove are collinear. The lower end of the supplement plate abuts against the rib. The supplement plate and the compensation groove are slidably connected.

[0011] A compensation groove is set on the outside of the partition groove on the other side. The compensation groove and the replacement plate slide. When the deflection packing rotates, it is guided by the rib plate installed on the partition. The replacement plate slides upward in the compensation groove and gradually inserts into the second replacement stroke. During the upward sliding process, the gap between the replacement plate and the replacement groove located in the second replacement stroke decreases.

[0012] Furthermore, the deflection assembly includes a deflection motor; The deflector packing has toothed grooves on its outer side; The partition is equipped with deflection grooves; The deflection motor is placed in the deflection slot, and the output end of the deflection motor is equipped with a gear. The deflection motor meshes with the gear and the slot.

[0013] The partition plate is used to install the deflection motor through the deflection slot. The deflection motor is used to output torque to drive the deflection packing to rotate. The torque is transmitted by gear and tooth meshing. The corresponding components can be made of acid corrosion resistant materials or coated with corrosion resistant coating.

[0014] Furthermore, the deflection assembly also includes a sensing plate and a trigger coil, with a trigger rod inside the sensing plate, and the trigger rod is made of magnetic material; A sensing cavity is provided on the inner side of the upper end of the partition; An elastic element is provided inside the sensing cavity. The side of the elastic element away from the wall of the sensing cavity abuts against the trigger rod. One end of the trigger rod is inserted into the trigger coil, and the trigger coil is placed inside the sensing cavity.

[0015] The trigger coil is installed in the induction chamber, which guides the sliding induction plate. The induction chamber is located above the packing material; the liquid phase contacts the induction plate before entering the packing. The greater the instantaneous liquid flow, the greater the pressure. This pressure pushes the induction plate along the induction chamber, causing the magnetic trigger rod to slide, resulting in the coil cutting magnetic lines of force and generating an induced current. The greater the liquid flow, the greater the current. A spring-like structure is used for pre-tensioning. When the induction plate moves, it compresses the spring. When the external liquid pressure decreases, the spring pushes the induction plate in the opposite direction, facilitating automatic adjustment based on instantaneous flow fluctuations.

[0016] Furthermore, the trigger coil and the deflection motor are electrically connected; When the liquid phase increases: the overlapping area of ​​the displacement tank and the partition tank increases, and the length of the partition tank into which the filling plate is inserted near the compensation tank increases.

[0017] As the liquid phase increases, the amount of sulfuric acid present in the liquid phase also increases. However, the increased flow rate can affect the replacement efficiency. The current generated on the trigger coil is used as a control signal to control the current input to the deflection motor. That is, when the liquid phase increases, the deflection motor drives the deflection packing to rotate. The partition groove near the first replacement stroke is inserted into the replacement groove for horizontal adjustment. The replacement plate moves upward, thus inserting into the replacement groove of the second replacement stroke for vertical adjustment. By adjusting the replacement gap in a dual-stroke manner, the replacement gap is reduced, the contact area is increased, and the liquid phase flow resistance is increased, extending the replacement time and ensuring replacement efficiency.

[0018] As an optimization, the extraction device includes a condenser, and a collection tank is provided at the lower end of the condenser; The collection trough is placed inside the working chamber, and one side of the collection trough is connected to the extraction outlet.

[0019] By setting up a condenser, sulfuric acid vapor is condensed at the extraction point and collected through a collection tank at the bottom. High-purity finished sulfuric acid is then exported through an extraction outlet, meeting the stringent requirements of semiconductor grade.

[0020] As an optimization, a feed inlet is provided on one side of the tower body, and a distributor is provided at the upper end of the working chamber. The return channel and the distributor pipeline are connected.

[0021] By setting up an inlet for automatic liquid feeding, the liquid undergoes initial displacement and preheating as it flows downwards, improving subsequent evaporation efficiency. A distributor ensures even distribution of the reflux liquid, enhancing distillation and purification efficiency.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows: Both the fixed packing and the deflecting packing adopt a comb-shaped design, which allows them to interlock during the rotation driven by the deflecting component. The fixed packing and the deflecting packing can be two semi-cylinders. When there is a large amount of downward-flowing liquid phase, there is also a large amount of excess sulfuric acid in the liquid phase. By driving the deflecting component on the baffle, the deflecting packing rotates, and a part of the deflecting packing inserts into the fixed packing, reducing the displacement gap between the fixed packing and the deflecting packing. This reduces the instantaneous flow cross-section, thereby reducing the flow velocity and increasing the contact area and displacement efficiency. When the deflecting packing rotates, the partition groove on one side and the adjacent displacement groove interlock, creating a gap between the walls. The displacement groove at this point is the first displacement stroke, and the other side is the second displacement stroke. The displacement gap at this point includes the part where the displacement groove and the partition groove cooperate, as well as the displacement... As the insertion depth increases, the remaining length of the trough and partition trough decreases, resulting in a smaller displacement gap and improved filtration efficiency for the gas phase and recovery efficiency for the liquid phase. When the deflecting packing rotates, it is guided by ribs mounted on the partition plate, allowing the compensation plate to slide upwards within the compensation trough and gradually insert into the second displacement stroke. During this upward sliding process, the gap between the compensation plate and the displacement trough located in the second displacement stroke decreases. The sensing chamber is located on the upper side of the packing, meaning that before the liquid phase enters the packing, it first contacts the sensing element. The greater the instantaneous liquid flow, the greater the pressure generated. This pressure pushes the sensing element to slide along the sensing chamber, causing the magnetic trigger rod to slide, which in turn causes the coil to cut magnetic field lines and generate an induced current. The greater the liquid flow, the greater the current generated. When the external liquid pressure decreases, the elastic element pushes the sensing element to move in the opposite direction, facilitating automatic adjustment based on instantaneous flow fluctuations. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram of the extraction device and adjustment device of the present invention; Figure 3 This is a schematic diagram of the deflection component structure of the present invention; Figure 4 This is a schematic diagram of the structure of the separate component of the present invention; Figure 5 This is a schematic diagram of the deflection packing rotation according to the present invention; Figure 6 This is a schematic diagram of the deflection power transmission of the present invention; Figure 7 for Figure 3 A magnified view of a portion of the view (A).

[0024] In the diagram: 1. Tower body; 11. Feed inlet; 12. Outlet; 13. Working chamber; 14. Return channel; 2. Outlet device; 21. Condenser; 22. Collection tank; 3. Adjustment device; 31. Separation assembly; 311. Fixed packing; 3111. Replacement tank; 312. Deflection packing; 3121. Isolation tank; 3122. Compensation tank; 3123. Toothed groove; 313. Filler plate; 314. Rib plate; 32. Partition plate; 321. Induction chamber; 322. Deflection tank; 33. Deflection assembly; 331. Induction plate; 332. Elastic element; 333. Trigger rod; 334. Trigger coil; 335. Deflection motor; 4. Heater; 5. Distributor. Detailed Implementation

[0025] 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.

[0026] Example: Figure 1 - Figure 7 As shown, the present invention provides a technical solution for a semiconductor electronic-grade sulfuric acid distillation column and distillation method.

[0027] The sulfuric acid distillation column includes a column body 1, a collection device 2, a regulating device 3, and a heater 4, with the heater 4 connected to the column body 1 by a pipeline; The tower body 1 is provided with a working chamber 13, and a number of adjusting devices 3 are provided in the working chamber 13. A mining outlet 12 is provided on one side of the working chamber 13, and the mining device 2 and the mining outlet 12 are connected by a pipeline. The adjusting device 3 includes a separation component 31, a partition plate 32, and a deflection component 33. The separation component 31 is connected to the partition plate 32, and the deflection component 33 is connected to the partition plate 32. The deflection component 33 is used to drive the separation component 31 to rotate. The separation assembly 31 includes a fixed packing 311 and a deflecting packing 312, with the axes of the fixed packing 311 and the deflecting packing 312 being collinear. The partition 32 is placed inside the working chamber 13. A fixed packing 311 is fitted on the partition 32. The partition 32 and the deflecting packing 312 are rotatably connected. The deflecting assembly 33 is connected to the deflecting packing 312. The deflecting assembly 33 adjusts the displacement gap between the fixed packing 311 and the deflecting packing 312.

[0028] The tower body 1 serves as the main supporting foundation, providing a space for sulfuric acid distillation through the working chamber 13. Sulfuric acid vapor is generated by the heater 4 and flows upward along the working chamber 13. The reflux liquid enters the working chamber and flows downward together with the raw material liquid, and is replaced by sulfuric acid vapor at the regulating device 3. Excess sulfuric acid molecules in the liquid phase vaporize and enter the gas phase, while excess water vapor molecules in the vapor enter the liquid phase, causing the water-absorbing solid-liquid liquid phase to continuously flow downward, while the impurity-removed sulfuric acid vapor continuously flows upward. The sulfuric acid vapor is gradually purified by multiple regulating devices 3, making it easier to finally be extracted from the outlet 12 and ensuring purity. The baffle 32 is installed in the working chamber 13 to install the fixed packing 311 and limit the installation of the deflecting packing 312. Both the fixed packing 311 and the deflecting packing 312 adopt a comb-shaped design. During the rotation of the deflecting packing 312 driven by the deflecting component 33, they can be inserted into each other. The fixed packing 311 and the deflecting packing 312 can be two semi-cylinders. When there is a large amount of downward flowing liquid phase, there is also a large amount of excess sulfuric acid in the liquid phase. By driving the deflecting component 33 on the baffle 32, the deflecting packing 312 rotates, and part of the deflecting packing 312 is inserted into the fixed packing, which reduces the displacement gap between the fixed packing 311 and the deflecting packing 312. This reduces the instantaneous flow cross section, thereby reducing the flow velocity. At the same time, it increases the contact area and improves the displacement efficiency.

[0029] Furthermore, the fixed packing 311 is arranged in an arc shape, and several replacement grooves 3111 are provided on both sides of the fixed packing 311, with the axes of the several replacement grooves 3111 being arranged collinearly. Several partition grooves 3121 are provided on both sides of the deflecting packing 312; A return channel 14 is provided on one side of the working chamber 13; The axis of the replacement groove 3111 and the axis of the partition groove 3121 are collinear, and the replacement groove 3111 and the partition groove 3121 are staggered, with openings at opposite ends of the replacement groove 3111 and the partition groove 3121.

[0030] Both the fixed packing 311 and the deflecting packing 312 are arranged in an arc shape to facilitate the adjustment of the displacement gap. The fixed packing 311 cooperates with the displacement grooves 3111 on both sides and the partition grooves 3121 of the deflecting packing 312. When the deflecting packing 312 rotates, the partition groove 3121 on one side and the adjacent displacement groove 3111 are inserted into each other in an alternating manner, creating a gap between the walls. The displacement groove 3111 at this point is the first displacement stroke, and the other side is the second displacement stroke. The displacement gap at this time includes the part of the displacement groove 3111 and the partition groove 3121 that cooperate, as well as the remaining length of the displacement groove 3111 and the partition groove 3121. As the insertion depth increases, the displacement gap becomes smaller and smaller, and the filtration effect on the gas phase and the recovery efficiency of the liquid phase become better and better.

[0031] Furthermore, the separation component 31 also includes a plurality of replacement plates 313, the lower ends of which are arranged at an angle and the replacement plates 313 are arranged in an arc shape; A number of compensation grooves 3122 are provided on one side of the deflection packing 312, and the compensation grooves 3122 are arranged vertically. The partition 32 is arranged in a ring shape, and the inner side of the partition 32 is provided with a rib 314. The axis of the supplementary plate 313 and the axis of the partition groove 3121 are collinear. The lower end of the supplementary plate 313 is inclined and abuts against the rib 314. The supplementary plate 313 and the compensation groove 3122 are slidably connected.

[0032] On the other side, a compensation groove 3122 is provided on the outside of the partition groove 3121. The compensation groove 3122 and the replacement plate 313 slide. When the deflection packing 312 rotates, it is guided by the rib plate 314 installed on the partition plate 32. The replacement plate 313 slides upward in the compensation groove 3122 and gradually inserts into the second replacement stroke. During the upward sliding process, the gap between the replacement plate 313 and the replacement groove 3111 located in the second replacement stroke decreases.

[0033] Furthermore, the deflection assembly 33 includes a deflection motor 335; The deflecting packing 312 has a toothed groove 3123 on its outer side; The partition 32 is provided with a deflection groove 322; The deflection motor 335 is placed in the deflection slot 322. The output end of the deflection motor 335 is equipped with a gear, and the deflection motor 335 meshes with the gear and the tooth slot 3123.

[0034] The partition 32 is used to install the deflection motor 335 through the deflection groove 322. The deflection motor 335 is used to output torque to drive the deflection packing 312 to rotate. The torque is transmitted by the meshing of gears and tooth grooves 3123. The corresponding components can be made of acid corrosion resistant materials or coated with corrosion resistant coatings.

[0035] Furthermore, the deflection assembly 33 also includes a sensing plate 331 and a trigger coil 334. The sensing plate 331 has a trigger rod 333 inside, and the trigger rod 333 is made of magnetic material. A sensing cavity 321 is provided on the inner side of the upper end of the partition 32; An elastic element 332 is provided inside the sensing cavity 321. The side of the elastic element 332 away from the wall of the sensing cavity 321 abuts against the trigger rod 333. One end of the trigger rod 333 is inserted into the trigger coil 334, and the trigger coil 334 is placed inside the sensing cavity 321.

[0036] The trigger coil 334 is installed in the induction cavity 321, which also guides the induction plate 331. The induction cavity 321 is located above the packing material; before the liquid phase enters the packing, it contacts the induction plate 331. The greater the instantaneous liquid flow rate, the greater the pressure generated. This pressure pushes the induction plate 331 to slide along the induction cavity 321, causing the magnetic trigger rod 333 to slide. This causes the trigger coil 334 to cut magnetic field lines and generate an induced current. The greater the liquid flow rate, the greater the current generated. A spring-like structure, such as an elastic element 332, is used for pre-tensioning. When the induction plate 331 moves, it compresses the elastic element 332. When the external liquid pressure decreases, the elastic element 332 pushes the induction plate 331 to move in the opposite direction, facilitating automatic adjustment based on instantaneous flow fluctuations.

[0037] Furthermore, the trigger coil 334 and the deflection motor 335 are electrically connected; When the liquid phase increases: the overlapping area of ​​the displacement tank 3111 and the partition tank 3121 increases, and the length of the insertion of the filling plate 313 into the partition tank 3121 near the side of the compensation tank 3122 increases.

[0038] When the liquid phase increases, the amount of sulfuric acid present in the liquid phase also increases. However, the increased flow rate can affect the replacement efficiency. The current generated on the trigger coil 334 is used as a control signal to control the current input to the deflection motor 335. That is, when the liquid phase increases, the deflection motor 335 drives the deflection packing 312 to rotate, inserting it into the replacement groove 3111 near the first replacement stroke for horizontal adjustment. The supplementary plate 313 moves upward, inserting itself into the replacement groove 3111 of the second replacement stroke for vertical adjustment. By adjusting the replacement gap in both strokes, the replacement gap is reduced, the contact area is increased, and the liquid phase flow resistance is increased, extending the replacement time and ensuring replacement efficiency.

[0039] As an optimization, the extraction device 2 includes a condenser 21, and a collection tank 22 is provided at the lower end of the condenser 21; The collection trough 22 is placed inside the working chamber 13, and one side of the collection trough 22 is connected to the extraction outlet 12.

[0040] By setting up a condenser 21, sulfuric acid vapor is condensed at the extraction point and collected through the collection tank 22 at the bottom. By setting up an extraction outlet 12, high-purity finished sulfuric acid is exported to meet the hard requirements of semiconductor grade.

[0041] As an optimization, a feed inlet 11 is provided on one side of the tower body 1, and a distributor 5 is provided at the upper end of the working chamber 13. The return channel 14 and the distributor 5 are connected by a pipe.

[0042] By setting up inlet 11, automatic liquid feeding is achieved. During the downward flow of the liquid, preliminary displacement and preheating occur, improving subsequent evaporation efficiency. By setting up distributor 5, the reflux liquid is evenly distributed, improving the distillation and purification efficiency.

[0043] A method for distilling sulfuric acid for semiconductor electronic grade, the distillation method comprising the following steps: Step 1: Supply raw material liquid, allowing it to flow downwards from the lower part of the working chamber 13, and distribute the return liquid evenly through the distributor 5; Step 2: After preliminary replacement and preheating, the raw material liquid enters heater 4, where it is heated and vaporized before entering the working chamber. Step 3: During the reflux liquid descent and the gas phase rise, component replacement occurs to purify the sulfuric acid. The replacement gap between the fixed packing 311 and the deflecting packing 312 is automatically adjusted according to the reflux liquid volume to prevent incomplete component replacement when the instantaneous liquid phase increases.

[0044] Step 4: The purified sulfuric acid is condensed near the outlet 12 by the condenser 21 and collected by the collection tank 22. The generated electronic-grade sulfuric acid is then discharged from the outlet 12.

[0045] The working principle of this invention: Both the fixed packing 311 and the deflecting packing 312 adopt a comb-shaped design. During the rotation of the deflecting packing 312 driven by the deflecting component 33, they can be interlocked. The fixed packing 311 and the deflecting packing 312 can be two semi-cylinders. When there is a large amount of downward flowing liquid phase, there is also a large amount of excess sulfuric acid in the liquid phase. Driven by the deflecting component 33 on the partition plate 32, the deflecting packing 312 rotates, and a part of the deflecting packing 312 inserts into the fixed packing, thereby reducing the displacement gap between the fixed packing 311 and the deflecting packing 312. This reduces the instantaneous flow cross section, thereby reducing the flow velocity. At the same time, it increases the contact area and improves the displacement efficiency. When the deflecting packing 312 rotates, the partition groove 3121 on one side and the adjacent displacement groove 3111 are interlocked, creating a gap between the walls. The displacement groove 3111 at this point is the first displacement stroke, and the other side is the second displacement stroke. The displacement gap at this time includes the part where the displacement groove 3111 and the partition groove 3121 cooperate, as well as the displacement groove 3111. As the insertion depth increases, the remaining length of the partition groove 3121 decreases, resulting in a smaller displacement gap and improved filtration efficiency for the gas phase and recovery efficiency for the liquid phase. When the deflecting packing 312 rotates, it is guided by the ribs 314 mounted on the partition plate 32. The supplementary plate 313 slides upward within the compensation groove 3122 and gradually inserts into the second displacement stroke. During the upward sliding process, the gap between the supplementary plate 313 and the displacement groove 3111 located in the second displacement stroke decreases. The sensing chamber 321 is located on the upper side of the packing. Before the liquid phase enters the packing, it will first contact the sensing plate 331. The greater the instantaneous liquid flow, the greater the pressure generated. The pressure pushes the sensing plate 331 to slide along the sensing chamber 321, causing the magnetic trigger rod 333 to slide, which in turn causes the trigger coil 334 to cut magnetic lines of force and generate an induced current. The greater the liquid flow, the greater the current generated. When the external liquid pressure decreases, the elastic element 332 pushes the sensing plate 331 to move in the opposite direction, facilitating automatic adjustment based on instantaneous flow fluctuations.

[0046] 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. A distillation column for semiconductor electronic-grade sulfuric acid, characterized in that: The sulfuric acid distillation column includes a column body (1), a collection device (2), a regulating device (3), and a heater (4), wherein the heater (4) and the column body (1) are connected by a pipeline; The tower body (1) is provided with a working chamber (13), and a number of adjusting devices (3) are provided in the working chamber (13). A mining outlet (12) is provided on one side of the working chamber (13), and the mining device (2) and the mining outlet (12) are connected by pipes. The adjustment device (3) includes a separation component (31), a partition (32) and a deflection component (33). The separation component (31) and the partition (32) are connected, and the deflection component (33) and the partition (32) are connected. The deflection component (33) is used to drive the separation component (31) to rotate. The separation assembly (31) includes a fixed packing (311) and a deflecting packing (312), wherein the axis of the fixed packing (311) and the axis of the deflecting packing (312) are collinear; The partition (32) is placed inside the working chamber (13). A fixed packing (311) is fitted on the partition (32). The partition (32) and the deflection packing (312) are rotatably connected. The deflection assembly (33) is connected to the deflection packing (312). The deflection assembly (33) adjusts the displacement gap between the fixed packing (311) and the deflection packing (312).

2. The semiconductor electronic-grade sulfuric acid distillation column according to claim 1, characterized in that: The fixed packing (311) is arc-shaped, and a plurality of replacement grooves (3111) are provided on both sides of the fixed packing (311), and the axes of the plurality of replacement grooves (3111) are arranged collinearly. The deflecting packing (312) has several partition grooves (3121) on both sides. A return channel (14) is provided on one side of the working chamber (13); The axis of the replacement groove (3111) and the axis of the partition groove (3121) are collinear, the replacement groove (3111) and the partition groove (3121) are staggered, and the replacement groove (3111) and the partition groove (3121) have openings at opposite ends.

3. A sulfuric acid distillation column for semiconductor electronic grade according to claim 2, characterized in that: The separation component (31) also includes a plurality of replacement plates (313), the lower ends of the plurality of replacement plates (313) are arranged at an angle, and the replacement plates (313) are arranged in an arc shape; The deflecting packing (312) has a plurality of compensation grooves (3122) on one side, and the compensation grooves (3122) are arranged vertically; The partition (32) is arranged in a ring shape, and a rib (314) is provided on the inner side of the partition (32). The axis of the supplement plate (313) and the axis of the partition groove (3121) are collinear. The lower end inclined surface of the supplement plate (313) abuts against the rib (314). The supplement plate (313) and the compensation groove (3122) are slidably connected.

4. A sulfuric acid distillation column for semiconductor electronic grade according to claim 3, characterized in that: The deflection assembly (33) includes a deflection motor (335); The deflecting packing (312) has a toothed groove (3123) on its outer side; The partition (32) is provided with a deflection groove (322); The deflection motor (335) is placed in the deflection slot (322), and the output end of the deflection motor (335) is provided with a gear. The deflection motor (335) meshes with the gear and the tooth groove (3123).

5. A sulfuric acid distillation column for semiconductor electronic grade according to claim 4, characterized in that: The deflection assembly (33) also includes a sensing plate (331) and a trigger coil (334). The sensing plate (331) has a trigger rod (333) inside, and the trigger rod (333) is made of magnetic material. The upper inner side of the partition (32) is provided with a sensing cavity (321); The sensing cavity (321) is provided with an elastic element (332). The side of the elastic element (332) away from the wall of the sensing cavity (321) abuts against the trigger rod (333). One end of the trigger rod (333) is inserted into the trigger coil (334), and the trigger coil (334) is placed in the sensing cavity (321).

6. A sulfuric acid distillation column for semiconductor electronic grade according to claim 5, characterized in that: The trigger coil (334) and the deflection motor (335) are electrically connected; When the liquid phase increases: the overlapping area of ​​the displacement tank (3111) and the partition tank (3121) increases, and the length of the insertion of the filling plate (313) into the partition tank (3121) near the side of the compensation tank (3122) increases.

7. A distillation column for semiconductor electronic-grade sulfuric acid according to any one of claims 1 to 6, characterized in that: The extraction device (2) includes a condenser (21), and a collection tank (22) is provided at the lower end of the condenser (21). The collection trough (22) is placed inside the working chamber (13), and one side of the collection trough (22) is connected to the extraction outlet (12).

8. A sulfuric acid distillation column for semiconductor electronic grade according to claim 2, characterized in that: The tower body (1) has a feed inlet (11) on one side, and a distributor (5) is provided at the upper end of the working chamber (13). The return channel (14) and the distributor (5) are connected by pipes.

9. A distillation method for a semiconductor electronic-grade sulfuric acid distillation column according to claim 8, characterized in that: The distillation method includes the following steps: Step 1: Automatic feeding, distributor (5) distributes the return liquid; Step 2: Heat the liquid material through heater (4) and send the evaporated gas into the working chamber (13); Step 3: The reflux liquid descends and the evaporated gas rises, and displacement purification is carried out. The displacement gap between the fixed packing (311) and the deflecting packing (312) is adjusted according to the liquid phase flow rate. Step 4: After condensation by condenser (21), the condenser collects the condenser through collection tank (22).

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