A preparation device and preparation method for preparing electronic grade nitric acid from raw materials

By designing homogenizing, scraping and fanning devices in the electronic-grade nitric acid preparation device, the problems of uneven temperature distribution of nitric acid and low evaporation purification rate are solved, uniform heating and efficient condensation of the nitric acid solution are achieved, and the preparation efficiency of electronic-grade nitric acid is improved.

CN118987661BActive Publication Date: 2025-04-04XIAN JI-LI ELECTRONIC & CHEM ENG CO LTD
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Patent Information

Application Number
CN202411488769.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-24
Publication Date
2025-04-04
Estimated Expiration
2044-10-24

AI Technical Summary

Technical Problem

During the heating and evaporation process of existing electronic grade nitric acid preparation devices, the heat transfer efficiency is poor, resulting in uneven temperature distribution of nitric acid, affecting the evaporation and purification rate of nitric acid.

Method used

A preparation device including a heat homogenization device, a scraper device and a fan device is designed. Through the combination of agitating blade rod, rotary ring, spiral blade and heating device, uniform heating and stirring of the nitric acid solution is achieved; by condensing the condensation device, scraper device and diversion inclined plate in the filter box, the condensation efficiency of nitric acid steam is improved; by promoting heat transfer through the fan device, it is improved to improve the heating efficiency of nitric acid solution.

Benefits of technology

Through the setting of the heat homogenization device, the temperature distribution of the nitric acid solution is ensured to be evenly distributed and the formation rate of nitric acid steam is improved; through the design of the scraping device and the inclined plate, the condensation efficiency of nitric acid steam is improved; through the use of the fan device, the efficiency and stability of the heating of the nitric acid solution are improved, and the preparation efficiency of electronic grade nitric acid is improved overall.

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Abstract

The present invention discloses a preparation device and a preparation method for preparing electronic-grade nitric acid from raw materials, and relates to the technical field of electronic-grade nitric acid preparation. The present invention includes a preparation device body, the top of the preparation device body is fixedly installed with an upper cover by bolts, the bottom of the upper cover is rotatably installed with a stirring blade rod, and the stirring blade rod is driven by a motor, a heating device is provided at the edge of the inner wall of the preparation device body, one side of the preparation device body is connected to a condensation filter box by a U-shaped tube, and a condensation device is provided above the inner wall of the condensation filter box. The present invention is provided with a heat equalization device, so that the stirring blade rod, the rotating ring, the spiral blade, the preparation device body, and the heating device cooperate to drive the spiral blade to stir the nitric acid solution and transport it to the inside of the filter cylinder, and the stirring action of the spiral blade can effectively stir the heated nitric acid solution evenly, ensure the uniform temperature distribution of the nitric acid solution, and then help the purification operation of nitric acid.
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Description

Technical Field

[0001] The invention relates to the technical field of electronic-grade nitric acid preparation, in particular to a preparation device and a preparation method for preparing electronic-grade nitric acid from raw materials. Background Art

[0002] The electronic-grade nitric acid production unit produces high-purity nitric acid, primarily for use in semiconductor manufacturing within the electronics industry. Through precise chemical reactions and purification processes, the unit removes impurities from industrial-grade nitric acid, ensuring the ultra-high purity and stability of the final product, meeting the extremely high demands placed on chemical raw materials in semiconductor manufacturing.

[0003] Patent publication number CN220714824U discloses an electronic-grade nitric acid purification device. An evaporator is fixed at the center of a heating base. A liquid inlet is provided on one side of the top of the evaporator. The steam outlet at the top of the evaporator is connected to one end of a condenser via a steam supply pipe. The other end of the condenser is connected to a collection tank via a liquid outlet pipe. A heating coil is mounted on the inner wall of the evaporator. One end of the heating coil is connected to a liquid supply pump at the bottom of the evaporator via a connecting pipe. A liquid return pipe is mounted on the other end of the heating coil. An electric heating assembly is installed within the heating base. A control panel is mounted on the outer wall of the heating base, electrically connecting the electric heating assembly and the liquid supply pump. This patent utilizes water bath heating to simultaneously heat the outer wall and interior of the evaporator, achieving uniform heating of the nitric acid. This prevents the production of excessive nitrogen oxides during the purification process and improves the quality of electronic-grade nitric acid purification.

[0004] However, the current electronic-grade nitric acid preparation device has the following problems: when the electronic-grade nitric acid preparation device heats and evaporates the nitric acid, the heat transfer efficiency inside the concentration kettle is poor due to the nitric acid stirring method alone, resulting in uneven temperature distribution of the nitric acid during the evaporation process, which in turn affects the evaporation and purification rate of the nitric acid. Therefore, we propose a preparation device and preparation method for preparing electronic-grade nitric acid from raw materials. Summary of the Invention

[0005] In view of the deficiencies in the prior art, the present invention provides a device and method for preparing electronic-grade nitric acid from raw materials, which solves the problems raised in the above-mentioned background technology.

[0006] To achieve the above purpose, the present invention is implemented through the following technical solutions: a preparation device for preparing electronic grade nitric acid from raw materials, including a preparation device body, an upper cover is fixedly installed on the top of the preparation device body by bolts, a stirring blade is rotatably installed on the bottom of the upper cover, and the stirring blade is driven by a motor, a heating device is provided at the edge of the inner wall of the preparation device body, one side of the preparation device body is connected to a condensation filter box through a U-shaped tube, a condensation device is provided above the inner wall of the condensation filter box, a water collection through-hole plate is fixed to the middle of the inner wall of the condensation filter box, a filter cartridge is fixed to the bottom of the inner wall of the condensation filter box, and the condensation filter is provided at the bottom of the inner wall of the condensation filter box. A drain pipe is fixed to one side of the box, and a heat equalizing device is provided inside the main body of the preparation device. The heat equalizing device includes a drum rack, which is fixedly installed on the bottom of the inner wall of the main body of the preparation device through a bracket. A rotating ring is fixed on the outer wall above the blades of the stirring blade rod, and the rotating ring is rotatably installed on the top of the drum rack. A spiral blade is fixed to the outside of the rotating ring, and the spiral blade is sleeved on the outside of the drum rack. When the stirring blade rod rotates, the blades of the stirring blade rod will drive the rotating ring to rotate, and the rotating ring will drive the spiral blade to rotate. The spiral blade stirs and lifts the nitric acid heated by the heating device at the edge of the main body of the preparation device upward, so that the nitric acid solution is stirred and transported to the inside of the drum rack by the spiral blade.

[0007] According to the above technical solution, a cavity is provided at the top of the rotating ring, and an opening is provided at the inner wall of the rotating ring. Several L-shaped connecting frames are fixed at the inner wall of the preparation device body, and two of the several L-shaped connecting frames form a group. A guide ramp is fixed on the side of the two L-shaped connecting frames away from the inner wall of the preparation device body, and the guide ramp is located on the inner side of the rotating ring. At the same time, part of the nitric acid stirred upward by the spiral blade will fall into the cavity of the rotating ring. When the opening of the rotating ring rotates to the position of the guide ramp, the nitric acid in the cavity of the rotating ring will flow into the guide ramp through the opening of the rotating ring, and the nitric acid flows downward along the guide ramp.

[0008] According to the above technical solution, a scraping device is provided above the interior of the condensation filter box, and the scraping device includes a double-sided elliptical groove ring and an L-shaped column rod. The double-sided elliptical groove ring is fixed to the outside of the stirring blade rod through a bracket, and the L-shaped column rod is horizontally penetrated and slidably installed on the inner wall of one side of the condensation filter box close to the preparation device body, and the L-shaped column rod penetrates the outer wall of the preparation device body, and one end of the L-shaped column rod is slidably installed in the elliptical groove above the double-sided elliptical groove ring. A plurality of L-shaped rods are fixed on the top of the L-shaped column rod. A plurality of through-groove scrapers are fixed at the bottom, and the through-groove scrapers are in contact with the outer wall of the condensing tube of the condensing device. The outer walls of the preparation device body and the condensing filter box are fixed with sealing rings for preventing nitric acid vapor from leaking from the through-hole of the L-shaped column. When the stirring blade rotates, the double-sided elliptical groove ring is driven to rotate, and the elliptical groove of the double-sided elliptical groove ring drives the L-shaped column to move back and forth. The L-shaped column drives the through-groove scrapers to move back and forth along the outer wall of the condensing tube of the condensing device through the four-shaped rod. The through-groove scrapers scrape off the liquid nitric acid formed on the outer wall of the condensing tube of the condensing device.

[0009] According to the above technical solution, the scraping device also includes a number of telescopic slides and a number of slow flow plates. The slow flow plates are evenly and equidistantly slidably installed inside the guide inclined plate. One end of the telescopic slides is respectively fixed on the top of the several slow flow plates. The other ends of the telescopic slides are all slidably installed inside the elliptical groove below the double-sided elliptical groove ring. At the same time, when the double-sided elliptical groove ring is rotating, the elliptical groove of the double-sided elliptical groove ring pushes the telescopic slide to drive the slow flow plate to move back and forth along the inside of the guide inclined plate. The movement of the slow flow plate can actively push the nitric acid flowing through the guide inclined plate.

[0010] According to the above technical solution, a plurality of elastic telescopic rods are fixed to the bottom of the shaped rod, and the telescopic end of the elastic telescopic rod is arranged toward the condensing tube of the condensing device, a pressure plate is fixed to the telescopic end of the elastic telescopic rod, a Teflon cloth plate is fixed to the side of the pressure plate away from the elastic telescopic rod, a through groove for accommodating the Teflon cloth plate is opened on the outer wall of the through groove scraper, a plurality of protrusion plates are fixed laterally to the inner wall of the condensation filter box, a semi-arc block is fixed to the side of the protrusion plate close to the condensing tube of the condensing device, and a semi-arc block is fixed to the bottom of the pressure plate away from the condensing tube of the condensing device Arc block, the semi-arc block of the protruding plate is located on the semi-arc block movement trajectory of the pressing plate, and at the same time, the polygonal rod drives the pressing plate and the Teflon cloth plate to move through the elastic telescopic rod. When the Teflon cloth plate moves, it will absorb the liquid nitric acid remaining on the outer wall of the condensing tube of the condensing device, thereby further reducing the residual amount of liquid nitric acid on the outer wall of the condensing tube of the condensing device. When the semi-arc block of the pressing plate moves to the semi-arc block position of the protruding plate, the semi-arc block of the protruding plate pushes the semi-arc block of the pressing plate to drive the pressing plate toward the Teflon cloth plate, and the pressing plate squeezes the Teflon cloth plate, and the liquid nitric acid adsorbed by the Teflon cloth plate is squeezed out of the Teflon cloth plate.

[0011] According to the above technical solution, a fanning device is provided above the interior of the preparation device body, and the fanning device includes a gear ring, which is fixed to the upper outer wall of the stirring blade rod through a bracket, and a number of fanning blades are evenly and equidistantly fixed on the inner wall of the gear ring. When the stirring blade rod rotates, the gear ring will be driven to rotate, and the gear ring will drive the fanning blades to rotate, and the fanning blades will fan the air above the interior of the preparation device body.

[0012] According to the above technical solution, the fanning device also includes an arc-shaped cover, which is fixed at the bottom of the upper cover and is located at the U-shaped tube. An L-shaped frame is fixed at the bottom edge of the arc-shaped cover, and a gear is rotatably installed on the top of the L-shaped frame, and the gear is engaged with a gear ring. A suction fan is fixed on the top of the gear, and at the same time, the gear ring drives the gear to rotate, and the gear drives the suction fan to rotate. The suction fan attracts the nitric acid vapor in the preparation device body through the arc-shaped cover into the U-shaped tube.

[0013] A preparation device for preparing electronic grade nitric acid from raw materials comprises the following steps:

[0014] S1. Add nitric acid solution into the preparation device body through the feed port of the upper cover;

[0015] S2, driving a stirring blade by a motor to stir the nitric acid in the preparation device body, and starting a heating device to heat the nitric acid in the preparation device body, so that the nitric acid is heated to form nitric acid vapor and is transmitted to the condensation filter box through a U-shaped tube;

[0016] S3. Start the condensing device, which condenses the nitric acid vapor into liquid and drops it onto the water collection hole plate;

[0017] S4, the water collection plate collects the liquefied nitric acid vapor and drips it into the filter cartridge. The nitric acid liquid then passes through the filter cartridge to filter out the larger particles inside and is purified.

[0018] S5. Then it is discharged through the drain pipe, completing the preparation of electronic grade nitric acid.

[0019] The present invention provides a device and method for preparing electronic-grade nitric acid from raw materials. The device and method have the following beneficial effects:

[0020] (1) The present invention provides a heat equalizing device, so that the stirring blade rod, the rotating ring, the spiral blade, the preparation device body, and the heating device cooperate to drive the spiral blade to stir the nitric acid solution and transport it to the inner side of the filter cylinder. The stirring action of the spiral blade can effectively stir the heated nitric acid solution evenly, ensuring that the temperature distribution of the nitric acid solution is uniform, thereby facilitating the formation of nitric acid vapor and further facilitating the purification operation of nitric acid; at the same time, when the opening of the rotating ring rotates to the position of the guide ramp, the nitric acid in the cavity of the rotating ring will flow into the guide ramp through the opening of the rotating ring, and the nitric acid will flow downward along the guide ramp. The guide ramp increases the evaporation area of ​​the nitric acid solution, thereby accelerating the formation of nitric acid vapor.

[0021] (2) The present invention sets a scraping device so that the stirring blade rod, the double-sided elliptical groove ring, the L-shaped column rod, and the polygonal rod cooperate to drive the through-groove scraper to scrape off the liquid nitric acid formed on the outer wall of the condensing tube of the condensing device, thereby effectively improving the condensation efficiency of the nitric acid vapor; at the same time, the polygonal rod, the elastic telescopic rod, and the pressure plate cooperate to drive the Teflon cloth plate to move and absorb the liquid nitric acid remaining on the outer wall of the condensing tube of the condensing device, thereby further reducing the residual amount of liquid nitric acid on the outer wall of the condensing tube of the condensing device; at the same time, the convex plate and the pressure plate cooperate to drive the liquid nitric acid absorbed by the Teflon cloth plate to be squeezed out of the Teflon cloth plate, thereby allowing the Teflon cloth plate to continuously absorb the liquid nitric acid remaining on the outer wall of the condensing tube of the condensing device; at the same time, the double-sided elliptical groove ring and the telescopic sliding column cooperate to drive the slow flow plate to slow down the flow rate of nitric acid when it flows through the guide inclined plate, thereby increasing the residence time of nitric acid on the guide inclined plate. The increase in residence time helps to increase the volatilization amount of nitric acid.

[0022] (3) The present invention sets a fanning device so that the stirring blade rod and the gear ring cooperate to drive the fan blade to fan the air above the interior of the preparation device body. Fanning the air can help promote heat transfer. During the heating process of the nitric acid solution, the nitric acid vapor will take away a large amount of heat, and the fanning air can distribute the heat more evenly throughout the interior of the preparation device body, which helps to improve the efficiency and stability of the nitric acid solution heating; at the same time, the gear ring and the gear cooperate to drive the suction fan to attract the nitric acid vapor in the preparation device body through the arc cover into the U-shaped tube, thereby improving the efficiency of the U-shaped tube in transmitting the nitric acid vapor, and further improving the preparation efficiency of electronic grade nitric acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 A schematic diagram of the present invention as a whole;

[0024] Figure 2 It is a partial cross-sectional schematic diagram of the present invention;

[0025] Figure 3 Schematic diagram of the heat equalizing device of the present invention Figure 1 ;

[0026] Figure 4Schematic diagram of the heat equalizing device of the present invention Figure 2 ;

[0027] Figure 5 is a schematic diagram of a wiper device according to the present invention;

[0028] Figure 6 It is a bottom view schematic diagram of a partial structure of the liquid scraping device of the present invention;

[0029] Figure 7 For the present invention Figure 6 Schematic diagram of the enlarged structure at A;

[0030] Figure 8 is a schematic diagram of a fanning device of the present invention;

[0031] Figure 9 For the present invention Figure 8 Schematic diagram of the enlarged structure at B;

[0032] Figure 10 The double-sided elliptical groove ring of the present invention is schematically shown. Figure 1 ;

[0033] Figure 11 The double-sided elliptical groove ring of the present invention is schematically shown. Figure 2 .

[0034] In the figure: 1. Preparation device body; 11. Upper cover; 12. Stirring blade rod; 13. Heating device; 2. Condensation filter box; 21. U-shaped tube; 22. Condensation device; 23. Drain pipe; 24. Water collecting hole plate; 25. Filter cartridge; 3. Heat equalization device; 31. Cartridge rack; 32. Spiral blade; 33. Rotating ring; 34. Guide ramp; 35. L-shaped connecting frame; 4. Scraping device; 41. Double-sided elliptical groove ring; 42. L-shaped column; 43. Ji-shaped rod; 44. Through-groove scraper; 45. Elastic telescopic rod; 46. Pressing plate; 47. Teflon cloth plate; 48. Bump plate; 49. Telescopic sliding column; 410. Slow flow plate; 5. Fanning device; 51. Gear ring; 52. Fan blade; 53. Arc cover; 54. Gear; 55. L-shaped frame; 56. Suction fan. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0036] See also Figure 1-11One embodiment of the present invention is: a preparation device for preparing electronic grade nitric acid from raw materials, comprising a preparation device body 1, an upper cover 11 is fixedly installed on the top of the preparation device body 1 by bolts, a stirring blade rod 12 is rotatably installed on the bottom of the upper cover 11, and the stirring blade rod 12 is driven by a motor, a heating device 13 is provided at the edge of the inner wall of the preparation device body 1, one side of the preparation device body 1 is connected to a condensation filter box 2 through a U-shaped tube 21, a condensation device 22 is provided above the inner wall of the condensation filter box 2, a water collection through-hole plate 24 is fixed to the middle of the inner wall of the condensation filter box 2, a filter cartridge 25 is fixed to the bottom of the inner wall of the condensation filter box 2, and a drain pipe 23 is fixed to one side of the condensation filter box 2. A heat equalizing device 3 is provided inside the device body 1, and the heat equalizing device 3 includes a drum rack 31, which is fixedly mounted on the bottom of the inner wall of the preparation device body 1 through a bracket, and a rotating ring 33 is fixed on the outer wall above the blades of the stirring blade rod 12, and the rotating ring 33 is rotatably mounted on the top of the drum rack 31, and a spiral blade 32 is fixed on the outside of the rotating ring 33, and the spiral blade 32 is sleeved on the outside of the drum rack 31. Through the arrangement of the above structure, the nitric acid solution is stirred and transported to the inside of the drum rack 31 by the spiral blade 32. The stirring action of the spiral blade 32 can effectively stir the heated nitric acid solution evenly, ensure that the temperature distribution of the nitric acid solution is uniform, thereby facilitating the formation of nitric acid vapor, and further facilitating the purification operation of nitric acid.

[0037] A cavity is provided at the top of the rotating ring 33, and an opening is provided at the inner wall of the rotating ring 33. Several L-shaped connecting frames 35 are fixed to the inner wall of the preparation device body 1. Two of the several L-shaped connecting frames 35 form a group. A guide ramp 34 is fixed on the side of the two L-shaped connecting frames 35 away from the inner wall of the preparation device body 1, and the guide ramp 34 is located on the inner side of the rotating ring 33. Through the arrangement of the above structure, the nitric acid in the cavity of the rotating ring 33 will flow downward along the guide ramp 34. The guide ramp 34 increases the evaporation area of ​​the nitric acid solution, thereby accelerating the formation of nitric acid vapor.

[0038] A scraping device 4 is provided above the interior of the condensation filter box 2. The scraping device 4 comprises a double-sided elliptical groove ring 41 and an L-shaped column 42. The double-sided elliptical groove ring 41 is fixed to the outside of the stirring blade rod 12 (such as Figure 5 As shown), and the double-sided elliptical groove ring 41 is horizontally arranged (as shown Figure 11As shown), the L-shaped column rod 42 is horizontally penetrated and slidably installed on the inner wall of the side of the condensation filter box 2 close to the preparation device body 1, and the L-shaped column rod 42 penetrates the outer wall of the preparation device body 1, and one end of the L-shaped column rod 42 is slidably installed in the upper elliptical groove of the double-sided elliptical groove ring 41, and a plurality of polygonal rods 43 are fixed on the top of the L-shaped column rod 42, and a plurality of through-groove scrapers 44 are fixed on the bottom of the polygonal rod 43, and the through-groove scrapers 44 are in contact with the outer wall of the condensation tube of the condensation device 22. The outer walls of the preparation device body 1 and the condensation filter box 2 are fixed with sealing rings for preventing nitric acid vapor from leaking from the penetration port of the L-shaped column rod 42. Through the arrangement of the above structure, the through-groove scrapers 44 scrape off the liquid nitric acid formed on the outer wall of the condensation tube of the condensation device 22, thereby effectively improving the condensation efficiency of the nitric acid vapor.

[0039] A plurality of elastic telescopic rods 45 are fixed to the bottom of the polygonal rod 43, and the telescopic ends of the elastic telescopic rods 45 are arranged in the direction of the condensing tube of the condensing device 22. A pressing plate 46 is fixed to the telescopic end of the elastic telescopic rod 45, and a Teflon cloth plate 47 is fixed to the side of the pressing plate 46 away from the elastic telescopic rod 45. The Teflon cloth plate 47 (polytetrafluoroethylene cloth) has excellent chemical corrosion resistance, including tolerance to nitric acid. It can maintain stability in a strong acid environment and is not easily corroded by nitric acid. Therefore, it is very suitable for processing nitric acid. A through groove for accommodating the Teflon cloth plate 47 is provided on the outer wall of the through-groove scraper 44. A plurality of protrusion plates 48 are fixed laterally on the inner wall of the condensation filter box 2. The protrusion plate 48 is close to the condensing device A semi-arc block is fixed on one side of the condenser tube 22, and a semi-arc block is fixed on the side of the bottom of the pressure plate 46 away from the condenser tube of the condensing device 22. The semi-arc block of the protrusion plate 48 is located on the movement trajectory of the semi-arc block of the pressure plate 46. Through the setting of the above structure, the Teflon cloth plate 47 will adsorb the liquid nitric acid remaining on the outer wall of the condenser tube of the condensing device 22 when it moves, thereby further reducing the residual amount of liquid nitric acid on the outer wall of the condenser tube of the condensing device 22. At the same time, through the setting of the above structure, the pressure plate 46 squeezes the Teflon cloth plate 47, and the liquid nitric acid adsorbed by the Teflon cloth plate 47 is squeezed out of the Teflon cloth plate 47, so that the Teflon cloth plate 47 can sustainably adsorb the liquid nitric acid remaining on the outer wall of the condenser tube of the condensing device 22.

[0040] The scraping device 4 also includes a plurality of telescopic slides 49 and a plurality of slow flow plates 410. The plurality of slow flow plates 410 are evenly and equidistantly slidably installed inside the guide inclined plate 34. One end of the plurality of telescopic slides 49 is respectively fixed on the top of the plurality of slow flow plates 410, and the other ends of the plurality of telescopic slides 49 are all slidably installed inside the elliptical groove below the double-sided elliptical groove ring 41. Through the arrangement of the above structure, the slow flow plates 410 slow down the flow rate of nitric acid when flowing through the guide inclined plate 34, thereby increasing the residence time of nitric acid on the guide inclined plate 34. The increase in residence time helps to increase the volatilization amount of nitric acid.

[0041] During use, the nitric acid solution is put into the preparation device body 1 through the feed port of the upper cover 11, the stirring blade 12 is driven by the motor to stir the nitric acid in the preparation device body 1, and the heating device 13 is started to heat the nitric acid in the preparation device body 1. After the nitric acid is heated, nitric acid vapor is formed and transmitted to the condensation filter box 2 through the U-shaped tube 21, and the condensing device 22 is started. The condensing device 22 will condense and liquefy the nitric acid vapor and drip it onto the water collecting through-hole plate 24. The water collecting through-hole plate 24 collects the liquefied nitric acid vapor and drips it into the filter cylinder 25. Then the nitric acid liquid is purified after filtering the larger particles inside the filter cylinder 25, and then discharged through the drain pipe 23, completing the preparation operation of electronic grade nitric acid. When the stirring blade 12 rotates, the blades of the stirring blade 12 will drive the rotating ring 33 to rotate. The rotating ring 33 will drive the spiral blades 32 to rotate, and the spiral blades 32 will stir and lift the nitric acid heated by the heating device 13 at the edge of the preparation device body 1, so that the nitric acid solution is stirred and transported to the inner side of the drum rack 31 by the spiral blades 32. The stirring action of the spiral blades 32 can effectively stir the heated nitric acid solution evenly, ensure that the temperature distribution of the nitric acid solution is uniform, which is conducive to accelerating the formation of nitric acid vapor; at the same time, part of the nitric acid stirred and lifted upward by the spiral blades 32 will fall into the cavity of the rotating ring 33. When the opening of the rotating ring 33 rotates to the position of the guide ramp 34, the nitric acid in the cavity of the rotating ring 33 will flow into the guide ramp 34 through the opening of the rotating ring 33. The nitric acid flows downward along the guide ramp 34. The guide ramp 34 increases the evaporation area of ​​the nitric acid solution, thereby accelerating the formation of nitric acid vapor.

[0042] When the stirring blade rod 12 rotates, it drives the double-sided elliptical groove ring 41 to rotate, and the elliptical groove of the double-sided elliptical groove ring 41 drives the L-shaped column rod 42 to move back and forth horizontally left and right, and the L-shaped column rod 42 drives the through-groove scraper 44 to move back and forth horizontally left and right along the outer wall of the condensing tube of the condensing device 22 through the polygonal rod 43. The through-groove scraper 44 scrapes off the liquid nitric acid formed on the outer wall of the condensing tube of the condensing device 22, thereby effectively improving the condensation efficiency of the nitric acid vapor; at the same time, the polygonal rod 43 drives the pressing plate 46 and the Teflon cloth plate 47 to move along through the elastic telescopic rod 45, and the Teflon cloth plate 47 moves When the semi-arc block of the pressure plate 46 moves to the semi-arc block position of the protrusion plate 48, the semi-arc block of the protrusion plate 48 pushes the semi-arc block of the pressure plate 46 to drive the pressure plate 46 toward the Teflon cloth plate 47, and the pressure plate 46 squeezes the Teflon cloth plate 47. The liquid nitric acid adsorbed by the Teflon cloth plate 47 is squeezed out of the Teflon cloth plate 47, so that the Teflon cloth plate 47 can sustainably adsorb the liquid nitric acid remaining on the outer wall of the condenser tube of the condensing device 22.

[0043] At the same time, when the double-sided elliptical groove ring 41 is rotating, the elliptical groove of the double-sided elliptical groove ring 41 pushes the telescopic sliding column 49 to drive the slow flow plate 410 to move back and forth along the inside of the guide inclined plate 34. The movement of the slow flow plate 410 can actively push the nitric acid flowing through the guide inclined plate 34, so that the slow flow plate 410 slows down the flow rate of nitric acid when flowing through the guide inclined plate 34, thereby increasing the residence time of nitric acid on the guide inclined plate 34. The increase in residence time helps to increase the volatilization amount of nitric acid.

[0044] See also Figure 1-11 Based on the above embodiment, in another embodiment of the present invention, a fanning device 5 is provided above the interior of the preparation device body 1.

[0045] The fanning device 5 includes a gear ring 51, which is fixed to the upper outer wall of the stirring blade rod 12 through a bracket. A number of fanning blades 52 are evenly and equidistantly fixed on the inner wall of the gear ring 51. Through the setting of the above structure, the fanning blades 52 fan the air above the inside of the preparation device body 1. Fanning the air can help promote heat transfer. During the heating process of the nitric acid solution, nitric acid vapor will take away a large amount of heat, and fanning the air can distribute the heat more evenly throughout the entire preparation device body 1, which helps to improve the efficiency and stability of the heating of the nitric acid solution.

[0046] The fanning device 5 also includes an arc-shaped cover 53, which is fixed to the bottom of the upper cover 11 and is located at the U-shaped tube 21. An L-shaped frame 55 is fixed at the bottom edge of the arc-shaped cover 53. A gear 54 is rotatably installed on the top of the L-shaped frame 55, and the gear 54 is engaged with the gear ring 51. A suction fan 56 is fixed on the top of the gear 54. Through the arrangement of the above structure, the suction fan 56 attracts the nitric acid vapor in the preparation device body 1 through the arc-shaped cover 53 into the U-shaped tube 21, thereby improving the efficiency of the U-shaped tube 21 in transmitting nitric acid vapor, and further improving the preparation efficiency of electronic-grade nitric acid.

[0047] During use, when the stirring blade rod 12 rotates, it will drive the gear ring 51 to rotate, and the gear ring 51 will drive the fan blades 52 to rotate, and the fan blades 52 will fan the air above the inside of the preparation device body 1. Fanning the air can help promote heat transfer. During the heating process of the nitric acid solution, the nitric acid vapor will take away a large amount of heat, and fanning the air can distribute the heat more evenly throughout the entire preparation device body 1, which helps to improve the efficiency and stability of the nitric acid solution heating; at the same time, the gear ring 51 drives the gear 54 to rotate, and the gear 54 drives the suction fan 56 to rotate, and the suction fan 56 attracts the nitric acid vapor in the preparation device body 1 through the arc cover 53 into the U-shaped tube 21, thereby improving the efficiency of the U-shaped tube 21 in transmitting nitric acid vapor, and thereby improving the preparation efficiency of electronic-grade nitric acid.

[0048] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A preparation device for preparing electronic grade nitric acid from raw materials, comprising a preparation device body (1), an upper cover (11) being fixedly mounted on the top of the preparation device body (1) by bolts, a stirring blade rod (12) being rotatably mounted on the bottom of the upper cover (11), and the stirring blade rod (12) being driven by a motor, a heating device (13) being arranged at the edge of the inner wall of the preparation device body (1), one side of the preparation device body (1) being connected to a condensation filter box (2) by a U-shaped tube (21), a condensation device (22) being arranged above the inner wall of the condensation filter box (2), a water collecting through-hole plate (24) being fixed at the middle of the inner wall of the condensation filter box (2), a filter cartridge (25) being fixed at the bottom of the inner wall of the condensation filter box (2), and a liquid discharge pipe (23) being fixed at one side of the condensation filter box (2); Features: A heat equalizing device (3) is arranged inside the preparation device body (1), and the heat equalizing device (3) comprises a cartridge frame (31), the cartridge frame (31) is fixedly mounted on the bottom of the inner wall of the preparation device body (1) via a bracket, a rotating ring (33) is fixed on the outer wall above the blades of the stirring blade rod (12), and the rotating ring (33) is rotatably mounted on the top of the cartridge frame (31), and a spiral blade (32) is fixed on the outside of the rotating ring (33), and the spiral blade (32) is sleeved on the outside of the cartridge frame (31); A cavity is formed at the top of the rotating ring (33), and an opening is formed at the inner wall of the rotating ring (33). A plurality of L-shaped connecting frames (35) are fixed to the inner wall of the preparation device body (1), two of the plurality of L-shaped connecting frames (35) form a group, and a guide inclined plate (34) is fixed to the side of the two L-shaped connecting frames (35) away from the inner wall of the preparation device body (1), and the guide inclined plate (34) is located on the inner side of the rotating ring (33); A scraping device (4) is arranged above the interior of the condensation filter box (2), and the scraping device (4) comprises a double-sided elliptical groove ring (41) and an L-shaped column (42), wherein the double-sided elliptical groove ring (41) is fixed to the outside of the stirring blade rod (12) by a bracket, and the L-shaped column rod (42) transversely penetrates and is slidably installed on the inner wall of one side of the condensation filter box (2) close to the preparation device body (1), and the L-shaped column rod (42) penetrates the outer wall of the preparation device body (1), and one end of the L-shaped column rod (42) is slidably installed inside the elliptical groove above the double-sided elliptical groove ring (41), a plurality of L-shaped rods (43) are fixed to the top of the L-shaped column rod (42), and a plurality of through-groove scrapers (44) are fixed to the bottom of the L-shaped rod (43), and the through-groove scrapers (44) are in contact with the outer wall of the condensation tube of the condensation device (22); A plurality of elastic telescopic rods (45) are fixed to the bottom of the shaped rod (43), and the telescopic ends of the elastic telescopic rods (45) are arranged in the direction of the condensing tube of the condensing device (22), a pressing plate (46) is fixed to the telescopic end of the elastic telescopic rod (45), a Teflon cloth plate (47) is fixed to the side of the pressing plate (46) away from the elastic telescopic rod (45), a through groove for accommodating the Teflon cloth plate (47) is provided on the outer wall of the through groove scraper (44), a plurality of protrusion plates (48) are transversely fixed to the inner wall of the condensing filter box (2), a semi-arc block is fixed to the side of the protrusion plate (48) close to the condensing tube of the condensing device (22), a semi-arc block is fixed to the bottom of the pressing plate (46) away from the condensing tube of the condensing device (22), and the semi-arc block of the protrusion plate (48) is located on the movement track of the semi-arc block of the pressing plate (46); The liquid scraping device (4) further comprises a plurality of telescopic sliding columns (49) and a plurality of slow flow plates (410), wherein the plurality of slow flow plates (410) are evenly and equidistantly slidably mounted inside the guide inclined plate (34), one end of the plurality of telescopic sliding columns (49) is respectively fixed to the top of the plurality of slow flow plates (410), and the other ends of the plurality of telescopic sliding columns (49) are slidably mounted inside the lower elliptical groove of the double-sided elliptical groove ring (41).

2. A preparation device for preparing electronic grade nitric acid from raw materials according to claim 1, characterized in that: A sealing ring is fixed to the outer wall of the preparation device body (1) and the condensation filter box (2) to prevent nitric acid vapor from leaking from the through-hole of the L-shaped column rod (42).

3. A preparation device for preparing electronic grade nitric acid from raw materials according to claim 2, characterized in that: A fanning device (5) is arranged above the interior of the preparation device body (1), and the fanning device (5) comprises a toothed ring (51). The toothed ring (51) is fixed to the upper outer wall of the stirring blade rod (12) through a bracket, and a plurality of fanning blades (52) are evenly and equidistantly fixed to the inner wall of the toothed ring (51).

4. A preparation device for preparing electronic grade nitric acid from raw materials according to claim 3, characterized in that: The fanning device (5) further comprises an arc-shaped cover (53), wherein the arc-shaped cover (53) is fixed to the bottom of the upper cover (11), and the arc-shaped cover (53) is located at the U-shaped tube (21), an L-shaped frame (55) is fixed at the bottom edge of the arc-shaped cover (53), a gear (54) is rotatably mounted on the top of the L-shaped frame (55), and the gear (54) is meshed with the gear ring (51), and a suction fan (56) is fixed to the top of the gear (54).

5. A method for preparing electronic-grade nitric acid from raw materials, comprising a preparation device for preparing electronic-grade nitric acid from raw materials as claimed in any one of claims 1 to 4, characterized in that: The following steps are involved: S1, feeding nitric acid solution into the preparation device body (1) through the feed port of the upper cover (11); S2, driving the stirring blade (12) by a motor to stir the nitric acid in the preparation device body (1), and starting the heating device (13) to heat the nitric acid in the preparation device body (1), so that the nitric acid is heated to form nitric acid vapor and is transmitted to the condensation filter box (2) through the U-shaped tube (21); S3, starting the condensing device (22), the condensing device (22) condenses the nitric acid vapor into liquid and drips it onto the water collecting hole plate (24); S4, the water collecting hole plate (24) collects the liquefied nitric acid vapor and drips it into the filter cartridge (25), and then the nitric acid liquid passes through the filter cartridge (25) to filter out the larger particles inside and is purified; S5. Then the nitric acid is discharged through the drain pipe (23), thus completing the preparation of electronic grade nitric acid.

Citation Information

Patent Citations

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    CN220714824U

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