Electronic-grade ammonia water rectification device

Through the combination of a multi-stage distillation tower system and a heat exchanger, the problems of low ammonia water separation efficiency and high energy consumption in the prior art are solved, and efficient and energy-saving ammonia water separation is achieved, and ammonia water that meets the electronic grade purity is produced.

CN223184100UActive Publication Date: 2025-08-05ZHENJIANG RUNJING HIGH PURITY CHEM TECH CO LTD
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Patent Information

Application Number
CN202422423173.6
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-10-09
Publication Date
2025-08-05
Estimated Expiration
2034-10-09

AI Technical Summary

Technical Problem

The existing ammonia water purification technology in the production of electronic grade ammonia water has low separation efficiency, high energy consumption and insufficient automation, making it difficult to meet the requirements of high purity.

Method used

A multi-stage distillation tower system is adopted, combined with a reboiler, condenser and heat exchanger, and the tower plate is designed as a screen plate or a bubble point plate, a reflow tank and a regulating return valve are set up, and the heat exchanger is used to recover the condenser heat to achieve efficient ammonia and water separation.

Benefits of technology

It improves the separation efficiency and purity of ammonia water, reduces energy consumption, is suitable for large-scale industrial production, and meets the purity requirements of electronic grade ammonia water.

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Abstract

The utility model discloses an electronic grade ammonia water rectification device, which comprises a multistage rectification tower system, a reboiler and a condenser, the multistage rectification tower system comprises a plurality of rectification towers connected in series, a plurality of horizontally placed tower plates are arranged in the tower bodies of the rectification towers from top to bottom, downcomers vertical to the tower plates are arranged at the end parts of the tower plates, and the downcomers are connected with the reboiler. Uniformly distributed holes are formed in the tower plates, a feeding hole is formed in the tower plate in the middle of the first rectifying tower and is connected with a feeding pump, a gas outlet is formed in the tower top of each rectifying tower and is connected with a feeding hole of the next rectifying tower, a gas outlet of the last-stage rectifying tower is connected with a condenser, and the condenser is connected with a return tank; the outlet of the reflux tank is divided into two paths, one path is connected with the finished product tank, the other path is connected to the tower top of the last-stage rectifying tower, a liquid outlet is formed in the tower bottom of each stage of rectifying tower, all the liquid outlets are connected in parallel and connected with a reboiler, and a steam outlet of the reboiler is connected to the lowest layer of the first rectifying tower.
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Description

Technical Field

[0001] The utility model relates to an electronic-grade ammonia water distillation device. Background Art

[0002] Ammonia is a key industrial chemical used in a wide range of applications, including fertilizer production, chemical cleaning, pharmaceuticals, and electronics manufacturing. Within electronics manufacturing, ammonia is used in etching, cleaning, and other precision machining processes. In particular, the manufacture of semiconductors, liquid crystal displays, and solar cells requires extremely high ammonia purity, necessitating the production of electronic-grade ammonia. Electronic-grade ammonia typically requires very low levels of metallic impurities and trace contaminants to ensure that no harmful impurities are introduced during the cleaning and etching of semiconductor wafers.

[0003] Existing ammonia refining technologies mainly rely on traditional physical separation technologies such as distillation, absorption and distillation. However, faced with the high purity requirements of electronic-grade ammonia, these traditional processes have certain limitations in actual operation, such as limited separation efficiency, high energy consumption, low degree of automation and limited product purity. Utility Model Content

[0004] The purpose of the utility model is to solve the deficiencies of the above-mentioned prior art and to provide an efficient and energy-saving electronic-grade ammonia distillation device.

[0005] An electronic grade ammonia distillation device comprises a multi-stage distillation tower system, a reboiler and a condenser. The multi-stage distillation tower system comprises a plurality of distillation towers connected in series. The interior of the distillation tower body is provided with a plurality of horizontally placed tower plates from top to bottom. Downcomers are provided at the ends of the tower plates perpendicular to the tower plates. Two adjacent tower plates in relatively upper and lower positions are respectively connected to the left and right sides of the inner wall of the tower body to achieve a stepped distribution of the tower plates inside the tower body. The tower plates are provided with evenly distributed holes. A feed port is provided on the tower plate in the middle of the first distillation tower and is connected to the feed pump. The top of each distillation tower is provided with a gas outlet and is connected to the feed port of the next distillation tower. The gas outlet of the final distillation tower is connected to the condenser, the condenser is connected to the reflux tank, and the outlet of the reflux tank is divided into two paths, one is connected to the finished product tank, and the other is connected to the top of the final distillation tower. A liquid outlet is provided at the bottom of each distillation tower, and all liquid outlets are connected in parallel and connected to the reboiler. The steam outlet of the reboiler is connected to the position below the lowest tower plate of the first distillation tower. A residual liquid pump is also provided at the liquid inlet of the reboiler and is connected to the residual liquid tank.

[0006] As a further improvement, the outside of the distillation tower is provided with insulation material to reduce energy loss.

[0007] As a further improvement, the tower plate is a sieve plate or a bubble point plate, and the pore size of the holes on the tower plate is 1 to 5 mm.

[0008] As a further improvement, an analyzer is provided at the outlet of the reflux tank for detecting the purity of the ammonia water, thereby determining whether the ammonia water passing through the reflux tank is refluxed into the distillation tower or exported to the finished product tank.

[0009] As a further improvement, the outlet of the reflux tank is further provided with a regulating reflux valve and a reflux pump for diverting the ammonia water. The regulating reflux valve is used to adjust the proportion of the ammonia water reflux, and the reflux pump is used to provide power.

[0010] As a further improvement, a heat exchanger is provided between the reboiler and the condenser for recovering heat from the condenser to provide heating for the reboiler.

[0011] Beneficial effects:

[0012] The utility model provides an efficient and intelligent electronic-grade ammonia distillation device with the following advantages:

[0013] This device utilizes a multi-stage distillation tower design to effectively improve the separation efficiency of ammonia and water. Through staged distillation, the evaporation and condensation processes are more complete, ensuring efficient mass transfer and heat exchange between the gas and liquid. The resulting ammonia water meets electronic-grade purity requirements.

[0014] This device adopts a high-efficiency heat exchanger and energy recovery system. By fully utilizing the heat of the condenser, the energy consumption of the reboiler is greatly reduced, and the energy utilization rate is significantly improved, thereby reducing the overall operating cost and achieving higher economic benefits.

[0015] The multi-stage distillation tower design increases the gas-liquid contact area and mass transfer rate, thereby improving the separation speed and distillation efficiency of ammonia. Compared with traditional single-tower distillation, this device significantly enhances production capacity and can produce high-purity ammonia in a shorter time, making it suitable for large-scale industrial continuous production. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the overall structure of an electronic grade ammonia distillation device;

[0017] 1. Feed pump 2. Distillation tower 21. Tray 22. Downcomer 3. Condenser 4. Reflux drum 41. Reflux pump 42. Adjustable reflux valve 5. Raffinate pump 6. Reboiler DETAILED DESCRIPTION

[0018] In order to deepen the understanding of the present invention, the present invention will be further described in detail below with reference to embodiments and drawings. The embodiments are only used to explain the present invention and do not constitute a limitation on the scope of protection of the present invention.

[0019] like Figure 1As shown, an electronic grade ammonia distillation device includes a feed pump 1, a distillation tower 2, a tower plate 21, a downcomer 22, a condenser 3, a reflux tank 4, a reflux pump 41, a regulating reflux valve 42, a residual liquid pump 5 and a reboiler 6.

[0020] An electronic grade ammonia distillation device comprises a multi-stage distillation tower system, a reboiler 6 and a condenser 3, wherein the multi-stage distillation tower 2 system comprises several distillation towers 2 connected in series, the tower body of the distillation tower 2 is provided with insulation material on the outside to reduce energy loss, the tower body of the distillation tower 2 is provided with several horizontally placed tower plates 21 from top to bottom, the end of the tower plate 21 is provided with a downcomer 22 perpendicular to the tower plate 21, and two adjacent tower plates 21 in relatively upper and lower positions are respectively connected to the left and right sides of the inner wall of the tower body to achieve a stepped distribution of the tower plates 21 inside the tower body, the tower plates 21 are sieve plates or bubble point plates, and are provided with evenly distributed holes on the tower plates 21, and the aperture size of the holes on the tower plates 21 is 1 to 5 mm, a feed port is provided at the tower plate 21 in the middle of the first distillation tower 2 and is connected to the feed pump 1, a gas outlet is provided at the top of each distillation tower 2 and is connected to the feed port of the next distillation tower 2, and the gas outlet of the last distillation tower 2 It is connected to the condenser 3, and the condenser 3 is connected to the reflux tank 4. The outlet of the reflux tank 4 is divided into two routes, one route is connected to the finished product tank, and the other route is connected to the top of the final distillation tower 2. The outlet of the reflux tank 4 is provided with an analyzer for detecting the purity of the ammonia water, so as to determine whether the ammonia water passing through the reflux tank 4 is refluxed into the distillation tower 2 or exported to the finished product tank. The outlet of the reflux tank 4 is also provided with a regulating reflux valve 42 and a reflux pump 41 for diverting the ammonia water. The regulating reflux valve 42 is used to adjust the ratio of the reflux of ammonia water, and the reflux pump 41 is used to provide power. A liquid outlet is provided at the bottom of each stage of the distillation tower 2, and all liquid outlets are connected in parallel and connected to a reboiler 6. The steam outlet of the reboiler 6 is connected to the position below the lowest tower plate 21 of the first distillation tower 2. A residual liquid pump 5 is also provided at the liquid inlet of the reboiler 6 and is connected to the residual liquid tank. A heat exchanger is provided between the reboiler 6 and the condenser 3 for recovering the heat of the condenser 3 to provide heating for the reboiler 6.

[0021] The raw ammonia water enters the middle of the first distillation tower 2 through the feed pipe. Before entering the distillation tower 2, the ammonia water is usually preheated to ensure that its temperature is close to the boiling point, thereby reducing the load of the reboiler 6;

[0022] The reboiler 6 is responsible for providing a heating source for the liquid in the tower. The ammonia water is heated at the bottom of the tower until it is partially vaporized. The low-boiling-point ammonia gas begins to vaporize and rise upward, while the high-boiling-point water remains in the liquid.

[0023] When ammonia vapor rises and comes into contact with liquid ammonia, the light component in the gas (low-boiling-point ammonia) is not easily condensed upon contact with the liquid and instead continues to accumulate in the gas phase. Simultaneously, a small amount of high-boiling-point component (water) in the gas condenses into liquid during the contact process and flows downward with the liquid, gradually increasing the heavy component (water) in the liquid phase. This process achieves the enrichment of the light component (ammonia) and the removal of the heavy component (water) through multiple gas-liquid exchange cycles.

[0024] The tower is provided with trays 21 to increase the gas-liquid contact area and further enhance the separation of ammonia and water. Ammonia is gradually concentrated in the gas phase, while the water content in the liquid is gradually reduced.

[0025] After the ammonia gas reaches the top of the final distillation tower 2, it is cooled and condensed into liquid through the condenser 3. Part of the condensed ammonia water returns to the tower as reflux liquid and continues to participate in the distillation process to improve the purity; the other part of the high-purity ammonia water is collected as the finished product.

[0026] After multiple cycles, the residual liquid at the bottom of the tower is mainly water-rich waste liquid, which will be discharged regularly through the discharge pipe for further treatment or as wastewater treatment. This ensures that the impurities rich in the liquid phase at the bottom of the tower will not continue to affect the distillation process.

[0027] Through the above steps, the device can effectively separate ammonia and water in ammonia water, and finally obtain ammonia water that meets the electronic grade purity standard.

[0028] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An electronic grade ammonia distillation device, characterized in that: The multi-stage distillation tower system includes a plurality of series-connected distillation towers, wherein a plurality of horizontally placed tower plates are arranged from top to bottom inside the tower body of the distillation tower, and a downcomer is arranged at the end of the tower plate perpendicular to the tower plate. Two adjacent tower plates in a relatively upper and lower position are respectively connected to the left and right sides of the inner wall of the tower body to realize the stepped distribution of the tower plates inside the tower body. The tower plates are provided with evenly distributed holes. A feed port is provided on the tower plate in the middle of the first distillation tower and is connected to a feed pump. Each distillation tower is connected to a feed pump. The top of the tower is provided with a gas outlet and is connected to the feed port of the next distillation tower. The gas outlet of the final distillation tower is connected to the condenser, the condenser is connected to the reflux tank, the outlet of the reflux tank is divided into two routes, one is connected to the finished product tank, and the other is connected to the top of the final distillation tower. A liquid outlet is provided at the bottom of each distillation tower, and all liquid outlets are connected in parallel and connected to the reboiler. The steam outlet of the reboiler is connected to the position below the lowest tower plate of the first distillation tower. A residual liquid pump is also provided at the liquid inlet of the reboiler and is connected to the residual liquid tank.

2. An electronic grade ammonia distillation device according to claim 1, characterized in that: The outside of the distillation tower is provided with heat-insulating material to reduce energy loss.

3. An electronic grade ammonia distillation device according to claim 1, characterized in that: The tower plate is a sieve plate or a bubble point plate, and the aperture of the holes on the tower plate is 1 to 5 mm.

4. The electronic grade ammonia distillation device according to claim 1, characterized in that: An analyzer is provided at the outlet of the reflux tank for detecting the purity of the ammonia water, thereby determining whether the ammonia water passing through the reflux tank is refluxed into the distillation tower or exported to the finished product tank.

5. The electronic grade ammonia distillation device according to claim 1, characterized in that: The outlet of the reflux tank is also provided with a regulating reflux valve and a reflux pump for diverting the ammonia water. The regulating reflux valve is used to adjust the proportion of the ammonia water reflux, and the reflux pump is used to provide power.

6. The electronic grade ammonia distillation device according to claim 1, characterized in that: A heat exchanger is provided between the reboiler and the condenser for recovering heat from the condenser to provide heating for the reboiler.