Preparation system of electronic-grade ammonia

Through the electronic grade ammonia preparation system with double-column distillation and recirculation reflux mechanism, the problems of high energy consumption and waste of raw materials are solved, the preparation of high-purity ammonia and the effective utilization of resources are achieved, energy consumption is reduced and gas emissions are reduced.

CN223082280UActive Publication Date: 2025-07-11TIANJIN ZHAOYIN TECH CO LTD
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Patent Information

Application Number
CN202421828768.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-07-30
Publication Date
2025-07-11
Estimated Expiration
2034-07-30

AI Technical Summary

Technical Problem

In the prior art, the preparation process of electronic grade ammonia has high energy consumption, serious waste of raw materials, and gas emissions pollute the environment, making it impossible to effectively utilize energy and resources.

Method used

A double-column distillation system is adopted, including a first distillation tower and a second distillation tower, and a circulation circuit is formed by combining a condenser and a reboiler. The separation of gas and liquid is achieved through a gas-liquid separator, and a closed heat pump circulation is performed using an ammonia cycle compressor to achieve heat recovery and utilization.

Benefits of technology

It improves the purity of ammonia, reduces raw material waste and gas emissions, reduces energy consumption, realizes the stable operation of the system and the effective utilization of resources, and meets the purity requirements of electronic grade ammonia.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the field of preparation of electronic-grade ammonia, and particularly discloses a preparation system of electronic-grade ammonia, which comprises a raw material tank, a first rectifying tower, a second rectifying tower, a reboiler, a condenser, an ammonia recovery tank and a gas-liquid separator, the second rectifying tower is communicated with the first rectifying tower, so that the liquid ammonia raw material in the first rectifying tower enters the second rectifying tower; the condenser further comprises a first raw material outlet and a fourth raw material inlet, the reboiler comprises a fifth raw material inlet and a second raw material outlet, the first raw material outlet is communicated with the fifth raw material inlet, and the second raw material outlet is communicated with the fourth raw material inlet, so that a circulation loop is formed between the condenser and the reboiler; liquid ammonia enriched with heavy components in the second rectifying tower enters the ammonia recovery tank; the gas-liquid separator further comprises a third gas phase outlet, the third gas phase outlet is communicated with the ammonia recovery tank, and the raw material ammonia is rectified twice, so that impurities can be more effectively removed, and the purity of the ammonia is improved.
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Description

Technical Field

[0001] The utility model relates to the field of the preparation industry of electronic-grade ammonia, and particularly relates to a preparation system of electronic-grade ammonia. Background Technique

[0002] Electronic-grade ammonia (NH3) is a high-purity ammonia used in the electronics industry and has a wide range of uses, including semiconductor manufacturing, flat panel display manufacturing, and photovoltaic cell manufacturing.

[0003] In the prior art, the purification process usually focuses on various unit operations around the vaporization of liquid ammonia and the condensation of gaseous ammonia. The whole process only pays attention to how to remove impurities in ammonia and improve the purity of ammonia, without considering optimizing the process flow from the perspective of comprehensive energy utilization, which easily causes problems such as high energy consumption, raw material waste, and environmental pollution caused by gas emissions.

[0004] For a super ammonia process for purifying electronic-grade ammonia with the existing patent application number CN202311326033.0, the selected raw material is liquid anhydrous ammonia, which is sent to a vaporizer through a liquid ammonia transfer pump. The vaporizer is heated by steam. The ammonia gas after oil removal enters an adsorption tower to remove moisture, and then enters a rectification system composed of a light component removal tower and a heavy component removal tower. A condenser is arranged at the top of the light component removal tower. After the gas phase at the top of the tower is condensed by the condenser, the liquid phase flows back to the light component removal tower, and the light components are discharged to a collection tank. A condenser is arranged in the collection tank, and the non-condensable gas is discharged to a tail gas treatment system. The liquid phase is collected in an industrial ammonia storage tank and sold as industrial ammonia; a reboiler is arranged at the bottom of the light component removal tower, and the liquid phase at the bottom of the tower is taken out to remove the light components and enter the heavy component removal tower. A condenser is arranged at the top of the heavy component removal tower. After the gas phase at the top of the tower is condensed by the condenser, the non-condensable gas is discharged to the collection tank. Part of the liquid phase flows back to the heavy component removal tower, and the remaining part is taken out as an ultra-pure ammonia product. In this process, the rectification system for purifying ammonia gas is relatively single, without energy recovery and utilization, and directly discharges the non-condensable gas to the tail gas treatment system after condensation by the condenser, without setting up equipment for separating the condensed liquid from the uncondensed gas, which easily causes incomplete separation and discharge of gas and liquid, and easily causes problems such as high energy consumption, raw material waste, and environmental pollution caused by gas emissions. Content of the Utility Model

[0005] The utility model provides a preparation system of electronic-grade ammonia to solve the technical problems of high energy consumption, raw material waste, and environmental pollution caused by gas emissions in the prior art.

[0006] To solve the above problems, a preparation system of electronic-grade ammonia provided by the utility model adopts the following technical solutions: including a raw material tank, a first rectification tower, a second rectification tower, a reboiler, a condenser, an ammonia recovery tank, and a gas-liquid separator;

[0007] The first distillation column includes a first raw material inlet, a first gas phase outlet, and a second raw material inlet. The raw material tank is interconnected with the first raw material inlet. The condenser includes a first raw material gas inlet and a first raw material gas outlet. The gas-liquid separator includes a condensed raw material inlet and a liquid phase outlet. The first gas phase outlet is interconnected with the first raw material gas inlet. The first raw material gas outlet is interconnected with the condensed raw material inlet. The liquid phase outlet is interconnected with the second raw material inlet;

[0008] The second distillation column is interconnected with the first distillation column so that the liquid ammonia raw material in the first distillation column enters the second distillation column;

[0009] The second distillation column includes a second gas phase outlet and a third raw material inlet. The condenser further includes a second raw material gas inlet and a second raw material gas outlet. The second gas phase outlet is interconnected with the second raw material gas inlet. The second raw material gas outlet is interconnected with the third raw material inlet;

[0010] The condenser further includes a first raw material outlet and a fourth raw material inlet. The reboiler includes a fifth raw material inlet and a second raw material outlet. The first raw material outlet is interconnected with the fifth raw material inlet. The second raw material outlet is interconnected with the fourth raw material inlet so that a circulation loop is formed between the condenser and the reboiler;

[0011] The reboiler further includes a liquid ammonia outlet so that the liquid ammonia enriched with heavy components in the second distillation column enters the ammonia recovery tank through the liquid ammonia outlet;

[0012] The gas-liquid separator further includes a third gas phase outlet. The third gas phase outlet is interconnected with the ammonia recovery tank.

[0013] The beneficial effects of the preparation system for electronic-grade ammonia provided by the present utility model are as follows: The raw material ammonia undergoes two distillations, which can more effectively remove impurities and improve the purity of ammonia; the circulation loop formed between the condenser and the reboiler enables the liquid in the system to be recycled, achieving effective utilization of heat and stable operation of the system. This not only reduces waste of raw materials but also improves the operation efficiency of the system; the setting of the gas-liquid separator can effectively separate the condensed liquid from the uncondensed gas, ensuring the purity of liquid ammonia. The separated gas enters the ammonia recovery tank through the third gas phase outlet, realizing the recovery and utilization of the uncondensed gas, avoiding waste of gas, and providing convenience for further recovery of ammonia; through the two-tower distillation and circulation reflux mechanism, the liquid ammonia finally produced by the system has extremely high purity and can meet the requirements of electronic-grade ammonia; the various components in the system cooperate with each other to jointly complete the conversion process from raw material ammonia to electronic-grade ammonia. The condenser and reboiler used in the system can effectively recover and utilize heat, reducing the energy consumption of the system. At the same time, by reducing waste of raw materials and gas emissions, the goal of energy conservation and emission reduction is also achieved.

[0014] Further, a pipeline 1 is provided between the raw material tank and the first raw material inlet. A raw material pump is provided on the pipeline 1. The liquid ammonia raw material liquid in the raw material tank enters the first rectification column through the raw material pump and the first raw material inlet in sequence.

[0015] Further, the second raw material gas outlet is connected to a three-way connector, and the other two interfaces of the three-way connector are respectively connected to the third raw material inlet and the product storage tank.

[0016] Further, a pipeline 2 is provided between the first raw material outlet and the fifth raw material inlet. An ammonia circulation compressor is provided on the pipeline 2. The raw material in the condenser enters the reboiler through the first raw material outlet, the ammonia circulation compressor, and the fifth raw material inlet in sequence to realize the closed heat pump cycle of the ammonia working medium.

[0017] Further, the liquid ammonia mole fraction of the liquid in the ammonia recovery tank is N1, the liquid ammonia mole fraction of the liquid ammonia raw material liquid in the raw material tank is N2, the liquid ammonia mole fraction of the liquid ammonia raw material rich in heavy components obtained at the bottom of the first rectification column is N3, and the liquid ammonia mole fraction of the ultra-pure ammonia product obtained at the top of the second rectification column is N4, where N1 < N2 < N3 < N4.

[0018] Further, the first rectification column, the second rectification column, and the reboiler are integrally designed.

[0019] Further, a pipeline 3 is connected between the second gas phase outlet of the second rectification column and the second raw material gas inlet of the condenser, a pipeline 4 is connected between the three-way connector and the product storage tank, a pipeline 5 is connected between the third gas phase outlet of the gas-liquid separator and the ammonia recovery tank, a pipeline 6 is connected between the liquid ammonia outlet of the reboiler and the ammonia recovery tank, and a pipeline 7 is connected between the second raw material outlet of the reboiler and the fourth raw material inlet of the condenser. Control valves are provided on the pipeline 3, the pipeline 4, the pipeline 5, the pipeline 6, and the pipeline 7. Description of the Drawings

[0020] By referring to the accompanying drawings and reading the detailed description below, the above and other objectives, features, and advantages of the exemplary embodiments of the present utility model will become easily understandable. In the drawings, several embodiments of the present utility model are shown in an exemplary rather than restrictive manner, and the same or corresponding reference numerals represent the same or corresponding parts, where:

[0021] Figure 1 is a schematic structural diagram of a preparation system for electronic-grade ammonia of the present utility model;

[0022] Figure 2 is a schematic structural diagram of steps S1 and S2 of a preparation system for electronic-grade ammonia of the present utility model;

[0023] Figure 3 is a schematic structural diagram of steps S3 and S4 of a preparation system for electronic-grade ammonia of the present utility model;

[0024] Figure 4 It is a schematic structural diagram of step S5 of a preparation system for electronic-grade ammonia according to the present utility model;

[0025] Figure 5 It is a schematic structural diagram of the cooperation of the first rectification column, the second rectification column, and the reboiler of a preparation system for electronic-grade ammonia according to the present utility model.

[0026] Explanation of reference numerals:

[0027] 1. Raw material tank; 11. Pipeline 1; 12. Raw material pump;

[0028] 2. First rectification column; 21. First raw material inlet; 22. First gas phase outlet; 23. Second raw material inlet;

[0029] 3. Second rectification column; 31. Second gas phase outlet; 311. Pipeline 3; 32. Third raw material inlet;

[0030] 4. Reboiler; 41. Fifth raw material inlet; 42. Second raw material outlet; 421. Pipeline 7; 43. Liquid ammonia outlet; 431. Pipeline 6;

[0031] 5. Condenser; 51. First raw material gas inlet; 52. First raw material gas outlet; 53. Second raw material gas inlet; 54. Second raw material gas outlet; 541. Three-way connector; 542. Product storage tank; 543. Pipeline 4; 55. First raw material outlet; 551. Pipeline 2; 552. Ammonia circulation compressor; 56. Fourth raw material inlet;

[0032] 6. Ammonia recovery tank;

[0033] 7. Gas-liquid separator; 71. Condensed raw material inlet; 72. Liquid phase outlet; 73. Third gas phase outlet; 731. Pipeline 5;

[0034] 8. Control valve. Detailed implementation manners

[0035] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present utility model. Those skilled in the art should know that the embodiments described below are part of the embodiments of the present disclosure, rather than all of the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative efforts shall fall within the protection scope of the present utility model.

[0036] The quantity of any element in the accompanying drawings is for illustration rather than limitation, and any naming is only for distinction and does not have any limiting meaning.

[0037] The principles and spirit of the present utility model will be explained in detail below with reference to several representative embodiments of the present utility model.

[0038] A preparation system for electronic-grade ammonia provided by the present utility model is as Figures 1 to 5 shown:

[0039] A preparation system for electronic-grade ammonia includes a raw material tank 1, a first rectification tower 2, a second rectification tower 3, a reboiler 4, a condenser 5, an ammonia recovery tank 6, and a gas-liquid separator 7;

[0040] The first rectification tower 2 includes a first raw material inlet 21, a first gas phase outlet 22, and a second raw material inlet 23. The raw material tank 1 is interconnected with the first raw material inlet 21. The condenser 5 includes a first raw material gas inlet 51 and a first raw material gas outlet 52. The gas-liquid separator 7 includes a condensed raw material inlet 71 and a liquid phase outlet 72. The first gas phase outlet 22 is interconnected with the first raw material gas inlet 51. The first raw material gas outlet 52 is interconnected with the condensed raw material inlet, and the liquid phase outlet 72 is interconnected with the second raw material inlet 23;

[0041] The second rectification tower 3 is interconnected with the first rectification tower 2 so that the liquid ammonia raw material in the first rectification tower 2 enters the second rectification tower 3;

[0042] The second rectification tower 3 includes a second gas phase outlet 31 and a third raw material inlet 32. The condenser 5 further includes a second raw material gas inlet 53 and a second raw material gas outlet 54. The second gas phase outlet 31 is interconnected with the second raw material gas inlet 53, and the second raw material gas outlet 54 is interconnected with the third raw material inlet 32;

[0043] The condenser 5 further includes a first raw material outlet 55 and a fourth raw material inlet 56. The reboiler 4 includes a fifth raw material inlet 41 and a second raw material outlet 42. The first raw material outlet 55 is interconnected with the fifth raw material inlet 41, and the second raw material outlet 42 is interconnected with the fourth raw material inlet 56 to form a circulation loop between the condenser 5 and the reboiler 4;

[0044] The reboiler 4 further includes a liquid ammonia outlet 43 so that the liquid ammonia enriched with heavy components in the second rectification tower 3 enters the ammonia recovery tank 6 through the liquid ammonia outlet 43;

[0045] The gas-liquid separator 7 further includes a third gas phase outlet 73, and the third gas phase outlet 73 is interconnected with the ammonia recovery tank 63.

[0046] In this embodiment, a pipeline 11 is provided between the raw material tank 1 and the first raw material inlet 21. A raw material pump 12 is provided on the pipeline 11. The liquid ammonia raw material liquid in the raw material tank 1 enters the first rectification tower 2 through the raw material pump 12 and the first raw material inlet 21 in sequence, and the pressure of the liquid ammonia raw material liquid after the raw material pump 12 increases.

[0047] In this embodiment, the second raw material gas outlet 54 is connected to a tee joint 541, and the other two interfaces of the tee joint 541 are respectively connected to the third raw material inlet 32 and the product storage tank 542.

[0048] In this embodiment, a second pipeline 551 is provided between the first raw material outlet 55 and the fifth raw material inlet 41, and an ammonia circulation compressor 552 is provided on the second pipeline 551.

[0049] When the above-mentioned preparation system for electronic-grade ammonia is used, it mainly includes the following steps:

[0050] S1: The liquid ammonia raw material in the raw material tank 1 enters the first distillation column 2 through the first raw material inlet 21 of the first distillation column 2; the composition of the liquid ammonia raw material liquid is methane, carbon dioxide, argon, nitrogen, ethane; the liquid ammonia raw material liquid in the raw material tank 1 is a saturated liquid. In this embodiment, the temperature of the raw material liquid in the raw material tank 1 is 22°C, the pressure is 0.6 MpaG, the liquid ammonia mole fraction ≥ 99%, the pressure of the raw material liquid after the raw material pump 12 is 0.8 MpaG, and the raw material liquid after the raw material pump 12 is a saturated liquid.

[0051] S2: The raw material gas is rectified and purified in the first distillation column 2. The rectified and purified gas phase enters the condenser 5 through the first gas phase outlet 22 of the first distillation column 2 and the first raw material gas inlet 51 of the condenser 5. After condensation, it passes through the first raw material gas outlet 52 and the condensed raw material inlet 71 into the gas-liquid separator 7. After gas-liquid separation, the non-condensable gas enters the ammonia recovery tank 6 through the third gas phase outlet 73 of the gas-liquid separator 7. The liquid phase successively passes through the liquid phase outlet 72 and the second raw material inlet 23 into the first distillation column 2 and serves as the reflux liquid required by the first distillation column 2. Under the action of the condenser 5, the temperature of the raw material gas at the first gas phase outlet 22 of the first distillation column 2 is higher than the temperature of the raw material gas at the first raw material gas outlet 52 of the condenser 5. In this embodiment, the first gas phase outlet 22 is located at the top of the first distillation column 2, and the temperature of the raw material gas at the first gas phase outlet 22 is 21°C. The temperature of the raw material gas at the first raw material gas inlet 51 of the condenser 5 is 16°C. The first distillation column 2 removes light components in the raw material gas, such as nitrogen, methane, carbon dioxide, etc., and a liquid ammonia raw material rich in heavy components is obtained at the bottom of the first distillation column 2. At this time, the liquid ammonia mole fraction ≥ 99.99%.

[0052] S3: The liquid ammonia raw material rich in heavy components obtained from the bottom of the first rectification column 2 in step S2 enters the second rectification column 3. The second rectification column 3 further rectifies and purifies the raw material gas. The second rectification column 3 mainly removes heavy components in the raw material gas, such as moisture, metal ions, particulate matters, etc. The gas phase after rectification and purification sequentially passes through the second gas phase outlet 31 of the second rectification column 3 and the second raw material gas inlet 53 of the condenser 5 and enters the condenser 5. Then, it passes through the second raw material gas outlet 54 of the condenser 5 and the third raw material inlet 32 and enters the second rectification column 3 as the reflux liquid required by the second rectification column 3. An ultra-pure ammonia product is obtained at the top of the second rectification column 3. In this embodiment, the ultra-pure ammonia product enters the product storage tank 542 through the three-way connector 541 for storage. In this embodiment, the mole fraction of liquid ammonia at the top of the second rectification column 3 ≥ 99.99999%, the temperature is 22 °C, and the pressure is 0.8 MpaG.

[0053] S4: The liquid ammonia enriched with heavy components obtained from the bottom of the second rectification column 3 in step S3 enters the ammonia recovery tank 6 through the liquid ammonia outlet 43 of the reboiler 4. The liquid in the ammonia recovery tank 6 can be sold as industrial-grade liquid ammonia. In this embodiment, the mole fraction of liquid ammonia in the ammonia recovery tank 6 ≥ 98.5%, the temperature is -28 °C, and the pressure is 0.03 MpaG.

[0054] S5: The raw material evaporated by the condenser 5 sequentially passes through the first raw material outlet 55 of the condenser 5 and the fifth raw material inlet 41 of the reboiler 4 and enters the reboiler 4 to provide heat source for the rectification process. After liquefying itself, it passes through the second raw material outlet 42 of the reboiler 4 and enters the condenser 5 through the fourth raw material inlet 56 of the condenser 5 to provide cold source for the rectification process. After vaporizing itself, it repeats step S5. In this embodiment, the raw material in the condenser 5 sequentially passes through the first raw material outlet 55, the ammonia circulation compressor 552, and the fifth raw material inlet 41 and enters the reboiler 4 to realize the closed heat pump cycle of the ammonia working medium. The inlet pressure of the ammonia circulation compressor 552 is less than the outlet pressure of the ammonia circulation compressor 552. In this embodiment, the inlet pressure of the ammonia circulation compressor 552 is 0.45 MpaG, and the outlet pressure of the ammonia circulation compressor 552 is 1.0 MpaG.

[0055] It should be noted that the temperature and pressure in steps S1 - S5 can be adjusted and optimized according to actual working needs.

[0056] In this embodiment, the temperature at the top of the second rectification column 3 is equal to the temperature of the liquid ammonia raw material in the raw material tank 1, and the pressure of the ultra-pure ammonia product at the top of the second rectification column 3 is equal to the pressure of the liquid ammonia raw material after the raw material pump 12.

[0057] In this embodiment, the liquid ammonia mole fraction of the liquid in the ammonia recovery tank 6 is N1, the liquid ammonia mole fraction of the liquid ammonia raw material liquid in the raw material tank 1 is N2, the liquid ammonia mole fraction of the liquid ammonia raw material rich in heavy components obtained at the bottom of the first distillation column 2 in step S2 is N3, and the liquid ammonia mole fraction of the ultra-pure ammonia product obtained at the top of the second distillation column 3 in step S3 is N4. N1 < N2 < N3 < N4, realizing the gradual purification of the raw material liquid ammonia and finally obtaining the ultra-pure ammonia product.

[0058] As Figure 5 shown, in this embodiment, the first distillation column 2, the second distillation column 3, and the reboiler 4 are integrally designed. Both the first distillation column 2 and the second distillation column 3 have the function of removing heavy components, which can not only greatly reduce the heat exchange load at the top of the column, but also reduce the number of theoretical plates of the distillation column, reducing equipment investment and installation difficulty.

[0059] In this embodiment, the raw material gas in the first distillation column 2 and the second distillation column 3 simultaneously realizes secondary condensation reflux, which can effectively improve the product concentration efficiency.

[0060] In this embodiment, the gas phase at the top of the first distillation column 2 and the gas phase at the top of the second distillation column 3 are both connected to the condenser 5. The condenser 5 and the gas-liquid separator 7 work together to realize the multiple condensation recovery of the product components in the light components. There is no need to support an industrial-grade product recovery system, which can effectively improve the product yield, reduce investment and production costs, and greatly simplify the process.

[0061] In this embodiment, a pipeline three 311 is connected between the second gas phase outlet 31 of the second distillation column 3 and the second raw material gas inlet 53 of the condenser 5. A pipeline four 543 is connected between the three-way connector 541 and the product storage tank 542. A pipeline five 731 is connected between the third gas phase outlet 73 of the gas-liquid separator 7 and the ammonia recovery tank 6. A pipeline six 431 is connected between the liquid ammonia outlet 43 of the reboiler 4 and the ammonia recovery tank 6. A pipeline seven 421 is connected between the second raw material outlet 42 of the reboiler 4 and the fourth raw material inlet 56 of the condenser 5. Control valves 8 are provided on the pipeline three 311, the pipeline four 543, the pipeline five 731, the pipeline six 431, and the pipeline seven 421, realizing the precise control of the flow direction and flow rate of different fluids during the distillation process, thereby ensuring the high efficiency and stability of the distillation process.

[0062] In the preparation system of the electronic-grade ammonia, the raw ammonia undergoes two rectification processes, which can more effectively remove impurities and improve the purity of ammonia. The circulating loop formed between the condenser 5 and the reboiler 4 enables the liquid in the system to be recycled, achieving the effective utilization of heat and the stable operation of the system. This not only reduces the waste of raw materials but also improves the operation efficiency of the system. The installation of the gas-liquid separator 7 can effectively separate the condensed liquid from the uncondensed gas, ensuring the purity of the liquid ammonia. The separated gas enters the ammonia recovery tank 6 through the third gas phase outlet 73, realizing the recovery and utilization of the uncondensed gas, avoiding the waste of gas, and providing convenience for the further recovery of ammonia. Through the double-column rectification and the circulating reflux mechanism, the liquid ammonia finally produced by this system has extremely high purity and can meet the requirements of electronic-grade ammonia. Each component in the system cooperates with each other to jointly complete the conversion process from raw ammonia to electronic-grade ammonia. The condenser 5 and the reboiler 4 used in the system can effectively recover and utilize heat, reducing the energy consumption of the system. At the same time, by reducing the waste of raw materials and gas emissions, the goal of energy conservation and emission reduction is also achieved.

[0063] Through the continuous rectification and purification of two rectification towers, the preparation system of the electronic-grade ammonia can effectively remove the light components and heavy components in the raw materials, achieve the deep purification of ammonia gas, and realize the production of high-purity ammonia products, the effective recovery and utilization of resources, the optimization of energy efficiency, the stable and reliable operation of the system, as well as environmental protection and sustainable development.

[0064] Based on the above description in this specification, those skilled in the art can also understand the following terms used. For example, terms indicating orientation or positional relationships such as "upper", "lower", "front", "rear", "left", "right", "width", "horizontal", "top", "bottom", "inner", "outer", etc. are based on the orientation or positional relationships shown in the drawings of this specification. They are only for the purpose of facilitating the description of the solution of the present invention and simplifying the description, rather than explicitly or implicitly indicating that the device or element involved must have the specific orientation, be constructed and operate in the specific orientation. Therefore, the above orientation or positional relationship terms cannot be understood or interpreted as a limitation to the solution of the present invention.

[0065] In addition, in the description of this specification, the meaning of "a plurality of" is at least two, such as two, three or more, etc., unless otherwise specifically and clearly defined.

Claims

1. An electronic-grade ammonia preparation system, characterized in that, It includes a raw material tank, a first rectification column, a second rectification column, a reboiler, a condenser, an ammonia recovery tank, and a gas-liquid separator; The first rectification column includes a first raw material inlet, a first gas phase outlet, and a second raw material inlet. The raw material tank is interconnected with the first raw material inlet. The condenser includes a first raw material gas inlet and a first raw material gas outlet. The gas-liquid separator includes a condensed raw material inlet and a liquid phase outlet. The first gas phase outlet is interconnected with the first raw material gas inlet, the first raw material gas outlet is interconnected with the condensed raw material inlet, and the liquid phase outlet is interconnected with the second raw material inlet; The second rectification column is interconnected with the first rectification column so that the liquid ammonia raw material in the first rectification column enters the second rectification column; The second rectification column includes a second gas phase outlet and a third raw material inlet. The condenser also includes a second raw material gas inlet and a second raw material gas outlet. The second gas phase outlet is interconnected with the second raw material gas inlet, and the second raw material gas outlet is interconnected with the third raw material inlet; The condenser also includes a first raw material outlet and a fourth raw material inlet. The reboiler includes a fifth raw material inlet and a second raw material outlet. The first raw material outlet is interconnected with the fifth raw material inlet, and the second raw material outlet is interconnected with the fourth raw material inlet to form a circulation loop between the condenser and the reboiler; The reboiler also includes a liquid ammonia outlet so that the liquid ammonia enriched with heavy components in the second rectification column enters the ammonia recovery tank through the liquid ammonia outlet; The gas-liquid separator also includes a third gas phase outlet, and the third gas phase outlet is interconnected with the ammonia recovery tank.

2. The preparation system of electronic-grade ammonia according to claim 1, wherein, A pipeline one is provided between the raw material tank and the first raw material inlet. A raw material pump is provided on the pipeline one. The liquid ammonia raw material liquid in the raw material tank sequentially enters the first rectification column through the raw material pump and the first raw material inlet.

3. The preparation system of electronic-grade ammonia according to claim 2, characterized in that, The second raw material gas outlet is connected to a three-way connector, and the other two interfaces of the three-way connector are respectively connected to the third raw material inlet and the product storage tank.

4. A preparation system for electronic-grade ammonia according to any one of claims 1 to 3, characterized in that, A pipeline two is provided between the first raw material outlet and the fifth raw material inlet. An ammonia circulation compressor is provided on the pipeline two. The raw material in the condenser sequentially enters the reboiler through the first raw material outlet, the ammonia circulation compressor, and the fifth raw material inlet to realize the closed heat pump cycle of the ammonia working medium.

5. A preparation system for electronic-grade ammonia according to any one of claims 1 to 3, characterized in that, The first rectification column, the second rectification column, and the reboiler are integrally designed.

6. A preparation system for electronic-grade ammonia according to any one of claims 1 to 3, characterized in that, A pipeline three is connected between the second gas phase outlet of the second rectification column and the second raw material gas inlet of the condenser. A pipeline four is connected between the three-way connector and the product storage tank. A pipeline five is connected between the third gas phase outlet of the gas-liquid separator and the ammonia recovery tank. A pipeline six is connected between the liquid ammonia outlet of the reboiler and the ammonia recovery tank. A pipeline seven is connected between the second raw material outlet of the reboiler and the fourth raw material inlet of the condenser. Control valves are provided on the pipeline three, the pipeline four, the pipeline five, the pipeline six, and the pipeline seven.

Citation Information

Patent Citations

  • Process for purifying super ammonia from electronic-grade ammonia gas

    CN117285047A