Production device and production method of electronic-grade nitric oxide

By adopting a capsule filter and circulating pump system in the electronic-grade nitric oxide production process, combined with the double-tower distillation and purification method, the problems of high load on the stirring blade and high wastewater are solved, and high-efficiency and low-cost large-scale production is achieved.

CN119608060APending Publication Date: 2025-03-14HUBEI SINOPHORUS ELECTRONIC MATERIALS CO LTD
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Patent Information

Application Number
CN202411656910.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-19
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

The existing electronic-grade nitric oxide purification process has problems such as high load on stirring blades and a lot of wastewater, and the adsorption process cannot meet the needs of large-scale production.

Method used

The capsule filter and circulation pump system are used instead of the traditional stirring blades. Through the switching between the capsule filters A and B, the supersaturated crystals of sodium sulfate are effectively removed and the wastewater production is reduced. The double-tower distillation purification method is used to use liquid nitrogen as the refrigerant to achieve high purity nitric oxide production.

Benefits of technology

Nitric oxide with low load, less wastewater and large-scale continuous production is achieved, reducing production costs and improving the purity and quality of the product.

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Abstract

The invention discloses an electronic grade nitric oxide production device and method, the electronic grade nitric oxide production device comprises a sulfuric acid storage tank and a reactor, the reactor is connected with a bag type filter A and a bag type filter B in parallel, the bag type filter A, the bag type filter B and a reactor pipeline circulate through a pump, and are connected with a nitrogen pipeline and an evacuation vacuum pipeline; an outlet pipeline at the upper end of the reactor is connected with the first rectifying tower and the second rectifying tower, and electronic-grade nitric oxide is extracted from the second rectifying tower and filled into a steel cylinder. Compared with a traditional reaction kettle using stirring blades, sodium sulfate supersaturated crystals produced through reaction are effectively separated through circulation of a pump and a bag type filter, generation of waste water is reduced, meanwhile, the reaction speed in the reactor is increased, the problems that a large number of solids are generated in the reaction, and the stirring blades are high in energy consumption and damaged are solved, and the reaction kettle is worthy of industrial popularization.
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Description

Technical Field

[0001] The invention relates to a production device and a production method of electronic-grade nitric oxide, belonging to the field of electronic special gases. Background Art

[0002] Nitric oxide is a nitrogen oxide compound, a colorless, odorless, highly toxic gas that is difficult to dissolve in water. Nitric oxide has multiple functions and applications in chip production processes, such as cleaning, deposition, and surface treatment. Its high reactivity, gas state, and biological activity make it one of the indispensable raw materials in the chip manufacturing process. By rationally utilizing nitric oxide, the quality and performance of chips can be improved, and the continuous development and innovation of chip manufacturing technology can be promoted. Therefore, with the development of semiconductors, the purity requirements for nitric oxide have become increasingly stringent.

[0003] In the current electronic grade nitric oxide purification method on the market, sodium nitrite and dilute sulfuric acid are used to react to prepare nitric oxide raw materials. Because the reaction of sodium nitrite and dilute sulfuric acid involves the dissolution of solid sodium nitrate, the traditional reactor uses a stirring blade to accelerate the dissolution to achieve the purpose of sufficient reaction. The solubility of the sodium sulfate supersaturated crystal produced by the reaction is low relative to that of sodium nitrite. The reaction produces a large amount of sodium sulfate supersaturated crystals, which increases the load of the stirring blade. In the traditional process, the sodium sulfate supersaturated crystals are dissolved by adding water to reduce the load of the stirring blade. However, this method will produce a large amount of wastewater, and at the same time, it will have a certain impact on the reaction rate and increase the production cost. In addition, the traditional nitric oxide purification technology uses an adsorption process to remove gas impurities such as water, nitrogen dioxide, and nitrous oxide, which cannot meet the needs of large-scale production.

[0004] In summary, the existing processes for preparing raw nitric oxide have problems such as high load on the stirring blades and a lot of wastewater, and the adsorption and purification process of nitric oxide cannot be mass-produced. Therefore, it is necessary to develop a large-scale continuous production device and method for electronic-grade nitric oxide with stable operation, low load, less wastewater and low cost.

[0005] The supersaturated sodium sulfate crystals produced by the reaction can be effectively separated through the circulation of the pump and the capsule filter, thus reducing the generation of wastewater and increasing the reaction rate in the reactor. This solves the problem of high energy consumption and damage of the stirring blades due to the generation of a large amount of solids in the reaction, and is worthy of promotion in the industry. Summary of the invention

[0006] The purpose of the present invention is to overcome the above-mentioned shortcomings and provide a production device and a production method for electronic-grade nitric oxide, so as to achieve continuous large-scale production of electronic-grade nitric oxide with less wastewater, high reaction rate, low cost and comprehensive resource utilization.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is: A production device for electronic grade nitric oxide, comprising a sulfuric acid storage tank, a reactor, a capsule filter A, and a capsule filter B; The tops of capsule filters A and B are connected in parallel through a pipeline, and the bottoms of capsule filters A and B are connected in parallel through a pipeline, so that capsule filters A and B can be used interchangeably. The bottom outlet of the reactor is connected to the pipeline connected in parallel with the tops of the capsule filter A and the capsule filter B through a liquid phase feed pump to form a circulation pipeline; The pipes connected in parallel at the bottom of capsule filter A and capsule filter B are then connected to the lower inlet of the reactor to form a circulation pipeline; The outlet pipeline at the upper end of the reactor is connected to the first distillation tower and the second distillation tower, and the electronic grade nitric oxide is extracted from the second distillation tower and filled into a steel cylinder.

[0008] A sulfuric acid storage tank and a water inlet pipeline are arranged on the top of the reactor, and a sulfuric acid metering pump is connected to the sulfuric acid pipeline; Valves are arranged on the pipes connected in parallel at the tops of capsule filter A and capsule filter B, namely, valve three of capsule filter A and valve three of capsule filter B.

[0009] A valve is provided on the liquid phase pipeline 1 connected in parallel at the bottom of the capsule filter A and the capsule filter B, namely, valve 4 of the capsule filter A and valve 4 of the capsule filter B; The filter membranes of the capsule filter A and the capsule filter B are made of one of PTFE, ceramics and 316L metal.

[0010] A nitrogen valve 1 is provided at the top of the reactor; a gas phase valve 2 is provided on the pipeline from the top of the reactor to the first distillation tower, and a gas phase feed pump is provided on the pipeline; The capsule filter A and the capsule filter B are respectively provided with nitrogen inlet pipes on the top, i.e., nitrogen inlet pipe A1 and nitrogen inlet pipe B1, and valves are respectively provided on the nitrogen inlet pipe A1 and the nitrogen inlet pipe B1, i.e., nitrogen inlet pipe A valve 2 and nitrogen inlet pipe B valve 2.

[0011] The capsule filter A and the capsule filter B are respectively provided with nitrogen output pipelines at the bottom, i.e., nitrogen output pipeline A 6 and nitrogen output pipeline B 6, and valves are respectively provided on the nitrogen output pipeline A 6 and nitrogen output pipeline B 6, i.e., nitrogen output pipeline A valve 5 and nitrogen output pipeline B valve 5; The nitrogen output pipeline A and the nitrogen output pipeline B are connected to the evacuation pipe after merging; the bottom of the reactor is connected to the exhaust pipe, and the exhaust pipe is provided with an exhaust pipe vacuum pump, and the end of the exhaust pipe is connected to the waste liquid tank.

[0012] The first distillation tower is connected to the first heat exchanger, the second distillation tower is connected to the second heat exchanger, and the heat exchanger uses liquid nitrogen as the refrigerant.

[0013] Based on the above technical solution, the present invention also provides a method for producing electronic-grade nitric oxide, which is implemented using the electronic-grade nitric oxide production device, and the production method comprises the following steps: S1: After evacuating all components in the production device for electronic grade nitric oxide, the entire production device is purged with nitrogen; S2: Add NaNO2 solid into the reactor, add water and then add dilute sulfuric acid into the reactor to react; S3: when the pressure in the reactor is constant, open the gas phase valve 2 connected to the distillation tower, start the liquid phase feed pump, open the capsule filter A valve 3 and the capsule filter A valve 4 on the capsule filter A, so that the reactor and the capsule reactor A form a cycle, and a pressure difference is formed at both ends of the capsule reactor A, first close the capsule filter A valve 3, open the capsule filter B valve 3 and the capsule filter B valve 4 on the capsule filter B, and finally close the capsule filter A valve 4, open the nitrogen output pipeline A valve 5, start the emptying pipe vacuum pump, evacuate the capsule filter A, make the precipitated Na2SO4 supersaturated crystals on the filter screen fall off to the bottom of the capsule filter, empty the Na2SO4 supersaturated crystals through the emptying pipe, and close the nitrogen output pipeline A valve 5; S4: When a pressure difference is achieved at both ends of the capsule reactor B, first close the valve 3 of the capsule filter B, open the valve 3 of the capsule filter A and the valve 4 of the capsule filter A on the capsule filter A, and finally close the valve 4 of the capsule filter B, open the valve 5 of the nitrogen output pipeline B, start the vacuum pump of the emptying pipe, evacuate the capsule filter B, make the supersaturated crystals of Na2SO4 precipitated on the filter screen fall off to the bottom of the capsule filter, empty the supersaturated crystals of Na2SO4 through the emptying pipe, close the valve 5 of the nitrogen output pipeline B, repeat the S3 operation to switch to the capsule filter A; S5: The nitric oxide gas produced by the reactor enters the first distillation tower and the second distillation tower in sequence, and the electronic grade nitric oxide is taken out from the second distillation tower and filled into a steel cylinder; S6: After the reactor no longer produces nitric oxide, switch to the reactor and start the S2-S5 reaction process.

[0014] The reactor can also be provided with another standby reactor, so that the reactors can be used as a standby reactor and switched to each other. Then step S6 is: after the reactor no longer produces nitric oxide, switch to the standby reactor to start the reaction process of S2-S5, open the bottom valve of the reactor, start the vacuum pump 7, and discharge the reactants in the reactor to the waste liquid tank through the drain pipe.

[0015] In the S1, the mass ratio of NaNO2 solid, water and dilute sulfuric acid is: 1-1.5: 1.5-2: 0.5-1.5; the mass concentration of the dilute sulfuric acid is 50-70%. In some embodiments, the mass concentration of the dilute sulfuric acid is 60%.

[0016] The pressure difference obtained in S2 and S3 is 0.4-1.0 MPa, and more preferably 0.5-0.8 MPa. This pressure difference is to protect the filter. Too high pressure will cause the filter membrane to break, and too low pressure will cause too low efficiency.

[0017] In a preferred embodiment, the number of plates of the first distillation tower is 25-40, more preferably 28-35, and the feed plate position is the 18th to 22nd plate from the bottom, and more preferably the 19th to 21st plate.

[0018] In a preferred embodiment, the number of plates of the second distillation tower is 28-40, more preferably 28-35, and the feed plate position is the 18th to 22nd plate from the bottom, and more preferably the 19th to 21st plate.

[0019] In a preferred embodiment, the top temperature of the first distillation tower is -115~-105°C, more preferably -110~-106°C, the bottom temperature is -108~-100°C, more preferably -109~-103°C, and the mass reflux ratio of the first distillation tower is 1.5~5, more preferably 2~4.

[0020] In a preferred embodiment, the top temperature of the second distillation tower is -140~-128°C, more preferably -138~-130°C, the bottom temperature is -110~-100°C, more preferably -108~-105°C, and the mass reflux ratio of the first distillation tower is 20~35, more preferably 22~28.

[0021] Compared with the prior art, the present invention has the following advantages: 1. The present invention adopts sodium nitrite and dilute sulfuric acid to react and prepare raw material nitric oxide. By establishing a reactor-pump-capsule filter circulation system, the traditional stirring blade is replaced to make the reaction material fully contact, and the materials can be effectively mixed evenly. At the same time, the capsule filter is used for filtering, and the sodium sulfate supersaturated crystals with low solubility generated by the reaction can be effectively removed, and the load of solid stirring on the stirring blade is reduced, and the sodium sulfate supersaturated crystals are prevented from being adsorbed on the blade surface, which solves the problem of the fragility of the stirring blade. Through the mutual switching of the capsule filter A and the capsule filter B, the effective removal of the sodium sulfate supersaturated crystals is guaranteed, and the traditional process is avoided to use water to dissolve the sodium sulfate supersaturated crystals, which not only reduces the reaction rate, but also generates a large amount of saline wastewater that needs to be treated, increasing the production cost, filtering through the capsule filter, and the mutual switching of the capsule filter A and the capsule filter B ensures the continuity of the production process.

[0022] 2. The present invention adopts a distillation process to purify nitric oxide to prepare electronic-grade nitric oxide with a purity of 99.9995% or above. A double-tower distillation purification method is adopted, and liquid nitrogen is used as a refrigerant. It can effectively remove water, nitrogen dioxide, nitrous oxide, nitrogen, oxygen and other gaseous impurities in crude nitric oxide prepared by sodium nitrite and dilute sulfuric acid, effectively solving the problem that the traditional adsorbent purification process cannot meet the requirements of large-scale industrial production, and also solving the problem that the adsorbent activation process is cumbersome and complicated. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a diagram of the device structure for electronic grade nitric oxide.

[0024] Figure 2 It is a schematic diagram of the structure of part A of the capsule filter.

[0025] Among them, sulfuric acid storage tank 1, water inlet pipeline 2, reactor 3, liquid phase feed pump 4, capsule filter A5, nitrogen inlet pipeline A-5-1, pipeline A valve two 5-2, capsule filter A valve three 5-3, capsule filter A valve four 5-4, nitrogen output pipeline A valve five 5-5, nitrogen output pipeline A six 5-6, nitrogen entering pipeline B-6-1, pipeline B valve two 6-2, capsule filter B valve three 6-3, capsule filter B valve four 6-4, nitrogen output pipeline B valve five 6-5, nitrogen output pipeline B six 6-6, capsule filter B 6, exhaust pipe vacuum pump 7 first distillation tower 8, heat exchanger one 9, second distillation tower 10, heat exchanger two 11, liquid phase pipeline one 12, exhaust pipe 13, gas phase valve two 14, gas phase feed pump 15, nitrogen valve one 16. DETAILED DESCRIPTION

[0026] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0027] Example 1 Figure 1 Schematic diagram of the device for directly producing electronic grade hydrochloric acid from hydrogen chloride.

[0028] A production device for electronic grade nitric oxide, the production device comprising a sulfuric acid storage tank 1, a reactor 3, a capsule filter A 5, and a capsule filter B 6; The capsule filter A5 is connected in parallel with the top of the capsule filter B6 through a pipeline, and the capsule filter A5 is connected in parallel with the bottom of the capsule filter B6 through a pipeline, so that the capsule filter A5 and the capsule filter B6 can be used interchangeably; The bottom outlet of the reactor 3 is connected to the pipeline connected in parallel with the top of the capsule filter A 5 and the capsule filter B 6 through the liquid phase feed pump 4 to form a circulation pipeline; The pipe 12 connected in parallel at the bottom of the capsule filter A 5 and the capsule filter B 6 is then connected to the lower inlet of the reactor 3 to form a circulation pipeline; The outlet pipeline at the upper end of the reactor 3 is connected to the first distillation tower 8 and the second distillation tower 10, and the electronic grade nitric oxide is extracted from the second distillation tower 10 and filled into a steel cylinder.

[0029] A sulfuric acid storage tank 1 and a water inlet pipe 2 are provided on the top of the reactor 3; Valves are provided on the pipelines connected in parallel at the tops of capsule filter A 5 and capsule filter B 6, namely, valve three 5-3 of capsule filter A and valve three 6-3 of capsule filter B.

[0030] Valves are provided on the liquid phase pipeline 12 connected in parallel at the bottom of capsule filter A 5 and capsule filter B 6, namely valve 4 5-4 of capsule filter A and valve 4 6-4 of capsule filter B; The filter membranes of the capsule filter A 5 and the capsule filter B 6 are made of one of PTFE, ceramic, and 316L metal. In the following examples of the present case, the filter membrane is made of PTFE.

[0031] A nitrogen valve 16 is provided on the top of the reactor 3; a gas phase valve 2 14 is provided on the pipeline from the top of the reactor 3 to the first distillation tower 8, and a gas phase feed pump 15 is provided on the pipeline; The capsule filter A5 and the capsule filter B6 are respectively provided with nitrogen inlet pipes on the top, i.e., nitrogen inlet pipe A-5-1 and nitrogen inlet pipe B-6-1, and valves are respectively provided on the nitrogen inlet pipe A-5-1 and the nitrogen inlet pipe B-6-1, i.e., nitrogen inlet pipe A valve 25-2 and nitrogen inlet pipe B valve 26-2.

[0032] The capsule filter A5 and the capsule filter B6 are respectively provided with nitrogen output pipelines at the bottom, i.e., nitrogen output pipeline A65-6 and nitrogen output pipeline B66-6, and valves are respectively provided on the nitrogen output pipeline A65-6 and nitrogen output pipeline B66-6, i.e., nitrogen output pipeline A valve 55-5 and nitrogen output pipeline B valve 56-5; The nitrogen output pipeline A-5-1 and the nitrogen output pipeline B-6-1 are connected to the evacuation pipe 13 after merging; the bottom of the reactor 3 is connected to the evacuation pipe 13, and the evacuation pipe is provided with an evacuation pipe vacuum pump 7.

[0033] The first distillation tower 8 is connected to the heat exchanger 1 9, and the second distillation tower 10 is connected to the heat exchanger 2 11, and the heat exchanger uses liquid nitrogen as a refrigerant.

[0034] use Figure 1 The production system shown is produced using the following production method: S1: Open the bottom valve of the reactor, start the evacuation pipe vacuum pump 7 to evacuate the reactor, then close the bottom valve, open the nitrogen valve and valves at other parts of the device, purge and replace with nitrogen, and then close the valves at other parts; S2: 138 kg of NaNO2 solid was added to the reactor, the water pipe valve was opened, 150 L of water was added to the reactor, and then the water pipe valve was closed, the sulfuric acid feed line valve was opened, and 98 kg of 60% dilute sulfuric acid was added to the reactor through a sulfuric acid metering pump for reaction; S3: When the pressure of the reactor is greater than 1 bar, open the gas phase valve 2 14 connected to the distillation tower, start the liquid phase feed pump 4, open the capsule filter A valve 3 5-3, the capsule filter A valve 4 5-4 and the reactor bottom valve on the capsule filter A, so that the reactor and the capsule reactor form a cycle, when the pressure difference between the two ends of the capsule reactor A 5 reaches 0.6 MPa, first close the capsule filter A valve 3 5-3, open the capsule filter B valve 3 6-3 and the capsule filter B valve 4 6-4 of the capsule filter B 6, and finally close the capsule filter A valve 4 5-4, open the nitrogen output pipeline A valve 5 5-5, start the emptying pipe vacuum pump 7, evacuate the capsule filter A 5, make the precipitated Na2SO4 supersaturated crystals on the filter screen fall off to the bottom of the capsule filter, empty the Na2SO4 supersaturated crystals through the emptying pipe, and close the valve 5-5; S4: When the pressure difference at both ends of the capsule reactor B 6 reaches 0.6MPa, first close the valve 36-3 of the capsule filter B, open the valve 35-3 of the capsule filter A and the valve 45-4 of the capsule filter A on the capsule filter A 5, and finally close the valve 46-4 of the capsule filter B, open the valve 56-5 of the nitrogen output pipeline B, start the vacuum pump 7 of the emptying pipe, evacuate the capsule filter B 6, make the supersaturated crystals of Na2SO4 precipitated on the filter screen fall off to the bottom of the capsule filter, empty the supersaturated crystals of Na2SO4 through the emptying pipe, close the valve 56-5 of the nitrogen output pipeline B, repeat the S3 operation to switch to the capsule filter A; S5: The nitric oxide gas produced by the reactor enters the first distillation tower and the second distillation tower, and the electronic grade nitric oxide is taken out from the second distillation tower and filled into a steel cylinder; S6: After the reactor no longer produces nitric oxide, switch to the standby reactor to start the S2-S5 reaction process, open the reactor valve, start the evacuation pipe vacuum pump 7, and discharge the reactants in the reactor to the waste liquid tank through the evacuation pipe; In step S6, the number of plates of the first distillation tower is 28, the feed plate position is 20 plates from the bottom, the number of plates of the second distillation tower is 32, the feed plate position is 20 plates from the bottom, the top temperature of the first distillation tower is -109~-107°C, the bottom temperature is -106~-104°C, and the mass reflux ratio of the first distillation tower is 3; the top temperature of the second distillation tower is -136~-134°C, the bottom temperature is -108~-106°C, and the mass reflux ratio of the first distillation tower is 25; The purity of the electronic grade nitric oxide in Example 1 is 99.995%.

[0035] Example 2 The production method is the same as that of Example 1, except that in step S6, the number of plates of the first distillation tower is 30, and the feed plate position is 20 plates from the bottom, the number of plates of the second distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the top temperature of the first distillation tower is -109 to -107°C, the bottom temperature is -106 to -104°C, and the mass reflux ratio of the first distillation tower is 3; the top temperature of the second distillation tower is -136 to -134°C, the bottom temperature is -108 to -106°C, and the mass reflux ratio of the first distillation tower is 25; The purity of the electronic grade nitric oxide in Example 2 is 99.9995%.

[0036] Example 3 The production method is the same as that of Example 1, except that in step S6, the number of plates of the first distillation tower is 30, and the feed plate position is 20 plates from the bottom, the number of plates of the second distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the top temperature of the first distillation tower is -107 to -106°C, the bottom temperature is -104 to -103°C, and the mass reflux ratio of the first distillation tower is 3; the top temperature of the second distillation tower is -136 to -134°C, the bottom temperature is -108 to -106°C, and the mass reflux ratio of the first distillation tower is 25; The purity of the electronic grade nitric oxide in Example 3 is 99.999%.

[0037] Example 4 The production method is the same as that of Example 1, except that in step S6, the number of plates of the first distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the number of plates of the second distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the top temperature of the first distillation tower is -109 to -107°C, the bottom temperature is -106 to -104°C, and the mass reflux ratio of the first distillation tower is 3; the top temperature of the second distillation tower is -132 to -130°C, the bottom temperature is -106 to -105°C, and the mass reflux ratio of the first distillation tower is 25; The purity of the electronic grade nitric oxide in Example 4 is 99.99%.

[0038] Example 5 The production method is the same as that of Example 1, except that in step S6, the number of plates of the first distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the number of plates of the second distillation tower is 30, and the feed plate position is the 20th plate from the bottom, the top temperature of the first distillation tower is -109 to -107°C, the bottom temperature is -106 to -104°C, and the mass reflux ratio of the first distillation tower is 4; the top temperature of the second distillation tower is -136 to -134°C, the bottom temperature is -108 to -106°C, and the mass reflux ratio of the first distillation tower is 22; The purity of the electronic grade nitric oxide in Example 5 is 99.995%.

[0039] The above-mentioned embodiments are only preferred technical solutions of the present invention and should not be regarded as limitations of the present invention. The embodiments and features in the embodiments of the present application can be arbitrarily combined with each other without conflict. The protection scope of the present invention shall be the technical solutions recorded in the claims, including the equivalent replacement solutions of the technical features in the technical solutions recorded in the claims. That is, equivalent replacement improvements within this scope are also within the protection scope of the present invention.

Claims

1. A production device for electronic grade nitric oxide, characterized in that: The production device comprises a sulfuric acid storage tank (1), a reactor (3), a capsule filter A (5), and a capsule filter B (6); The capsule filter A (5) and the capsule filter B (6) are connected in parallel at the top through a pipe, and the capsule filter A (5) and the capsule filter B (6) are connected in parallel at the bottom through a pipe, so that the capsule filter A (5) and the capsule filter B (6) can be used interchangeably; The bottom outlet of the reactor (3) is connected to the pipeline connected in parallel to the tops of the capsule filter A (5) and the capsule filter B (6) via a liquid phase feed pump (4) to form a circulation pipeline; The pipe (12) connected in parallel at the bottom of the capsule filter A (5) and the capsule filter B (6) is then connected to the lower inlet of the reactor (3) to form a circulation pipeline; The outlet pipeline at the upper end of the reactor (3) is connected to the first distillation tower (8) and the second distillation tower (10), and electronic grade nitric oxide is extracted from the second distillation tower (10) and filled into a steel cylinder.

2. The production device of electronic grade nitric oxide according to claim 1, characterized in that: A sulfuric acid storage tank (1) and a water inlet pipe (2) are provided on the top of the reactor (3); Valves are provided on the pipes connected in parallel at the tops of the capsule filters A (5) and B (6), namely, valve three (5-3) of capsule filter A and valve three (6-3) of capsule filter B.

3. The production device of electronic grade nitric oxide according to claim 1, characterized in that: Valves are provided on the liquid phase pipeline one (12) connected in parallel at the bottom of the capsule filter A (5) and the capsule filter B (6), namely, valve four (5-4) of the capsule filter A and valve four (6-4) of the capsule filter B; The filter membranes of the capsule filter (5) A and the capsule filter B (6) are made of one of PTFE, ceramic, and 316L metal.

4. The production device of electronic grade nitric oxide according to claim 1, characterized in that: A nitrogen valve 1 (16) is provided at the top of the reactor (3); a gas phase valve 2 (14) is provided on the pipeline from the top of the reactor (3) to the first distillation tower (8), and a gas phase feed pump (15) is provided on the pipeline; The capsule filter A (5) and the capsule filter B (6) are respectively provided with nitrogen inlet pipes at the top, i.e., nitrogen inlet pipe A-1 (5-1) and nitrogen inlet pipe B-1 (6-1), and the nitrogen inlet pipe A-1 (5-1) and the nitrogen inlet pipe B-1 (6-1) are respectively provided with valves, i.e., nitrogen inlet pipe A valve 2 (5-2) and nitrogen inlet pipe B valve 2 (6-2).

5. The production device of electronic grade nitric oxide according to claim 4, characterized in that: The capsule filter A (5) and the capsule filter B (6) are respectively provided with nitrogen output pipelines at the bottom, namely, nitrogen output pipeline A six (5-6) and nitrogen output pipeline B six (6-6), and the nitrogen output pipeline A six (5-6) and the nitrogen output pipeline B six (6-6) are respectively provided with valves, namely, nitrogen output pipeline A valve five (5-5) and nitrogen output pipeline B valve five (6-5); The nitrogen output pipeline A-(5-1) and the nitrogen output pipeline B-(6-1) are connected to the evacuation pipe (13) after merging; the bottom of the reactor (3) is connected to the evacuation pipe (13), and the evacuation pipe is provided with an evacuation pipe vacuum pump (7).

6. The production device of electronic grade nitric oxide according to claim 1, characterized in that: The first distillation tower (8) is connected to the first heat exchanger (9), and the second distillation tower (10) is connected to the second heat exchanger (11), and the heat exchangers use liquid nitrogen as a refrigerant.

7. A method for producing electronic grade nitric oxide, characterized in that The production method is implemented by using the production device of electronic grade nitric oxide according to any one of claims 1 to 5, and the production method comprises the following steps: S1: After evacuating all components in the production device for electronic grade nitric oxide, the entire production device is purged with nitrogen; S2: Add NaNO2 solid into the reactor, add water and then add dilute sulfuric acid into the reactor to react; S3: When the pressure in the reactor is constant, open the gas phase valve 2 (14) connected to the distillation tower, start the liquid phase feed pump (4), open the capsule filter A valve 3 (5-3) and the capsule filter A valve 4 (5-4) on the capsule filter A (5), so that the reactor and the capsule reactor A (5) form a circulation, and a pressure difference is formed at both ends of the capsule reactor A (5), first close the capsule filter A valve 3 (5-3) and open the capsule filter B valve 3 (6-3) and the capsule filter B valve 4 (6-4) on the capsule filter B (6), and finally close the capsule filter A valve 4 (5-4), open the nitrogen output pipeline A valve 5 (5-5), start the emptying pipe vacuum pump (7), evacuate the capsule filter A (5), make the supersaturated Na2SO4 crystals precipitated on the filter screen fall off to the bottom of the capsule filter, empty the Na2SO4 supersaturated crystals through the emptying pipe, and close the nitrogen output pipeline A valve 5 (5-5); S4: When a pressure difference is achieved at both ends of the capsule reactor B (6), first close the valve three (6-3) of the capsule filter B, open the valve three (5-3) and valve four (5-4) of the capsule filter A on the capsule filter A (5), and finally close the valve four (6-4) of the capsule filter B, open the valve five (6-5) of the nitrogen output pipeline B, start the vacuum pump (7) of the exhaust pipe, evacuate the capsule filter B (6), and make the supersaturated crystals of Na2SO4 precipitated on the filter screen fall off to the bottom of the capsule filter, exhaust the supersaturated crystals of Na2SO4 through the exhaust pipe, close the valve five (6-5) of the nitrogen output pipeline B, and repeat the S3 operation to switch to the capsule filter A; S5: The nitric oxide gas produced by the reactor enters the first distillation tower and the second distillation tower in sequence, and the electronic grade nitric oxide is taken out from the second distillation tower and filled into a steel cylinder; S6: After the reactor no longer produces nitric oxide, switch to reactor (3) and start the S2-S5 reaction process.

8. The method for producing electronic grade nitric oxide according to claim 1, characterized in that: In S1, the mass ratio of NaNO2 solid, water and dilute sulfuric acid is: 1-1.5: 1.5-2: 0.5-1.5; the mass concentration of the dilute sulfuric acid is 50-70%.

9. The method for producing electronic grade nitric oxide according to claim 1, characterized in that: The pressure difference obtained in S2 and S3 is 0.4-1.0 MPa, and more preferably the pressure difference is 0.5-0.8 MPa.

10. The method for producing electronic grade nitric oxide according to any one of claims 6 to 9, characterized in that: The number of plates of the first distillation tower is 25 to 40, and the feed plate is located at the 18th to 22nd plate from the bottom.

11. The method for producing electronic grade nitric oxide according to any one of claims 6 to 9, characterized in that: The number of plates of the second distillation tower is 28 to 40, and the feed plates are located at the 18th to 22nd plates from the bottom.

12. The method for producing electronic grade nitric oxide according to claim 6, characterized in that: The top temperature of the first distillation tower is -115~-105°C, the bottom temperature is -108~-100°C, and the mass reflux ratio of the first distillation tower is 1.5~5.

13. The production method according to claim 6, characterized in that: The top temperature of the second distillation tower is -140~-128°C, the bottom temperature is -110~-100°C, and the mass reflux ratio of the first distillation tower is 20~35.