CN216747020U

CN216747020U - Sampling device for nitrogen trifluoride electrolytic cell

Info

Publication number: CN216747020U
Application number: CN202220236269.XU
Authority: CN
Inventors: 曲昆; 毕伟革; 王鹏飞; 赵金旭; 曹娅妮; 宫磊; 王杰
Original assignee: Wulancha Bunanda Microelectronic Materials Co ltd
Current assignee: Nanda Optoelectronics Ulanqab Co ltd
Priority date: 2022-01-28
Filing date: 2022-01-28
Publication date: 2022-06-14
Anticipated expiration: 2032-01-28

Abstract

The utility model belongs to the technical field of process gas sampling, and relates to a sampling device of a nitrogen trifluoride electrolytic cell, which is connected to the nitrogen trifluoride electrolytic cell and comprises a fine sampling unit, wherein a filtering unit is arranged between the fine sampling unit and the nitrogen trifluoride electrolytic cell and is communicated with the nitrogen trifluoride electrolytic cell through an exhaust pipe; the gas inlet of the fine sampling unit is communicated with the gas outlet of the filtering unit, the gas outlet of the fine sampling unit is communicated with the gas extraction port of the vacuum pump, and the gas outlet of the vacuum pump is communicated with the nitrogen trifluoride electrolytic bath through a gas return pipe; the fine sampling unit comprises a gas storage box, two ends of the gas storage box are communicated with the filtering unit and the vacuum pump respectively, the gas storage box is communicated with one end of the sampling tube, the other end of the sampling tube is communicated with a first negative pressure bag, and the sampling tube is provided with a flowmeter and a sampling valve. The utility model can complete sampling work timely and accurately, effectively ensure that the sampling detection result has reference value, and reduce the risk of generating economic loss.

Description

Sampling device of nitrogen trifluoride electrolytic cell

Technical Field

The utility model relates to a sampling device for a nitrogen trifluoride electrolytic cell, and belongs to the technical field of process gas sampling.

Background

In the electrolytic process of producing nitrogen trifluoride, the generated gas is a key point of process control, the electrolytic cell is a closed system, the timeliness and the accuracy of sampling are key factors influencing the product quality, if the sampling is not timely and inaccurate, the detection structure has no representativeness and referential property, the difficulty of subsequent process treatment is increased, and huge economic loss is possibly caused; the sampling device used at present still has the problems of inaccurate sampling and the like.

SUMMERY OF THE UTILITY MODEL

The technical problem to be solved by the utility model is as follows: the utility model provides a nitrogen trifluoride electrolysis trough sampling device, completion sample work that can be timely and accurate, effectual assurance sample testing result has reference value, has reduced the risk that produces economic loss.

The sampling device of the nitrogen trifluoride electrolytic cell is connected to the nitrogen trifluoride electrolytic cell and comprises a fine sampling unit, wherein a filtering unit is arranged between the fine sampling unit and the nitrogen trifluoride electrolytic cell and is communicated with the nitrogen trifluoride electrolytic cell through an exhaust tube; the gas inlet of the fine sampling unit is communicated with the gas outlet of the filtering unit, the gas outlet of the fine sampling unit is communicated with the gas extraction port of the vacuum pump, and the gas outlet of the vacuum pump is communicated with the nitrogen trifluoride electrolytic bath through a gas return pipe; the fine sampling unit comprises a gas storage box, two ends of the gas storage box are communicated with the filtering unit and the vacuum pump respectively, the gas storage box is communicated with one end of the sampling tube, the other end of the sampling tube is communicated with a first negative pressure bag, and the sampling tube is provided with a flowmeter and a sampling valve.

In the course of the work, at first the sampling valve is the closed condition, under the effect of vacuum pump, the gas that is taken out by nitrogen trifluoride electrolysis trough is at first through the filtration absorption of filter unit, then get into the gas holder, get into the nitrogen trifluoride electrolysis trough again through vacuum pump and muffler after the gas holder is kept in, after this circulation operation a period, the gas that the gas holder was kept in is comparatively close the actual gas in the nitrogen trifluoride electrolysis trough, the sample then can be comparatively accurate this moment, open the sampling valve this moment, gas in the gas holder gets into in the negative pressure bag one, the accurate measurement of flowmeter simultaneously, when reaching the measurement requirement, the flowmeter is with signal transmission to the control unit, the control unit control sampling valve is closed, the accurate sample of ration has been realized, effectual assurance sample testing result has the reference value, the risk of producing economic loss has been reduced. The first negative pressure bag is connected with the sampling tube through a quick connector, and the first negative pressure bag is convenient to disassemble and assemble.

Preferably, the exhaust tube is connected with a coarse sampling unit, the coarse sampling unit comprises a middle tube, one end of the middle tube is communicated with the exhaust tube, the other end of the middle tube is communicated with a second negative pressure bag, and the middle tube is provided with a middle valve. The gas of the coarse sampling in the negative pressure bag II is detected, the detection result of the gas is compared with the detection result of the sampling gas in the negative pressure bag I, the removal efficiency of the filtering unit can be determined, whether the filtering unit is saturated or not is judged, the filtering substances in the filtering unit can be replaced in time, and the accuracy of sampling detection can be influenced if the filtering unit is saturated.

Preferably, the filtering unit comprises a potassium hydroxide column, a first drying column and a particle impurity adsorption column which are connected in series from front to back. The first drying column can be selected from anhydrous sodium sulfate, molecular sieves and the like; the potassium hydroxide column is used for removing hydrogen fluoride in the gas, the drying column I is used for removing moisture in the gas, and the particle impurity adsorption column is used for removing tiny particles in the gas.

Preferably, a second drying column is additionally arranged between the exhaust port of the vacuum pump and the nitrogen trifluoride electrolytic cell, anhydrous sodium sulfate, a molecular sieve and the like can be selected as the second drying column, so that the gas entering the nitrogen trifluoride electrolytic cell after passing through the vacuum pump is always dry, and the environment in the nitrogen trifluoride electrolytic cell is not greatly influenced.

Preferably, pipelines at two ends of the gas storage box are respectively provided with a first cut-off valve and a second cut-off valve, and during sampling, the first cut-off valve and the second cut-off valve are closed, so that the gas environment in the gas storage box is in a stable state, and the sampling accuracy is further ensured.

Compared with the prior art, the utility model has the beneficial effects that:

the utility model has reasonable structural design, can timely and accurately finish sampling work, effectively ensures that the sampling detection result has reference value, and reduces the risk of generating economic loss.

Drawings

FIG. 1 is a schematic view of a sampling apparatus of a nitrogen trifluoride electrolyzer.

In the figure: 1. a nitrogen trifluoride electrolytic cell; 2. an air return pipe; 3. an air return valve; 4. an air extraction valve; 5. an intermediate pipe; 6. an air exhaust pipe; 7. drying the column II; 8. a particulate impurity adsorption column; 9. a vacuum pump; 10. a gas storage tank; 11. a second block valve; 12. a sampling valve; 13. a flow meter; 14. a first negative pressure bag; 15. a first block valve; 16. drying the first column; 17. a potassium hydroxide column; 18. a second negative pressure bag; 19. an intermediate valve; 20. and a sampling tube.

Detailed Description

The utility model is further described below with reference to the accompanying drawings:

referring to fig. 1, the sampling device of the nitrogen trifluoride electrolyzer 1 of the utility model is connected to the nitrogen trifluoride electrolyzer 1 and comprises a fine sampling unit, a filtering unit is arranged between the fine sampling unit and the nitrogen trifluoride electrolyzer 1, and the filtering unit is communicated with the nitrogen trifluoride electrolyzer 1 through an air suction pipe 6; the gas inlet of the fine sampling unit is communicated with the gas outlet of the filtering unit, the gas outlet of the fine sampling unit is communicated with the gas extraction port of the vacuum pump 9, and the gas outlet of the vacuum pump 9 is communicated with the nitrogen trifluoride electrolytic bath 1 through the gas return pipe 2; the fine sampling unit comprises a gas storage box 10, two ends of the gas storage box 10 are respectively communicated with the filtering unit and the vacuum pump 9, the gas storage box 10 is communicated with one end of a sampling tube 20, the other end of the sampling tube 20 is communicated with a first negative pressure bag 14, and a flow meter 13 and a sampling valve 12 are arranged on the sampling tube 20.

In this embodiment:

the exhaust tube 6 is connected with a coarse sampling unit, the coarse sampling unit comprises a middle tube 5, one end of the middle tube 5 is communicated with the exhaust tube 6, the other end of the middle tube 5 is communicated with a second negative pressure bag 18, and a middle valve 19 is arranged on the middle tube 5. The gas roughly sampled in the second negative pressure bag 18 is detected, the detection result of the gas is compared with the detection result of the gas sampled in the first negative pressure bag 14, the removal efficiency of the filter unit can be determined, whether the filter unit is saturated or not can be judged, the filter substances in the filter unit can be replaced in time, and the accuracy of sampling detection can be influenced if the filter unit is saturated.

The filtering unit comprises a potassium hydroxide column 17, a first drying column 16 and a particle impurity adsorption column 8 which are connected in series. The first drying column 16 can be selected from anhydrous sodium sulfate, molecular sieves and the like; the potassium hydroxide column 17 is used for removing hydrogen fluoride in the gas, the first drying column 16 is used for removing moisture in the gas, and the particle impurity adsorption column 8 is used for removing micro particles in the gas.

A second drying column 7 is additionally arranged between an exhaust port of the vacuum pump 9 and the nitrogen trifluoride electrolytic cell 1, anhydrous sodium sulfate, a molecular sieve and the like can be selected for the second drying column 7, so that the gas entering the nitrogen trifluoride electrolytic cell 1 through the vacuum pump 9 is always dry, and the environment in the nitrogen trifluoride electrolytic cell 1 cannot be greatly influenced.

The pipeline at the two ends of the gas storage box 10 is respectively provided with the first block valve 15 and the second block valve 11, and during sampling, the first block valve 15 and the second block valve 11 are closed, so that the gas environment in the gas storage box 10 is in a stable state, and the sampling accuracy is further ensured.

In the working process, the sampling valve 12 is closed, the gas pumped out from the nitrogen trifluoride electrolytic tank 1 is filtered and absorbed by the filtering unit under the action of the vacuum pump 9, then enters a gas storage tank 10, enters a nitrogen trifluoride electrolytic tank 1 again through a vacuum pump 9 and a gas return pipe 2 after being temporarily stored in the gas storage tank 10, after the circulation is operated for a period of time, the gas temporarily stored in the gas storage box 10 is closer to the actual gas in the nitrogen trifluoride electrolytic cell 1, the sampling is more accurate, the sampling valve 12 is opened, the gas in the gas storage box 10 enters the first negative pressure bag 14, meanwhile, the flowmeter 13 measures accurately, when the measurement requirement is met, the flowmeter 13 transmits signals to the control unit, and the control unit controls the sampling valve 12 to be closed, so that quantitative accurate sampling is realized, the sampling detection result is effectively guaranteed to have a reference value, and the risk of generating economic loss is reduced. The first negative pressure bag 14 is connected with the sampling tube 20 through a quick connector, and the disassembly and the assembly are both convenient. The materials of the pipelines, the accessories and the like can be selected from polytetrafluoroethylene and the like, and the pipelines, the accessories and the like are corrosion-resistant. The air exhaust pipe 6 and the air return pipe 2 are respectively provided with an air exhaust valve 4 and an air return valve 3.

Claims

1. A nitrogen trifluoride electrolytic cell sampling device is connected to a nitrogen trifluoride electrolytic cell (1), and is characterized in that: the device comprises a fine sampling unit, wherein a filtering unit is arranged between the fine sampling unit and a nitrogen trifluoride electrolytic bath (1), and the filtering unit is communicated with the nitrogen trifluoride electrolytic bath (1) through an exhaust pipe (6); the gas inlet of the fine sampling unit is communicated with the gas outlet of the filtering unit, the gas outlet of the fine sampling unit is communicated with the gas extraction port of the vacuum pump (9), and the gas outlet of the vacuum pump (9) is communicated with the nitrogen trifluoride electrolytic bath (1) through the gas return pipe (2); the fine sampling unit comprises a gas storage box (10), two ends of the gas storage box (10) are communicated with the filtering unit and the vacuum pump (9) respectively, the gas storage box (10) is communicated with one end of the sampling pipe (20), the other end of the sampling pipe (20) is communicated with a first negative pressure bag (14), and a flow meter (13) and a sampling valve (12) are arranged on the sampling pipe (20).

2. Nitrogen trifluoride cell sampling device according to claim 1, characterized in that: the air exhaust pipe (6) is connected with a coarse sampling unit, the coarse sampling unit comprises a middle pipe (5), one end of the middle pipe (5) is communicated with the air exhaust pipe (6), the other end of the middle pipe is communicated with a second negative pressure bag (18), and a middle valve (19) is arranged on the middle pipe (5).

3. Nitrogen trifluoride cell sampling device according to claim 1, characterized in that: the filtering unit comprises a potassium hydroxide column (17), a drying column I (16) and a particle impurity adsorption column (8) which are connected in series from front to back.

4. Nitrogen trifluoride cell sampling device according to claim 1, characterized in that: a second drying column (7) is additionally arranged between the exhaust port of the vacuum pump (9) and the nitrogen trifluoride electrolytic tank (1).

5. Nitrogen trifluoride cell sampling device according to claim 1, characterized in that: pipelines at two ends of the gas storage box (10) are respectively provided with a first cut-off valve (15) and a second cut-off valve (11).