CN111118519A - Electrolytic system for preparing arsine by electrolytic method - Google Patents
Electrolytic system for preparing arsine by electrolytic method Download PDFInfo
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- CN111118519A CN111118519A CN201811279617.6A CN201811279617A CN111118519A CN 111118519 A CN111118519 A CN 111118519A CN 201811279617 A CN201811279617 A CN 201811279617A CN 111118519 A CN111118519 A CN 111118519A
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The invention provides an electrolysis system for preparing arsine by an electrolysis method. The electrolysis system comprises: an electrolytic cell having a cathode chamber and an anode chamber separated by an ionic semipermeable membrane, the cathode chamber electrolyzing to produce arsine and hydrogen, the anode chamber electrolyzing to produce oxygen; the cathode gas conveying pipeline is connected with the cathode chamber; an anode gas delivery pipeline connected with the anode chamber; a first differential pressure sensor is disposed between the cathode gas delivery line and the anode gas delivery line to monitor a differential pressure between the anode chamber and the cathode chamber. Utilize the pressure differential of first differential pressure sensor monitoring anode chamber and cathode chamber, adjust the gas pressure in anode chamber and/or the cathode chamber when the too big exceedes of pressure differential is injectd, for example through adjustment gas flow rate, voltage size etc. to avoid the too big damage to the ion semipermeable membrane of pressure differential, and then guaranteed that the cathode chamber generates and the gas quality that flows out is stable, need not carry out deep purification and guaranteed that follow-up application is gas flow's stability, and then guaranteed the safe and stable operation of system.
Description
Technical Field
The invention relates to the field of electronic gas preparation, in particular to an electrolysis system for preparing arsine by an electrolysis method.
Background
Nowadays, the technology of electronic gases such as arsine is more and more widely used in the semiconductor industry, the solar energy industry, the LED industry, the flat panel display industry and the optical fiber industry. Electronic gases are generally toxic gases, flammable and explosive gases, and the impurity removal and purification process is a great problem. The method for preparing the arsine by the electrolysis method directly adopts high-purity metal arsenic or a high-purity arsenic-containing raw material, can reduce the introduction of impurities from the raw material, and greatly simplifies the purification process of the arsine, so the method for preparing the arsine by the electrolysis method is a better way for solving the problem of gas supply in the future.
The electrolytic cell for producing arsine by electrolysis has various arrangements, and the following description will take arsenic oxide as an example of a cathode. The electrolytic cell is provided with a cathode chamber and an anode chamber, an anode of an electrolytic electrode and an anolyte are arranged in the anode chamber, the anolyte is pure water, a small amount of high-purity NaOH is added to be used as a conductive electrolyte, and the NaOH does not participate in electrolytic reaction. Reaction equation of anodic electrolysis reaction:
6H2O→3O2(g)+12e-+12H+
a cathode in the cathode chamber and provided with an electrolytic electrode, and a cathode electrolyte which is trivalent arsenic As2O3The aqueous solution can also be used as pentavalent arsenic aqueous solution, and small amount of high purity H is added2SO4As a conductive electrolyte, H2SO4Does not participate in the electrolytic reaction.
As2O3(s)+12H++12e-→2AsH3+3H2O
The electrolysis power supply is responsible for providing voltage to the cathode and the anode of the electrolysis electrodeAnd current to control the production of electrolytic arsine gas. An ion semipermeable membrane is designed between the cathode chamber and the anode chamber to allow positive ions H+From the anode chamber to the cathode chamber, other ions and molecules cannot permeate. The ion semipermeable membrane is a membrane with the thickness of only 50-100 microns, and can be directly blown through when the pressure between the cathode chamber and the anode chamber is too high. Even a small range of pressure causes repeated expansion and contraction of the ion semipermeable membrane between the cathode chamber and the anode chamber, and is easily broken by fatigue, and if a sharp protrusion or burr is encountered inside the cathode chamber or the anode chamber, the ion semipermeable membrane is easily broken, so that the catholyte and the anolyte are mixed, or gas generated by electrolysis of the anode chamber and the cathode chamber is mixed. Therefore, the arsine gas generated by cathode electrolysis is doped with oxygen and can be used only after the oxygen is deeply removed to be below 20ppb, so that the basic purpose of preparing arsine by using an electrolysis method is lost, the production period of the arsine gas is prolonged, and the price advantage of preparing electronic gas by using an electrolyte is also lost.
Therefore, the problem of the electrolytic method for preparing arsine is how to ensure that the gas with stable flow and quality of arsine can be obtained and the safety and reliability of the whole electrolytic system are ensured. The problem is a difficult problem to be solved in the engineering of the arsenic alkane preparation by the electrolysis method, the problem is not solved, and the engineering application is not mentioned.
Disclosure of Invention
The invention mainly aims to provide an electrolysis system for preparing arsine by electrolysis, which is used for solving the problem of unstable flow of arsine gas in the process of preparing arsine by electrolysis in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided an electrolysis system for producing arsine by electrolysis, the electrolysis system comprising: an electrolytic cell having a cathode chamber and an anode chamber separated by an ionic semipermeable membrane, the cathode chamber electrolyzing to produce arsine and hydrogen, the anode chamber electrolyzing to produce oxygen; the cathode gas conveying pipeline is connected with the cathode chamber; an anode gas delivery pipeline connected with the anode chamber; a first differential pressure sensor is disposed between the cathode gas delivery line and the anode gas delivery line to monitor a differential pressure between the anode chamber and the cathode chamber.
Furthermore, a first automatic pressure controller is arranged on the cathode gas conveying pipeline, and the first automatic pressure controller is electrically connected with the first differential pressure sensor and used for receiving a signal of the first differential pressure sensor to adjust the differential pressure between the cathode chamber and the anode chamber.
Further, the cathode gas delivery pipe is provided with a first pressure sensor.
Further, the cathode gas delivery pipeline is also provided with a first pressure switch.
Further, a second pressure sensor is provided in the anode gas transport line.
Furthermore, a second pressure switch is arranged on the anode gas conveying pipeline.
Furthermore, the electrolysis system further comprises a cathode gas conveying branch pipe, the cathode gas conveying branch pipe is connected with the cathode gas conveying pipeline, and a first pressure release valve is arranged on the cathode gas conveying branch pipe.
Furthermore, the electrolysis system further comprises an anode gas delivery branch pipe, the anode gas delivery branch pipe is connected with the anode gas delivery pipeline, and a second pressure release valve is arranged on the anode gas delivery branch pipe.
Furthermore, the electrolysis system further comprises a cathode tail gas treatment device, wherein the cathode tail gas treatment device is connected with the cathode gas conveying pipeline and is arranged at the tail end of the cathode gas conveying pipeline.
Furthermore, the electrolysis system further comprises an anode tail gas treatment device, wherein the anode tail gas treatment device is connected with the anode gas conveying pipeline and is arranged at the tail end of the anode gas conveying pipeline.
The technical scheme of the invention has the following beneficial effects:
be provided with first differential pressure sensor between cathode gas conveying line and anode gas conveying line in order to monitor the pressure differential of anode chamber and cathode chamber, adjust anode chamber and/or the interior gas pressure of cathode chamber when the too big exceedes of pressure differential is injectd, for example through adjustment gas flow rate, voltage size etc. to avoid the too big damage to ion semi-permeable membrane of pressure differential, and then guaranteed that the cathode chamber generates and the gas quality that flows is stable, need not carry out the stability that the follow-up application is gas flow, and then guaranteed the safe and stable operation of system.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic diagram of an electrolysis system provided in accordance with an embodiment of the present invention.
Wherein the figures include the following reference numerals:
11. a cathode chamber; 12. an ionic semipermeable membrane; 13. an anode chamber; 14. a power source;
20. a first differential pressure sensor;
30. a cathode gas delivery line; 31. a first pressure sensor; 32. a first pressure switch; 33. a first automatic pressure controller;
40. an anode gas delivery line; 41. a second pressure sensor; 42. a second pressure switch; 43. a variable frequency fan;
50. a cathode gas delivery manifold; 51. a first pressure relief valve;
60. an anode gas delivery manifold; 61. a second pressure relief valve.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As analyzed by the background technology of the application, the differential pressure of the anode chamber and the cathode chamber in the prior art is unstable, when the pressure between the cathode chamber and the anode chamber is too large, the ion semipermeable membrane can be directly blown open, or the repeated expansion and contraction of the ion semipermeable membrane between the cathode chamber and the anode chamber can be easily broken due to fatigue caused by the fluctuation of the differential pressure within a small range, so that the gas mixing of the cathode chamber and the anode chamber is caused, the quality of arsine in the gas flowing out from the cathode chamber is unstable, the arsine can be utilized only by further deep purification, and the preparation cost of the arsine is increased. In order to solve the problem, the application provides an electrolytic system for preparing arsine by an electrolytic method.
In an exemplary embodiment of the present application, an electrolysis system for producing arsine electrolytically, as shown in fig. 1, includes an electrolysis cell having a cathode chamber 11 and an anode chamber 13 separated by an ionic semipermeable membrane 12, the cathode chamber 11 electrolytically producing arsine and hydrogen, and the anode chamber 13 electrolytically producing oxygen; the cathode gas conveying pipeline 30 is connected with the cathode chamber 11; an anode gas delivery line 40 is connected to the anode chamber 13; a first differential pressure sensor 20 is provided between the cathode gas delivery line 30 and the anode gas delivery line 40 to monitor the differential pressure between the anode chamber 13 and the cathode chamber 11.
Be provided with first differential pressure sensor 20 between cathode gas conveying line 30 and anode gas conveying line 40 in order to monitor the pressure differential of anode chamber 13 and cathode chamber 11, adjust the interior gas pressure of anode chamber 13 and/or cathode chamber 11 when the pressure differential is too big to exceed the limited, for example through adjusting adjustment gas flow rate, voltage size etc. to avoid the too big damage to ion semi-permeable membrane 12 of pressure differential, and then guaranteed that cathode chamber 11 generates and the gas quality that flows out is stable, need not carry out the stability that deep purification has guaranteed that follow-up application is gas flow, and then guaranteed the safe and stable operation of system.
When the above differential pressure is too large to exceed the limit, the flow rate of the gas, the magnitude of the voltage, and the like may be manually adjusted, and in order to improve the degree of automation of the system operation, it is preferable that, as shown in fig. 1, the cathode gas delivery line 30 is provided with a first automatic pressure controller 33, and the first automatic pressure controller 33 is electrically connected to the first differential pressure sensor 20 to receive a signal from the first differential pressure sensor 20 to adjust the differential pressure between the cathode chamber 11 and the anode chamber 13. The first automatic pressure controller 33 is electrically connected to the first differential pressure sensor 20, and after receiving the signal from the first differential pressure sensor 20, the first automatic pressure controller 33 adjusts the temperature of the cathode chamber 11 by adjusting the flow rate of the gas in the cathode gas delivery pipeline 30, thereby controlling the differential pressure between the cathode chamber 11 and the anode chamber 13 within a safe range. The positional relationship between the first differential pressure sensor 20 and the first automatic pressure controller 33 may be various, and it is preferable that the interface between the first differential pressure sensor 20 and the cathode gas supply line 30 is a first interface, and the first automatic pressure controller 33 is provided downstream of the first interface.
In a preferred embodiment of the present invention, as shown in fig. 1, the cathode chamber 11 is provided with a first pressure sensor 31, and the pressure change in the cathode chamber 11 is monitored by the first pressure sensor 31, and the electrolysis rate, gas flow, and the like are determined according to the pressure change, thereby ensuring the safe operation of the electrolysis system. Preferably, the electrolysis system also has a safety control unit, to which the first pressure sensor 31 is electrically connected. And transmitting the monitoring result of the first pressure sensor 31 to a safety control unit, and making corresponding action by the safety control unit according to the monitoring result. For example, when the pressure fluctuation of the cathode chamber 11 is detected to be large, the control unit sends out graded alarm signals, and when the staff receives the low-grade alarm signals, the staff checks each operation structure of the electrolytic cell of the electrolytic system, if the alarm can be eliminated by adjusting the voltage or the airflow, the staff adjusts accordingly, and the shutdown control is performed once the danger is found. If the safety control unit sends out a high-level alarm signal, the equipment automatically starts a shutdown program to protect the safety of the equipment and operators.
In order to avoid safety problems caused by insufficient pressure monitoring, it is preferable that the cathode gas delivery line 30 is further provided with a first pressure switch 32 as shown in fig. 1, since the sensitivity of the operation of the first differential pressure sensor 20, the first automatic pressure controller 33, and the like is reduced even if the operation of the electrolysis system is not detected by the operator after a long time. The cathode chamber 11 pressure is monitored using a first pressure switch 32 and power-off protection is performed when the monitored pressure exceeds a preset value.
In order to automatically control the pressure in the cathode chamber 11 by providing the first automatic pressure controller 33 on the cathode gas conveying pipeline 30, and also to automatically control the pressure in the anode chamber 13, it is preferable that, as shown in fig. 1, the anode gas conveying pipeline 40 is provided with a variable frequency fan 43, and the variable frequency fan 43 is electrically connected to the first differential pressure sensor 20 for receiving a signal from the first differential pressure sensor 20 to adjust the differential pressure between the cathode chamber 11 and the anode chamber 13. The interface of the first differential pressure sensor 20 and the anode gas delivery line 40 is a second interface, and the variable frequency fan 43 is disposed downstream of the second interface.
Even if the gas composition generated by the anode has little influence on the application of arsine, in order to avoid unstable system operation caused by too large pressure fluctuation of the anode chamber 13, it is preferable that, as shown in fig. 1, a second pressure sensor 41 is arranged on the anode gas conveying pipeline 40, the pressure change of the anode chamber 13 is monitored by using the second pressure sensor 41, and the conditions such as the electrolysis rate and the gas flow are judged according to the pressure change condition, so as to ensure the safe operation of the electrolysis system. Preferably, the second pressure sensor 41 is electrically connected to the safety control unit. The monitoring result of the second pressure sensor 41 is transmitted to the safety control unit, and the safety control unit performs corresponding action according to the monitoring result. For example, when it is detected that the pressure fluctuation of the anode chamber 13 is large, the safety control unit sends an alarm signal, and the worker checks each operation structure of the electrolytic cell of the electrolytic system when receiving the alarm signal, and if the alarm can be eliminated by adjusting the voltage or the air flow, the worker adjusts accordingly, and stops the electrolytic system when finding a danger.
In order to avoid safety problems caused by insufficient pressure monitoring, it is preferable that the anode gas delivery line 40 is further provided with a second pressure switch 42, as shown in fig. 1, since the sensitivity of the second pressure sensor 41, the first automatic pressure controller 33, and the like is decreased even if the electrolytic system fails to be detected by the operator after a long time operation. The cathode chamber 11 pressure is monitored using a first pressure switch 32 and power-off protection is performed when the monitored pressure exceeds a preset value.
Since arsine is a toxic gas, it is preferable to ensure safety, as shown in fig. 1, that the electrolysis system further includes a cathode tail gas treatment device, which is connected to the cathode gas conveying pipeline 30 and disposed at the end of the cathode gas conveying pipeline 30, and the cathode tail gas treatment device may be a cathode dry tail gas treatment device 70, where the cathode dry tail gas treatment device 70 has a first tail gas inlet, the first tail gas inlet is connected to the cathode gas conveying pipeline 30, and the cathode dry tail gas treatment device 70 is disposed at the end of the cathode gas conveying pipeline 30, and the cathode dry tail gas treatment device 70 is used to treat the cathode gas to meet the emission requirement.
In addition, when the pressure sensors or the pressure switches fail (the occurrence probability is low), in order to ensure the safety of the electrolysis system, it is preferable that the electrolysis system further includes a cathode gas delivery branch 50, as shown in fig. 1, the cathode gas delivery branch 50 is connected to the cathode gas delivery pipeline 30, and the cathode gas delivery branch 50 is provided with a first pressure relief valve 51. When the pressure in the cathode chamber 11 is too high, the first pressure relief valve 51 is opened to relieve the pressure, so that the cathode chamber 11 in the electrolytic cell is not overpressurized. Preferably, the cathode dry-type tail gas processing device 70 further has a second tail gas inlet, and the second tail gas inlet is connected to the cathode gas conveying pipeline 30 through the cathode gas conveying branch pipe 50. The gas released during pressure relief is sent to the cathode dry-type tail gas treatment device 70 for treatment.
In order to avoid environmental pollution caused by the fact that the anode gas is doped with arsine and discharged outside, the general electrolysis system further comprises an anode tail gas treatment device, wherein the anode tail gas treatment device is connected with the anode gas conveying pipeline 40 and is arranged at the tail end of the anode gas conveying pipeline 40. The anode tail gas treatment device is generally an anode dry tail gas treatment device 80, the anode dry tail gas treatment device 80 is connected with the anode gas conveying pipeline 40 and is arranged at the tail end of the anode gas conveying pipeline 40, and the anode dry tail gas treatment device 80 is also used for treating the gas to be discharged by the anode so as to enable the gas to meet the discharge requirement.
Similarly, as shown in FIG. 1, the electrolysis system preferably further comprises an anode gas delivery branch pipe 60, the anode gas delivery branch pipe 60 is connected to the anode gas delivery pipeline 40, and the anode gas delivery branch pipe 60 is provided with a second pressure relief valve 61. When the pressure in the anode chamber 13 is too high, the first pressure relief valve 51 is used for pressure relief, so that the anode chamber 13 in the electrolytic cell is ensured not to be overpressurized. Preferably, the anode gas delivery branch pipe 60 is connected to the anode dry-type off-gas treatment device 80, and when the first pressure release valve 51 is opened, the gas can be delivered to the anode dry-type off-gas treatment device 80 for treatment.
The cathode material for preparing the arsine by the electrolysis method and the catalyst used by the cathode have great influence on the ratio of the arsine to the hydrogen generated in the electrolysis process, the current of the electrolysis electrode also has great influence on the ratio of the arsine to the hydrogen, and the gas factor has smaller influence on the ratio of the arsine to the hydrogen. When the cathode material and the cathode of the electrolysis electrode are fixed by using a catalyst and the electrode current, the fluctuation range of the ratio of the arsine and hydrogen generated by electrolysis is smaller. It is therefore preferred that the power supply 14 of the cell is a constant current supply so that the total amount of gas produced per unit time in the cathode chamber 11 and the anode chamber 13 is a constant value.
Except for the specific position, the sequence of the pressure sensors and the pressure switches is not particularly limited, and fig. 1 only shows one setting mode, which can be adjusted by a person skilled in the art.
The operation mechanism and effect of the electrolysis system of the present application will be described below with reference to examples.
As shown in FIG. 1, the power supply 14 of the electrolytic cell is designed as a constant current source, and the electrolysis current is controlled to be stable so that the electrolysis speed is controlled and the total amount of the gas generated in the cathode chamber 11 or the anode chamber 13 per unit time is a constant value. A first differential pressure sensor 20 is provided between the cathode gas delivery line 30 and the anode gas delivery line 40 to monitor the differential pressure between the anode chamber 13 and the cathode chamber 11, which can currently achieve an accuracy of 10 pa. A first automatic pressure controller 33 is designed on the cathode gas conveying pipeline 30, and the first automatic pressure controller 33 will automatically adjust the pressure in the cathode chamber 11 and the anode chamber 13 to be the same according to the information transmitted by the first differential pressure sensor 20, so as to ensure that the pressure difference between the cathode chamber 11 and the anode chamber 13 is within a preset range.
The first pressure sensor 31 is arranged on the cathode chamber 11, the second pressure sensor 41 is arranged on the anode chamber 13, and the pressure of the cathode chamber 11 and the pressure of the anode chamber 13 can be monitored in real time.
In order to solve the problem of the failure of the first pressure sensor 31 or the first pressure sensor 31 during the electrolysis of the electrolytic cell, the cathode gas conveying pipeline 30 is also provided with a first pressure switch 32, the anode gas conveying pipeline 40 is also provided with a second pressure switch 42, and if the pressure of the cathode chamber 11 or the anode chamber 13 exceeds a preset design value, the electrolytic cell is directly powered off for protection.
When the pressure sensors fail and the pressure switches also fail simultaneously, it is estimated that the possibility is only a few parts per million, and the predetermined pressure exceeded by the first pressure relief valve 51 on the cathode gas delivery line 30 and the second pressure relief valve 61 on the anode gas delivery line 40, respectively, is directly discharged to the off-gas treatment system, ensuring that the pressure in the electrolyzer is not over-pressurized.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
be provided with first differential pressure sensor between cathode gas conveying line and anode gas conveying line in order to monitor the pressure differential of anode chamber and cathode chamber, adjust anode chamber and/or the interior gas pressure of cathode chamber when the too big exceedes of pressure differential is injectd, for example through adjustment gas flow rate, voltage size etc. to avoid the too big damage to ion semi-permeable membrane of pressure differential, and then guaranteed that the cathode chamber generates and the gas quality that flows is stable, need not carry out the stability that the follow-up application is gas flow, and then guaranteed the safe and stable operation of system.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An electrolysis system for producing arsine electrolytically, the electrolysis system comprising:
an electrolysis cell having a cathode compartment (11) and an anode compartment (13) separated by an ionic semi-permeable membrane (12), the cathode compartment (11) being electrolysed to produce arsine and hydrogen, the anode compartment (13) being electrolysed to produce oxygen;
a cathode gas delivery line (30) connected to the cathode chamber (11);
an anode gas delivery line (40) connected to the anode chamber (13);
characterized in that a first differential pressure sensor (20) is arranged between the cathode gas supply line (30) and the anode gas supply line (40) to monitor the differential pressure between the anode chamber (13) and the cathode chamber (11).
2. An electrolysis system according to claim 1, wherein the cathode gas feed line (30) is provided with a first automatic pressure controller (33), the first automatic pressure controller (33) being electrically connected to the first differential pressure sensor (20) for receiving a signal from the first differential pressure sensor (20) to adjust the differential pressure between the cathode chamber (11) and the anode chamber (13).
3. An electrolysis system according to claim 2, wherein the cathode gas delivery line (30) is provided with a first pressure sensor (31).
4. An electrolysis system according to claim 2 or 3, wherein the cathode gas delivery line (30) is further provided with a first pressure switch (32).
5. An electrolysis system according to claim 2, wherein a second pressure sensor (41) is provided on the anode gas delivery line (40).
6. An electrolysis system according to claim 5, wherein the anode gas delivery line (40) is further provided with a second pressure switch (42).
7. The electrolysis system according to any one of claims 1 to 3, 5 and 6, further comprising a cathode gas delivery manifold (50), wherein the cathode gas delivery manifold (50) is connected to the cathode gas delivery line (30), and wherein a first pressure relief valve (51) is arranged on the cathode gas delivery manifold (50).
8. The electrolysis system according to any one of claims 1 to 3, 5 and 6, further comprising an anode gas delivery branch (60), wherein the anode gas delivery branch (60) is connected to the anode gas delivery line (40), and a second pressure relief valve (61) is arranged on the anode gas delivery branch (60).
9. The electrolysis system according to any one of claims 1 to 3, 5 and 6, further comprising a cathode off-gas treatment device connected to the cathode gas conveying line (30) and disposed at the end of the cathode gas conveying line (30).
10. The electrolysis system according to any one of claims 1 to 3, 5 and 6, further comprising an anode tail gas treatment device connected to the anode gas delivery line (40) and disposed at the end of the anode gas delivery line (40).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811279617.6A CN111118519A (en) | 2018-10-30 | 2018-10-30 | Electrolytic system for preparing arsine by electrolytic method |
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| CN201811279617.6A CN111118519A (en) | 2018-10-30 | 2018-10-30 | Electrolytic system for preparing arsine by electrolytic method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114438534A (en) * | 2022-01-05 | 2022-05-06 | 飞马牧场(上海)信息咨询服务有限公司 | High-purity gas preparation device and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114438534A (en) * | 2022-01-05 | 2022-05-06 | 飞马牧场(上海)信息咨询服务有限公司 | High-purity gas preparation device and preparation method |
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