CN117210825B - Electrolysis control system and control method for preparing nitrogen trifluoride - Google Patents
Electrolysis control system and control method for preparing nitrogen trifluoride Download PDFInfo
- Publication number
- CN117210825B CN117210825B CN202311196551.5A CN202311196551A CN117210825B CN 117210825 B CN117210825 B CN 117210825B CN 202311196551 A CN202311196551 A CN 202311196551A CN 117210825 B CN117210825 B CN 117210825B
- Authority
- CN
- China
- Prior art keywords
- electrolysis
- nitrogen trifluoride
- voltage
- value
- electrolyte
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 101
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000005457 optimization Methods 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims description 51
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 38
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 38
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 37
- 238000001514 detection method Methods 0.000 claims description 34
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 18
- 210000004027 cell Anatomy 0.000 claims description 8
- 210000002569 neuron Anatomy 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000003487 electrochemical reaction Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- -1 graphene modified carbon Chemical class 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses an electrolysis control system and a control method for preparing nitrogen trifluoride. The system comprises: the electrolysis control device comprises an operation control unit, a data acquisition unit, a target optimized voltage model building unit, an electrolysis efficiency calculation model building unit and a nitrogen trifluoride electrolysis voltage state model building unit. The target optimization voltage model building unit is used for building a target optimization voltage calculation model, the electrolysis efficiency calculation model building unit is used for building an electrolysis efficiency calculation model, the nitrogen trifluoride electrolysis voltage state model building unit is used for building a nitrogen trifluoride electrolysis voltage state model, and the operation control unit is used for controlling the nitrogen trifluoride electrolysis process according to the nitrogen trifluoride electrolysis voltage state value.
Description
Technical Field
The invention belongs to the technical field of automatic control, and particularly relates to an electrolysis control system and control method for preparing nitrogen trifluoride.
Background
Nitrogen trifluoride is a toxic, odorless, colorless, nonflammable gas, and is a strong oxidant and combustion improver. Nitrogen trifluoride gas is widely used in the electronics industry as an etchant and a cleaning agent. In recent years, the annual demand rate of nitrogen trifluoride has been increasing. At present, the preparation methods of nitrogen trifluoride mainly comprise a direct conversion method and a molten salt electrolysis method. The direct conversion method is to prepare nitrogen trifluoride by reacting ammonia gas with fluorine simple substance, and then obtain the final product through purification. In the direct conversion method, the magazines in the fluorine simple substance are difficult to remove, and the magazines are difficult to separate and remove after being mixed into a final product, so that the requirements on process equipment and processing conditions are very strict. Although explosive gas is not generated in the direct chemical method production process, the production is safer, the chemical synthesis process is not easy to control, the impurity content is relatively high, and the process equipment is more complex than the related equipment of the electrolytic method. The molten salt electrolysis method can effectively control the content of impurities, and is mainly used for obtaining a nitrogen trifluoride product by a method of electrolyzing hydrogen fluoride and ammonium fluoride. For example, the prior art CN106222688A discloses a method for preparing nitrogen trifluoride by electrolyzing ammonium bifluoride, which uses a conductive graphene modified carbon electrode as an electrolytic reaction anode, prepares electrolyte by using hydrogen fluoride and ammonium fluoride according to a molar ratio of 1-3:1, continuously injects the electrolyte into an electrolytic tank, the electrolysis temperature is 8 0-1-5 ℃ and the pressure is-0.0-0.01 MPa, the voltage is 5-10V, the anode generating gas contains nitrogen trifluoride, tetrafluoromethane and nitrous oxide, and some trace impurities, the mixed gas is subjected to impurity fluorine removal and acid impurity removal, then the nitrogen trifluoride and tetrafluoromethane are separated by adsorbing the nitrogen trifluoride by a molecular sieve, and the nitrogen trifluoride is refined by a water washing and alkaline washing procedure to obtain the product.
However, in the prior art, a mode of constant voltage with an empirical value is generally adopted for controlling the voltage of the electrolytic cell, the control process cannot be controlled according to the actual condition of the electrolytic cell, fluorine gas simple substance is generated in the electrolytic cell if the temperature is too low, the volatilization amount of the electrolyte is too high if the temperature is too high, and the control mode can cause larger energy consumption, so that the cost is not beneficial to reduction. Therefore, how to overcome the defects of the prior art is a problem to be solved in the technical field.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an electrolysis control system and a control method for preparing nitrogen trifluoride, which concretely adopts the following technical scheme:
an electrolytic control system for producing nitrogen trifluoride, the system comprising: an electrolytic tank, an electrolysis control device and an external detection device;
the electrolytic cell comprises an anode and a cathode for electrolyzing molten hydrogen fluoride and ammonium fluoride electrolyte, and the electrolysis control device is used for applying an electrolysis voltage between the anode and the cathode;
the external detection device is arranged in the electrolytic tank and connected with the electrolysis control device, and comprises a temperature sensor, a nitrogen trifluoride concentration detection device, a tetrafluoromethane concentration detection device and an electrolyte liquid level sensor;
the temperature sensor is used for detecting the real-time temperature of the electrolyte of hydrogen fluoride and ammonium fluoride, the nitrogen trifluoride concentration detection device is used for detecting the concentration of nitrogen trifluoride generated by the anode, the tetrafluoromethane concentration detection device is used for detecting the concentration of tetrafluoromethane generated by the anode, and the electrolyte liquid level sensor is used for detecting the liquid level variation of the electrolyte;
the temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor send detection data to the electrolysis control device;
the electrolysis control device comprises an operation control unit, a data acquisition unit, a target optimization voltage model building unit, an electrolysis efficiency calculation model building unit and a nitrogen trifluoride electrolysis voltage state model building unit.
The operation control unit calculates the volatilization amount of the electrolyte of hydrogen fluoride and ammonium fluoride according to the liquid level change amount of the electrolyte, and sends the volatilization amount to the data acquisition unit;
the data acquisition unit receives the volatilization amounts of the hydrogen fluoride and ammonium fluoride electrolyte, and acquisition data sent by the temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor, and sends the acquisition data to the target optimization voltage model establishment unit;
the target optimized voltage model building unit is used for building a target optimized voltage calculation model;
the electrolytic efficiency calculation model building unit is used for building an electrolytic efficiency calculation model;
the nitrogen trifluoride electrolysis voltage state model building unit is used for building a nitrogen trifluoride electrolysis voltage state model;
the operation control unit is used for controlling the nitrogen trifluoride electrolysis process according to the state value of the nitrogen trifluoride electrolysis voltage.
The invention also relates to an electrolytic control method for preparing nitrogen trifluoride, which is realized by adopting the system, and the method comprises the following steps:
s1, collecting real-time parameter values of nitrogen trifluoride electrolysis;
s2, establishing a target optimized voltage calculation model;
s3, establishing an electrolysis efficiency calculation model;
s4, establishing a nitrogen trifluoride electrolysis voltage state model;
s5, controlling the nitrogen trifluoride electrolysis process according to the state value of the electrolysis voltage of the nitrogen trifluoride.
According to the technical scheme, voltage control is performed according to the actual conditions of the electrolytic cell, control factors comprise the temperature in the electrolytic cell, the volatilization amount of the electrolyte and the concentration of impurities generated by the anode, and the stable production of nitrogen trifluoride can be ensured, the production efficiency is improved, and the energy consumption is reduced through the control process.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention. It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the present application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
Example 1 of the present invention relates to an electrolytic control system for producing nitrogen trifluoride. The system comprises an electrolytic tank, an electrolysis control device and an external detection device. The electrolytic cell comprises an anode and a cathode for electrolysis of molten hydrogen fluoride and ammonium fluoride electrolyte, and the electrolysis control means is for applying an electrolysis voltage between the anode and the cathode.
The external detection device is arranged in the electrolytic tank and connected with the electrolysis control device, and comprises a temperature sensor, a nitrogen trifluoride concentration detection device, a tetrafluoromethane concentration detection device and an electrolyte liquid level sensor.
The temperature sensor is used for detecting the real-time temperature of the electrolyte of hydrogen fluoride and ammonium fluoride, the nitrogen trifluoride concentration detection device is used for detecting the concentration of nitrogen trifluoride generated by the anode, the tetrafluoromethane concentration detection device is used for detecting the concentration of tetrafluoromethane generated by the anode, and the electrolyte liquid level sensor is used for detecting the liquid level change of the electrolyte.
The temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor send detection data to the electrolysis control device.
The electrolysis control device comprises an operation control unit, a data acquisition unit, a target optimization voltage model building unit, an electrolysis efficiency calculation model building unit and a nitrogen trifluoride electrolysis voltage state model building unit.
And the operation control unit calculates the volatilization amount of the electrolyte of the hydrogen fluoride and the ammonium fluoride according to the change of the liquid level of the electrolyte, and sends the volatilization amount to the data acquisition unit.
The data acquisition unit receives the volatilization amounts of the hydrogen fluoride and ammonium fluoride electrolyte, and detection data sent by the temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor, and the data acquisition unit also comprises the temperature values of the hydrogen fluoride and ammonium fluoride electrolyteMolar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>And sending the target optimized voltage model to the target optimized voltage model building unit.
The first threshold is a preset upper limit value of concentration of tetrafluoromethane generated by the anode, and the second threshold is a preset upper limit value of volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte.
The target optimized voltage model building unit is used for building a target optimized voltage calculation model, and the target optimized voltage calculation model is as follows:
in the method, in the process of the invention,weight value for the i-th input parameter value, is->For the ith neuron threshold, +.>For the input value of the real-time parameters of the electrolysis of nitrogen trifluoride,/->The combination function is represented by the connection weight value of the ith neuron and the output, and G.
Specifically, theComprises the above-mentioned hydrogen fluoride and ammonium fluoride electrolyte temperature values +.>Molar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>. The combination function specifically comprises the following steps:
where exp () represents an exponential function based on e.
The electrolytic efficiency calculation model building unit is used for building an electrolytic efficiency calculation model:
where m is the throughput of nitrogen trifluoride in a single cycle, I is the amperometric statistic of the electrolysis in a single cycle, and 0.442 is the electrochemical reaction equivalent of nitrogen trifluoride.
The nitrogen trifluoride electrolysis voltage state model building unit is used for building a nitrogen trifluoride electrolysis voltage state model:
in the method, in the process of the invention,for the value of the electrolysis voltage state>For real-time measurement of electrolytic voltage, < >>Optimizing the voltage value for the target, +.>Is the electrolytic efficiency value.
The operation control unit is also used for controlling the nitrogen trifluoride electrolysis process according to the state value of the nitrogen trifluoride electrolysis voltage. The method specifically comprises the following steps: when (when)When the current running state of the electrolysis system is maintained, when +.>When this is the case, the above steps S1-S4 are re-executed. Wherein (1)>The method is to preset a nitrogen trifluoride electrolysis voltage state deviation threshold value.
Embodiment 2 of the present invention relates to an electrolysis control method for preparing nitrogen trifluoride, which is implemented by using the electrolysis control system of embodiment 1, and specifically includes the following steps:
s1, collecting real-time parameter values of nitrogen trifluoride electrolysis. The method specifically comprises the steps of collecting the temperature values of the electrolyte of hydrogen fluoride and ammonium fluorideMolar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>。
The first threshold is a preset upper limit value of concentration of tetrafluoromethane generated by the anode, and the second threshold is a preset upper limit value of volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte.
S2, establishing a target optimized voltage calculation model. The target optimization voltage calculation model is used for calculating an electrolysis voltage target optimization value, and specifically comprises the following steps:
in the method, in the process of the invention,weight value for the i-th input parameter value, is->For the ith neuron threshold, +.>For the input value of the real-time parameters of the electrolysis of nitrogen trifluoride,/->The combination function is represented by the connection weight value of the ith neuron and the output, and G.
Specifically, theComprises the above-mentioned hydrogen fluoride and ammonium fluoride electrolyte temperature values +.>Molar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>. The combination function specifically comprises the following steps:
where exp () represents an exponential function based on e.
S3, establishing an electrolysis efficiency calculation model. The electrolytic efficiency calculation model is as follows:
where m is the throughput of nitrogen trifluoride in a single cycle, I is the amperometric statistic of the electrolysis in a single cycle, and 0.442 is the electrochemical reaction equivalent of nitrogen trifluoride.
S4, establishing a nitrogen trifluoride electrolysis voltage state model:
in the method, in the process of the invention,for the value of the electrolysis voltage state>For real-time measurement of electrolytic voltage, < >>Optimizing the voltage value for the target, +.>Is the electrolytic efficiency value.
S5, controlling the nitrogen trifluoride electrolysis process according to the state value of the electrolysis voltage of the nitrogen trifluoride. The method specifically comprises the following steps: when (when)When the current running state of the electrolysis system is maintained, when +.>When this is the case, the above steps S1-S4 are re-executed. Wherein (1)>The method is to preset a nitrogen trifluoride electrolysis voltage state deviation threshold value.
While only the preferred embodiments of the present invention have been described, it should be noted that modifications and variations can be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and variations should also be regarded as being within the scope of the invention.
Claims (2)
1. An electrolytic control system for producing nitrogen trifluoride, said system comprising: an electrolytic tank, an electrolysis control device and an external detection device;
the electrolytic cell comprises an anode and a cathode for electrolyzing molten hydrogen fluoride and ammonium fluoride electrolyte, and the electrolysis control device is used for applying an electrolysis voltage between the anode and the cathode;
the external detection device is arranged in the electrolytic tank and connected with the electrolysis control device, and comprises a temperature sensor, a nitrogen trifluoride concentration detection device, a tetrafluoromethane concentration detection device and an electrolyte liquid level sensor;
the temperature sensor is used for detecting the real-time temperature of the electrolyte of hydrogen fluoride and ammonium fluoride, the nitrogen trifluoride concentration detection device is used for detecting the concentration of nitrogen trifluoride generated by the anode, the tetrafluoromethane concentration detection device is used for detecting the concentration of tetrafluoromethane generated by the anode, and the electrolyte liquid level sensor is used for detecting the liquid level variation of the electrolyte;
the temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor send detection data to the electrolysis control device;
the electrolysis control device comprises an operation control unit, a data acquisition unit, a target optimization voltage model building unit, an electrolysis efficiency calculation model building unit and a nitrogen trifluoride electrolysis voltage state model building unit;
the operation control unit calculates the volatilization amount of the electrolyte of hydrogen fluoride and ammonium fluoride according to the liquid level change amount of the electrolyte, and sends the volatilization amount to the data acquisition unit;
the data acquisition unit receives the volatilization amounts of the hydrogen fluoride and ammonium fluoride electrolyte, and acquisition data sent by the temperature sensor, the nitrogen trifluoride concentration detection device, the tetrafluoromethane concentration detection device and the electrolyte liquid level sensor, and sends the acquisition data to the target optimization voltage model establishment unit; the collected data specifically comprises: hydrogen fluoride and ammonium fluoride electrolyte temperature valuesMolar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>；
The first threshold is a preset upper limit value of concentration of tetrafluoromethane generated by the anode, and the second threshold is a preset upper limit value of volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte;
the target optimized voltage model building unit is used for building a target optimized voltage calculation model, and the target optimized voltage calculation model is as follows:
；
in the method, in the process of the invention,weight value for the i-th input parameter value, is->For the ith neuron threshold, +.>For the input value of the real-time parameters of the electrolysis of nitrogen trifluoride,/->The connection weight value of the ith neuron and the output is represented by G;
the saidComprises the above-mentioned hydrogen fluoride and ammonium fluoride electrolyte temperature values +.>Molar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>；
The combination function specifically comprises the following steps:
；
wherein exp () represents an exponential function based on e;
the electrolytic efficiency calculation model building unit is used for building an electrolytic efficiency calculation model, and the electrolytic efficiency calculation model specifically comprises the following components:
；
wherein m is the throughput of nitrogen trifluoride in a single cycle, I is the amperometric statistic of the electrolysis in a single cycle, and 0.442 is the electrochemical reaction equivalent of nitrogen trifluoride;
the nitrogen trifluoride electrolysis voltage state model building unit is used for building a nitrogen trifluoride electrolysis voltage state model, and the nitrogen trifluoride electrolysis voltage state model specifically comprises:
；
in the method, in the process of the invention,for the value of the electrolysis voltage state>For real-time measurement of electrolytic voltage, < >>Optimizing the voltage value for the target, +.>Is an electrolysis efficiency value;
the operation control unit is used for controlling the nitrogen trifluoride electrolysis process according to the state value of the nitrogen trifluoride electrolysis voltage, and specifically comprises the following steps of judging the state of the nitrogen trifluoride electrolysis voltage:
when (when)When the electrolytic system is in the current running state, the current running state of the electrolytic system is maintained;
when (when)When the method is used, the operation of the electrolysis system is controlled by means of the target optimized voltage established by the target optimized voltage model establishing unit, and the nitrogen trifluoride electrolysis voltage state is judged again by means of the electrolysis efficiency calculation model establishing unit and the nitrogen trifluoride electrolysis voltage state model establishing unit;
wherein,the method is to preset a nitrogen trifluoride electrolysis voltage state deviation threshold value.
2. An electrolytic control method for producing nitrogen trifluoride using the system of claim 1, said method comprising the steps of:
s1, collecting real-time parameter values of nitrogen trifluoride electrolysis;
s2, establishing a target optimized voltage calculation model, wherein the target optimized voltage calculation model is as follows:
；
in the method, in the process of the invention,weight value for the i-th input parameter value, is->For the ith neuron threshold, +.>For the input value of the real-time parameters of the electrolysis of nitrogen trifluoride,/->The connection weight value of the ith neuron and the output is represented by G;
the saidComprising hydrogen fluoride and ammonium fluoride electrolyte temperature values +.>Molar ratio of hydrogen fluoride to ammonium fluoride>Anode generated nitrogen trifluoride concentration value +.>Difference between the first threshold and the concentration of tetrafluoromethane produced at the anode +.>Difference between the second threshold and the volatilization amounts of the hydrogen fluoride and the ammonium fluoride electrolyte +.>；
The combination function specifically comprises the following steps:
；
wherein exp () represents an exponential function based on e;
s3, establishing an electrolysis efficiency calculation model, wherein the electrolysis efficiency calculation model is as follows:
；
wherein m is the throughput of nitrogen trifluoride in a single cycle, I is the amperometric statistic of the electrolysis in a single cycle, and 0.442 is the electrochemical reaction equivalent of nitrogen trifluoride;
s4, establishing a nitrogen trifluoride electrolysis voltage state model, wherein the nitrogen trifluoride electrolysis voltage state model is as follows:
；
in the method, in the process of the invention,for the value of the electrolysis voltage state>For real-time measurement of electrolytic voltage, < >>Optimizing the voltage value for the target, +.>Is an electrolysis efficiency value;
s5, controlling the nitrogen trifluoride electrolysis process according to the state value of the electrolysis voltage of the nitrogen trifluoride, and specifically comprising the following steps:
when (when)When the current running state of the electrolysis system is maintained, when +.>When the above steps S1-S4 are executed again;
wherein,the method is to preset a nitrogen trifluoride electrolysis voltage state deviation threshold value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311196551.5A CN117210825B (en) | 2023-09-16 | 2023-09-16 | Electrolysis control system and control method for preparing nitrogen trifluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311196551.5A CN117210825B (en) | 2023-09-16 | 2023-09-16 | Electrolysis control system and control method for preparing nitrogen trifluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117210825A CN117210825A (en) | 2023-12-12 |
| CN117210825B true CN117210825B (en) | 2024-03-08 |
Family
ID=89034863
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311196551.5A Active CN117210825B (en) | 2023-09-16 | 2023-09-16 | Electrolysis control system and control method for preparing nitrogen trifluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117210825B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4324621A (en) * | 1979-12-26 | 1982-04-13 | Cominco Ltd. | Method and apparatus for controlling the quality of electrolytes |
| JP2000072416A (en) * | 1998-09-01 | 2000-03-07 | Mitsui Chemicals Inc | Production of nitrogen trifluoride gas |
| JP2000104186A (en) * | 1998-09-29 | 2000-04-11 | Mitsui Chemicals Inc | Production of nitrogen trifluoride gas |
| JP2008266741A (en) * | 2007-04-23 | 2008-11-06 | Mitsui Chemicals Inc | Gas-generating apparatus and gas-generating method |
| CN101624708A (en) * | 2008-07-10 | 2010-01-13 | 培尔梅烈克电极股份有限公司 | Method of electrolytically synthesizing nitrogen trifluoride |
| CN102534684A (en) * | 2010-12-21 | 2012-07-04 | 贵阳铝镁设计研究院有限公司 | Method for controlling electrolytic cell under low-voltage production |
| CN103460469A (en) * | 2011-04-05 | 2013-12-18 | 布莱克光电有限公司 | H2O-based electrochemical hydrogen-catalyst power system |
| WO2020036128A1 (en) * | 2018-08-13 | 2020-02-20 | 旭化成株式会社 | Water electrolysis apparatus |
| JP2020158838A (en) * | 2019-03-27 | 2020-10-01 | Ｅｎｅｏｓ株式会社 | Electrochemical-type hydrogen pump system and method for operating electrochemical-type hydrogen pump |
| WO2021158143A1 (en) * | 2020-02-04 | 2021-08-12 | Общество С Ограниченной Ответственностью "Объединенная Компания Русал Инженерно -Технологический Центр" | Process control method for use in aluminium electrolysis cell |
| CN114086204A (en) * | 2021-12-10 | 2022-02-25 | 清华四川能源互联网研究院 | Electrolytic cell array system and electrolytic water system control method |
| CN116254547A (en) * | 2022-12-30 | 2023-06-13 | 福建德尔科技股份有限公司 | Preparation method of nitrogen trifluoride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8945367B2 (en) * | 2011-01-18 | 2015-02-03 | Air Products And Chemicals, Inc. | Electrolytic apparatus, system and method for the safe production of nitrogen trifluoride |
-
2023
- 2023-09-16 CN CN202311196551.5A patent/CN117210825B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4324621A (en) * | 1979-12-26 | 1982-04-13 | Cominco Ltd. | Method and apparatus for controlling the quality of electrolytes |
| JP2000072416A (en) * | 1998-09-01 | 2000-03-07 | Mitsui Chemicals Inc | Production of nitrogen trifluoride gas |
| JP2000104186A (en) * | 1998-09-29 | 2000-04-11 | Mitsui Chemicals Inc | Production of nitrogen trifluoride gas |
| JP2008266741A (en) * | 2007-04-23 | 2008-11-06 | Mitsui Chemicals Inc | Gas-generating apparatus and gas-generating method |
| CN101624708A (en) * | 2008-07-10 | 2010-01-13 | 培尔梅烈克电极股份有限公司 | Method of electrolytically synthesizing nitrogen trifluoride |
| CN102534684A (en) * | 2010-12-21 | 2012-07-04 | 贵阳铝镁设计研究院有限公司 | Method for controlling electrolytic cell under low-voltage production |
| CN103460469A (en) * | 2011-04-05 | 2013-12-18 | 布莱克光电有限公司 | H2O-based electrochemical hydrogen-catalyst power system |
| WO2020036128A1 (en) * | 2018-08-13 | 2020-02-20 | 旭化成株式会社 | Water electrolysis apparatus |
| JP2020158838A (en) * | 2019-03-27 | 2020-10-01 | Ｅｎｅｏｓ株式会社 | Electrochemical-type hydrogen pump system and method for operating electrochemical-type hydrogen pump |
| WO2021158143A1 (en) * | 2020-02-04 | 2021-08-12 | Общество С Ограниченной Ответственностью "Объединенная Компания Русал Инженерно -Технологический Центр" | Process control method for use in aluminium electrolysis cell |
| CN114086204A (en) * | 2021-12-10 | 2022-02-25 | 清华四川能源互联网研究院 | Electrolytic cell array system and electrolytic water system control method |
| CN116254547A (en) * | 2022-12-30 | 2023-06-13 | 福建德尔科技股份有限公司 | Preparation method of nitrogen trifluoride |
Non-Patent Citations (3)
| Title |
|---|
| Performances of metal fluoride added carbon anodes with pre-electrolysis for electrolytic synthesis of NF3;Tomohiro Isogai等;《Electrochimica Acta》;20110328;第56卷;4425–4432 * |
| 三氟化氮气体的制备及纯化方法综述;尹强;许俊斌;周瑾艳;周阳;毛沅文;贾相锐;叶丽芳;;广东化工;20190430(第08期);112-113 * |
| 铝电解混合智能优化控制方法研究与应用;汪成亮;陆志坚;庞栩;熊西林;;轻金属;20091120(11);23-27 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117210825A (en) | 2023-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102877085B (en) | Method for preparing high-purity peroxysulphate based on electrolytic oxidation through ion-exchange membrane electrolyzer for chlor-alkali production | |
| CN110117794B (en) | Electro-reduction of CO2Three-chamber type electrolytic cell device for preparing formate and electrolytic method thereof | |
| CN102190573A (en) | Method for preparing formic acid through electrochemical catalytic reduction of carbon dioxide | |
| CN113373477A (en) | Method and system for controlling electrolyte flow and pressure of dynamic hydrogen production electrolytic cell | |
| CN112760672B (en) | Method for electrochemically preparing trifluoromethyl sulfonyl fluoride from methyl sulfonyl chloride | |
| CN110857470B (en) | Regeneration and circulation method of ferric trichloride etching solution | |
| CN101942675B (en) | Method for recycling Sn<2+> in waste water by electrolytic reduction | |
| JP2015091572A (en) | Biogas producing system and method of producing biogas and carbon dioxide reduced product using biogas producing system | |
| CN101798689A (en) | Process and device for preparing nitrogen trifluoride by continuous electrolytic process | |
| CN103866344B (en) | A kind of method of electrolytic preparation nitric acid | |
| CN117210825B (en) | Electrolysis control system and control method for preparing nitrogen trifluoride | |
| CN113603059B (en) | Molten salt, electrochemical purification method of molten salt and electrochemical device | |
| CN111636073A (en) | Device and process for recycling salt-containing wastewater | |
| CN110204017B (en) | Electrolytic treatment system and method for adjusting pH value of ammonia-containing wastewater | |
| CN101280432B (en) | Electrolytic apparatus for regenerating waste acid produced by acid cleaning of stainless steel, regeneration method therefor | |
| Chaenko et al. | Indirect electrochemical oxidation of aliphatic alcohols to carboxylic acids by active oxygen forms in aqueous media | |
| CN101864577B (en) | Method for electrochemically preparing peroxysulfuric acid | |
| CN114774946A (en) | Two-step water electrolysis hydrogen production device based on three-electrode system and application thereof | |
| CN111020614B (en) | Method for recycling phosphoric acid by electrolyzing mixed acid solution | |
| CN115411326A (en) | Vanadium electrolyte using ammonium metavanadate as raw material and preparation method thereof | |
| CN111996541B (en) | Indirect hydrogen sulfide electrolysis method and device for improving hydrogen yield | |
| CN113430547A (en) | Device for preparing potassium formate by electrolyzing carbon dioxide and electrolysis method | |
| KR102054248B1 (en) | Composite process of carbon dioxide reduction with preparing of formic acid and potasium sulfate, and apparatus for the same | |
| CN110416585B (en) | Preparation method and preparation device of flow battery electrolyte | |
| CN214327911U (en) | Anti-corrosion device for nitrogen trifluoride electrolysis process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |