CN111239230A - Real-time synchronous monitoring device and method for electrochemical positive and negative pole reaction products - Google Patents
Real-time synchronous monitoring device and method for electrochemical positive and negative pole reaction products Download PDFInfo
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Abstract
The invention relates to a device and a method for synchronously monitoring electrochemical positive and negative reaction products in real time, which solve the problem that the electrochemical reaction products of positive and negative electrodes cannot be monitored in real time and synchronously in the existing electrochemical-mass spectrometry technology. The device comprises an electrochemical reaction tank and an electrode combination, wherein an electrode is hermetically connected with a mounting port on the electrochemical reaction tank through a ferrule type end through pipe joint, high-pressure gas is introduced into the electrochemical reaction tank from a gas pressure port to ensure that a working electrode metal pipe and an auxiliary electrode metal pipe are filled with reaction liquid, when electrochemical reaction occurs, products generated on the surfaces of the working electrode and the auxiliary electrode are respectively sprayed out from an outer port of the working electrode metal pipe and an outer port of the auxiliary electrode metal pipe and respectively enter a mass spectrometer for detection, and real-time synchronous monitoring of positive and negative electrode electrochemical oxidation-reduction reaction products is realized; also provides a using method thereof. The invention is widely applied to the technical field of electrochemistry-mass spectrometry.
Description
Technical Field
The invention belongs to the technical field of electrochemistry-mass spectrometry, and particularly relates to a device and a method for synchronously monitoring reaction products of an electrochemical anode and a electrochemical cathode in real time.
Background
In the course of electrochemical development, modern electrochemical analysis techniques for the study of reaction products and intermediate transition substances play a crucial role. Among a plurality of electrochemical characterization means, the electrochemical-mass spectrometry combined technology has the advantages that the dynamic reaction process is monitored in real time, the instantaneously existing intermediate is captured, the electrochemical reaction mechanism, the dynamic parameters and the like can be deduced, the experimental result is visual and reliable, and the electrochemical-mass spectrometry combined technology becomes an efficient electrochemical characterization method.
At present, aiming at the electrochemical-mass spectrometry technology, the monitoring requirements of different reactions are realized mainly by improving and designing the structures of an electrochemical electrolytic cell and an electrode. Among them, the electrode is the main device for inputting electrons into the electrolyte to control the electrochemical reaction process, and usually adopts a three-electrode combination including a working electrode, an auxiliary electrode and a reference electrode, and the working electrode and the auxiliary electrode are also considered as a positive electrode and a negative electrode in the electrochemical reaction, and the reaction products are generated on the surface area of the two electrodes. However, the existing electrochemical electrolytic cells and electrode structures cannot isolate products generated by the working electrode and the auxiliary electrode respectively, so that all the products are mixed together and enter a mass spectrum for analysis, thereby reducing the accuracy, reliability and specificity of product data and influencing the accurate derivation of an electrochemical reaction mechanism.
Disclosure of Invention
The invention aims to provide a device and a method for synchronously monitoring electrochemical positive and negative reaction products in real time, which have the advantages of simple integral structure, convenient operation, no limitation of spraying by a solvent system, short mass spectrum response time, high sensitivity, capability of synchronously monitoring the positive and negative electrochemical reaction products and intermediates and capability of meeting the requirements of a more accurate electrochemical-mass spectrometry device.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the invention provides a real-time synchronous monitoring device for electrochemical positive and negative pole reaction products, which comprises an electrolytic cell and an electrode combination, wherein a solution cavity is arranged in the electrolytic cell, and the electrode combination comprises a working electrode, an auxiliary electrode and a reference electrode; the bottom of the side surface of the electrolytic cell is respectively provided with a working electrode mounting port and an auxiliary electrode mounting port which are communicated with the solution cavity, the top of the electrolytic cell is also provided with a reference electrode mounting port which is communicated with the solution cavity, and the upper part of the side surface of the electrolytic cell is also provided with a gas pressurizing port which is communicated with the solution cavity; the working electrode and the auxiliary electrode are both of metal tubular structures; the working electrode and the auxiliary electrode are communicated with a solution cavity in the electrolytic cell through a mounting hole at the bottom of the side surface of the electrolytic cell, and the reference electrode is communicated with the solution cavity of the electrolytic cell through a mounting hole at the top of the electrolytic cell; the outer port of the working electrode metal tube and the outer port of the auxiliary electrode metal tube are respectively opposite to a sample inlet of the mass spectrometer;
after reaction liquid is injected into the solution cavity of the electrolytic cell, the reference electrode is fixed through a mounting port at the top of the electrolytic cell, the measuring end of the reference electrode is immersed in the reaction liquid, and high-pressure gas is introduced into the solution cavity from a gas pressurizing port to ensure that the working electrode and the auxiliary electrode metal tube are filled with the reaction liquid; the working electrode, the auxiliary electrode and the reference electrode are connected with an electrochemical workstation through leads, a power supply of the electrochemical workstation is turned on to start electrochemical reaction, electrochemical reaction products formed on the surfaces of the working electrode and the auxiliary electrode are respectively sprayed out from an outer port of the working electrode metal tube and an outer port of the auxiliary electrode metal tube and respectively enter a mass spectrometer for detection, and the synchronization and real-time monitoring of respective reaction products of a positive electrode and a negative electrode in the electrochemical reaction process are realized.
Preferably, the working electrode mounting port and the auxiliary electrode mounting port are both arranged at the bottom of the side surface of the electrolytic cell.
Preferably, the metal tubular electrode is connected with the electrolytic cell by fixing the metal tubular electrode at the mounting port through a ferrule type end straight pipe joint; the ferrule type end straight-through pipe joint and the working electrode mounting opening are hermetically connected through threads.
Preferably, the reference electrode is also fixed to the top mounting port of the electrolytic cell through a clamping sleeve type end through pipe joint, and the clamping sleeve type end through pipe joint and the auxiliary electrode mounting port are in sealing connection through threads.
Preferably, the metal tubular electrode material is any one of platinum, copper and stainless steel.
Preferably, the metal tubular electrode has an inner diameter of 0.1mm, an outer diameter of 0.4mm to 0.8mm, and a length of 3cm to 4 cm.
Preferably, the electrolytic cell is prepared from an anti-corrosion material, and the anti-corrosion material is polyether ether ketone, polytetrafluoroethylene or quartz glass.
Preferably, the bottom of the electrolytic cell is further provided with a fixing base for fixing the electrolytic cell.
The method for synchronously monitoring the electrochemical positive and negative reaction products in real time comprises the following steps:
(1) aligning the outer port of the metal tubular working electrode with the sample inlet of the mass spectrometer, inserting the other end of the working electrode into the working electrode mounting port at the bottom of the side surface of the electrolytic cell, and sealing and fixedly connecting; aligning the outer port of the metal tubular auxiliary electrode with the sample inlet of the mass spectrometer, and inserting the other end of the auxiliary electrode into an auxiliary electrode mounting port at the bottom of the side surface of the electrolytic cell for sealing and fixed connection; after reaction liquid is injected into a solution cavity in the electrochemical reaction cell, the lower half part of the reference electrode is inserted into a reference electrode mounting hole at the top of the electrolytic cell for sealing and fixing, and the measuring end of the reference electrode is immersed into the reaction liquid;
(2) connecting a working electrode, an auxiliary electrode and a reference electrode with an electrochemical workstation through leads, introducing high-pressure gas into a solution cavity in an electrolytic cell from a gas pressurizing port, opening a power supply of the electrochemical workstation after ensuring that the interior of a metal tube of a metal tubular electrode is filled with reaction liquid, initiating the electrochemical reaction of the reaction liquid in the metal tube of the working electrode and the auxiliary electrode, simultaneously spraying reaction products generated on the surfaces of the working electrode and the auxiliary electrode to the outer end port of the metal tube of the metal tubular electrode, and respectively entering a mass spectrometer for detection, thereby realizing the real-time synchronous monitoring of the electrochemical redox reaction products of the positive electrode and the negative electrode.
The invention has the beneficial effects that:
(1) the invention discloses a device and a method for synchronously monitoring products of electrochemical positive and negative pole reactions in real time, and aims to provide an electrochemical-mass spectrometry technology and a using method thereof. The electrochemical reaction device has the advantages of simple structure, convenient operation, no limitation of a solvent system in spraying, short mass spectrum response time and high sensitivity, can synchronously monitor the electrochemical reaction products and the intermediate products of the anode and the cathode, and meets the requirements of more accurate and precise electrochemical in-situ observation devices.
(2) The device is used for the real-time synchronous monitoring device of the electrochemical positive and negative pole reaction products, can detect and analyze a series of products generated by the working electrode and the auxiliary electrode in the electrochemical reaction process by utilizing the electrochemical-mass spectrometry technology, synchronously monitors the oxidation reaction process and the reduction reaction process in real time, has the accuracy and the specificity of the measurement result, and improves the accuracy and the reliability of the reaction mechanism derivation.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural view of the electrolytic cell body in FIG. 1;
FIG. 3 is a schematic view of the cell of FIG. 2 with a reference electrode installed;
FIG. 4 is a schematic structural view of the electrolytic cell of FIG. 2 with a sealing plug device installed;
FIG. 5 is a schematic structural view of a use state of the present invention;
FIG. 6 is a schematic diagram of the structure of the use of the principle of the present invention;
fig. 7 is a schematic structural view of a partially enlarged view of a in fig. 6.
The figure is marked with: 1. the electrolytic cell comprises an electrolytic cell, 2, an electrolytic cell solution cavity, 3, a working electrode mounting port, 4, an auxiliary electrode mounting port, 5, a gas pressurizing port, 6, a reference electrode mounting port, 7, a metal tubular electrode, 8, a clamping sleeve type end direct pipe joint, 9, a reference electrode, 10, a sealing plug device and 11, and a fixed base.
Detailed Description
The invention is further described below in conjunction with the drawings and the specific embodiments to assist in understanding the contents of the invention. The method used in the invention is a conventional production method if no special provisions are made; the starting materials used, unless otherwise specified, are conventional commercial products.
As shown in fig. 1 and fig. 6, the present invention provides a real-time synchronous monitoring device for electrochemical anode and cathode reaction products, comprising an electrolytic cell 1 and an electrode assembly, wherein the bottom of the side surface of the electrolytic cell 1 is respectively provided with a working electrode mounting port 3 and an auxiliary electrode mounting port 4 which are communicated with an electrolytic cell solution cavity 2, and the upper part of the side surface of the electrolytic cell 1 is also provided with a gas pressurizing port 5 which is communicated with the electrolytic cell solution cavity 2; the top of the electrolytic cell 1 is also provided with a reference electrode mounting port 6 communicated with the electrolytic cell solution cavity 2; the working electrode mounting port 3 and the auxiliary electrode mounting port 4 are both internally and hermetically connected with a metal tubular electrode 7. Before the electrochemical reaction begins, reaction liquid is injected into the electrolytic cell solution cavity 2, the reference electrode 9 is tightly fixed at the position of a reference electrode mounting port 6, the measuring end of the reference electrode 9 is ensured to be immersed into the reaction liquid, high-pressure gas is introduced into the electrolytic cell solution cavity 2 from a gas pressurizing port 5, so that the metal tubular electrode 7 is fully filled with the reaction liquid, then the metal tubular electrode 7 and the reference electrode 9 are connected with an electrochemical workstation through leads, a power supply of the electrochemical workstation is turned on to initiate the sample to carry out the electrochemical reaction, meanwhile, products generated on the surface of the metal tubular electrode 7 are sprayed out from an outer port of the metal tube and respectively enter a mass spectrometer to be detected, so that the real-time and synchronous monitoring of electrochemical reaction products of a positive electrode and a negative electrode are realized, and a series of products generated by the working electrode and an auxiliary electrode in the electrochemical reaction process can, the oxidation reaction and the reduction reaction processes are synchronously monitored in real time, the measurement result has accuracy and specificity, and the accuracy and the reliability of reaction mechanism derivation are improved.
The working electrode mounting port 3 and the auxiliary electrode mounting port 4 are both arranged at the bottom of the side surface of the electrolytic cell 2 and are horizontally arranged oppositely, so that electrochemical reaction products generated by the metal tubular working electrode 3 and the metal tubular auxiliary electrode 7 are sprayed outwards at the same time and respectively enter a mass spectrometer for detection, the mass spectrum response time is short, the sensitivity is high, real-time effective monitoring of the electrochemical reaction processes of the positive electrode and the negative electrode is realized, the measurement result is high in accuracy and good in specificity, the accuracy and the reliability of reaction mechanism derivation are improved, and the method has great significance for mechanism research.
As shown in fig. 1 and 4, one end of each metal tubular electrode 7 is inserted into the mounting port through a ferrule type end straight-through pipe joint 8, and the electrolytic cell solution cavity 2 is communicated but does not extend into the solution cavity; the ferrule type end straight pipe joint 8 and the mounting port are connected in a sealing mode through threads, the sealing performance of the whole electrolytic cell solution tank 2 can be guaranteed, electrochemical reaction liquid is completely sprayed out from the outer port of the metal tubular electrode 7, the electrochemical reaction liquid enters the mass spectrometer from the sample inlet to be analyzed, the whole electrochemical reaction is effectively monitored in real time, the mass spectrometer response time is short, and the high accuracy and the reliability of detection results are achieved.
The reference electrode 9 is hermetically installed in the reference electrode installation opening 6, or the sealing plug device 10 is hermetically installed, so that the requirements of a two-electrode or three-electrode system can be met, and the application range is wide.
The metal tubular electrode 7 is any metal tube such as a platinum tube, a copper tube or a stainless steel metal tube, and has an inner diameter of 0.1mm, an outer diameter of 0.4mm to 0.8mm and a length of 3cm to 4 cm; the electrolytic cell 1 is prepared by adopting an anti-corrosion material, and the anti-corrosion material is polyether ether ketone, or polytetrafluoroethylene, or quartz glass. The device has simple structure, firmness and durability, long service life and wide application range; the installation, the maintenance and the replacement are all very convenient. The bottom of the electrolytic cell 1 is also fixedly provided with a fixed base 11 for fixing the electrolytic cell 1, so that the use is convenient, the stability of the whole reaction device in the use process is ensured, and the whole reaction is ensured to smoothly carry out and rapidly and effectively monitor the dynamic change in the reaction process.
The invention relates to a real-time synchronous monitoring method for electrochemical positive and negative pole reaction products, which uses the real-time synchronous monitoring device for the electrochemical positive and negative pole reaction products and comprises the following steps:
(1) as shown in fig. 5 and fig. 6, the outer ports of the metal tubular electrode 7 including the working electrode and the auxiliary electrode are respectively aligned with the sample inlet of the mass spectrometer and adjusted to a certain distance to obtain an optimal mass spectrum response signal, and the other ends of the metal tubular electrode 7 of the working electrode and the auxiliary electrode are respectively inserted into the working electrode mounting port 3 and the auxiliary electrode mounting port 4 at the bottom of the side surface of the electrolytic cell 1 for sealing and fixing to ensure that the metal tubular electrode 7 is communicated with the solution chamber 2; injecting reaction liquid into the solution cavity 2 of the electrolytic cell 1, and when a three-electrode reaction system is researched, hermetically installing a reference electrode 9 in the reference electrode installation opening 6, and immersing the bottom measuring end of the reference electrode 9 below the liquid level of the reaction liquid;
when a two-electrode reaction system is researched, the sealed plug device 10 is hermetically installed in the reference electrode installation notch 6; the device can realize the flexible conversion of a three-electrode reaction system and a two-electrode reaction system, and is suitable for electrochemical experiment requirements under different conditions.
(2) The metal tubular electrode 7 comprises a working electrode and an auxiliary electrode, and a reference electrode 9 is connected with an electrochemical workstation through a lead, so as to respectively initiate electrochemical reactions of solutions in the working electrode and the auxiliary electrode, and simultaneously high-pressure gas is introduced into the solution cavity 2 from the gas pressurization port 5, so that a series of products generated on the surfaces of the working electrode and the auxiliary electrode are sprayed out from the outer ports of the metal tubular electrode 7 and respectively enter a mass spectrometer for detection, and real-time and synchronous monitoring of positive and negative electrochemical reaction products is realized.
The use method of the device for real-time synchronous monitoring of the electrochemical positive and negative reaction products is convenient to operate, can detect and analyze products, instant intermediates and the like generated by the positive electrode and the negative electrode in the electrochemical reaction process, can monitor the electrochemical reaction process of the positive electrode and the negative electrode in real time and synchronously, can accurately obtain the reaction mechanism, and has the advantages of accuracy, reliability, specificity and the like of the analysis result.
In conclusion, the real-time synchronous monitoring device for electrochemical positive and negative electrode reaction products has the advantages of simple overall structure, convenience in operation, short mass spectrum response time, high sensitivity, no limitation of a solvent system on spraying, flexible conversion between a three-electrode system and a two-electrode system, wide application range, capability of synchronously monitoring a series of products generated by the electrochemical positive and negative electrode reactions and capability of meeting the requirements of a more accurate electrochemical-mass spectrometry device.
The above are only examples of the present invention, and for example, the material or specification and dimension of the metal tubular electrode 7 may be changed; and the material or specification and size of the electrolytic cell 1 are changed, so that the device for synchronously monitoring the electrochemical anode and cathode reaction products in real time and the using method thereof can be realized.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", "front", "rear", "inner", "outer", "middle", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
However, the above description is only exemplary of the present invention, and the scope of the present invention should not be limited thereby, and the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should be covered by the claims of the present invention.
Claims (9)
1. The device for synchronously monitoring the reaction products of the anode and the cathode in real time in electrochemistry comprises an electrolytic cell and an electrode assembly, wherein a solution cavity is arranged in the electrolytic cell, and the electrode assembly comprises a working electrode, an auxiliary electrode and a reference electrode; the electrolytic cell is characterized in that a working electrode mounting port and an auxiliary electrode mounting port which are communicated with the solution cavity are respectively arranged at the bottom of the side surface of the electrolytic cell, a reference electrode mounting port which is communicated with the solution cavity is also arranged at the top of the electrolytic cell, and a gas pressurizing port which is communicated with the solution cavity is also arranged at the upper part of the side surface of the electrolytic cell; the working electrode and the auxiliary electrode are both of metal tubular structures; the working electrode and the auxiliary electrode are communicated with a solution cavity in the electrolytic cell through a mounting hole at the bottom of the side surface of the electrolytic cell, and the reference electrode is communicated with the solution cavity of the electrolytic cell through a mounting hole at the top of the electrolytic cell; the outer port of the working electrode metal tube and the outer port of the auxiliary electrode metal tube are respectively opposite to a sample inlet of the mass spectrometer;
after reaction liquid is injected into the solution cavity of the electrolytic cell, the reference electrode is fixed through a mounting opening at the top of the electrolytic cell, the measuring end of the reference electrode is immersed in the reaction liquid, and high-pressure gas is introduced into the solution cavity from the gas pressurizing opening, so that the working electrode and the auxiliary electrode metal tube are ensured to be filled with the reaction liquid; and connecting the working electrode, the auxiliary electrode and the reference electrode with an electrochemical workstation through leads, turning on a power supply of the electrochemical workstation, starting an electrochemical reaction, respectively ejecting electrochemical reaction products formed on the surfaces of the working electrode and the auxiliary electrode from an external port of the working electrode metal tube and an external port of the auxiliary electrode metal tube, respectively entering a mass spectrometer for detection, and realizing the synchronization and real-time monitoring of respective reaction products of a positive electrode and a negative electrode in the electrochemical reaction process.
2. The device for real-time synchronous monitoring of positive and negative electrode reaction products of electrochemistry according to claim 1, wherein the working electrode mounting port and the auxiliary electrode mounting port are both arranged at the bottom of the side surface of the electrolytic cell.
3. The device for real-time synchronous monitoring of products of electrochemical positive and negative reactions of claim 1, wherein the connection of the tubular metal electrode to the electrolytic cell is fixed at the mounting port by a ferrule-type end straight-through pipe joint; the ferrule type end straight pipe joint and the working electrode mounting opening are in sealing connection through threads.
4. The device for real-time synchronous monitoring of positive and negative electrochemical reaction products according to claim 1, wherein the reference electrode is also secured to the top mounting opening of the electrolytic cell by a ferrule type end feedthrough connection, and the ferrule type end feedthrough connection and the auxiliary electrode mounting opening are both in sealed connection by threads.
5. The device for real-time synchronous monitoring of products of electrochemical positive and negative electrode reactions according to claim 1, wherein the tubular metal electrode material is any one of platinum, copper and stainless steel.
6. The device for real-time synchronous monitoring of products of electrochemical positive and negative electrode reactions according to claim 5, wherein the metal tubular electrode has an inner diameter of 0.1mm, an outer diameter of 0.4mm to 0.8mm, and a length of 3cm to 4 cm.
7. The device for real-time synchronous monitoring of the products of the electrochemical positive and negative electrode reactions according to claim 1, wherein the electrolytic cell is made of an anti-corrosion material, and the anti-corrosion material is polyetheretherketone, or polytetrafluoroethylene, or quartz glass.
8. The device for real-time synchronous monitoring of the products of electrochemical positive and negative reactions as claimed in claim 1, wherein a fixing base is further disposed at the bottom of the electrolytic cell for fixing the electrolytic cell.
9. Method for real-time simultaneous monitoring of products of electrochemical positive and negative reactions using the device for real-time simultaneous monitoring of products of electrochemical positive and negative reactions according to any one of claims 1 to 8, characterized in that it comprises the following steps:
(1) aligning an outer port of a metal tubular working electrode to a sample inlet of a mass spectrometer, and inserting the other end of the working electrode into a working electrode mounting port at the bottom of the side surface of the electrolytic cell for sealing and fixed connection; aligning an outer port of a metal tubular auxiliary electrode to a sample inlet of a mass spectrometer, and inserting the other end of the auxiliary electrode into an auxiliary electrode mounting port at the bottom of the side surface of the electrolytic cell for sealing and fixed connection; after reaction liquid is injected into a solution cavity in the electrochemical reaction cell, the lower half part of the reference electrode is inserted into a reference electrode mounting port at the top of the electrolytic cell for sealing and fixing, and the measuring end of the reference electrode is immersed into the reaction liquid;
(2) connecting the working electrode, the auxiliary electrode and the reference electrode with an electrochemical workstation through leads, introducing high-pressure gas into a solution cavity in the electrolytic cell from the gas pressurizing port, ensuring that the interior of the metal tube of the metal tubular electrode is filled with reaction liquid, then turning on a power supply of the electrochemical workstation to initiate the electrochemical reaction of the reaction liquid in the working electrode and the auxiliary electrode metal tube, and simultaneously spraying reaction products generated on the surfaces of the working electrode and the auxiliary electrode to the outer end port of the metal tube of the metal tubular electrode to respectively enter a mass spectrometer for detection, thereby realizing the real-time synchronous monitoring of the electrochemical redox reaction products of the positive electrode and the negative electrode.
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