CN113049660A - Intelligent response device and method for monitoring reaction endpoint in liquid electrolyte - Google Patents
Intelligent response device and method for monitoring reaction endpoint in liquid electrolyte Download PDFInfo
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- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Inorganic materials [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 1
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- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/4161—Systems measuring the voltage and using a constant current supply, e.g. chronopotentiometry
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- Health & Medical Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides an intelligent response device for monitoring a reaction endpoint in liquid electrolyte, which comprises a direct-current power supply, a voltage comparator module, an indicator lamp, a buzzer alarm, an independent power supply, an inert metal cathode and a graphite anode, wherein the direct-current power supply is connected with the voltage comparator module; mainly divide into monitoring return circuit and response return circuit, monitoring return circuit includes: the device comprises a direct current power supply, a voltage comparator module, an inert metal cathode and a graphite anode; the response loop comprises an indicator light, a buzzer alarm and an independent power supply, and the two loops are connected through an overvoltage comparison module; the device can provide a clear visual signal for the outside to prompt the end point of the reaction in the liquid electrolyte; the device has the advantages that other elements are not introduced into a liquid electrolyte system, the pollution of the liquid electrolyte is avoided, the structure is simple and reliable, the maintenance is convenient, the learning cost is low in the using process, the operating process of the device can be mastered by a front-line operator through simple training, and the device can be applied to industrial production in a large scale.
Description
Technical Field
The invention relates to an intelligent response device and method, in particular to an intelligent response device and method for monitoring a reaction endpoint in a liquid electrolyte, and belongs to the field of electrochemical application.
Background
In the current industrial production process, the liquid electrolyte is widely applied, and many reaction processes need to be carried out in the liquid electrolyte, such as smelting and refining processes of many nonferrous metals and rare metals, electroplating processes, corrosion and protection processes of metals, electrophoretic paint spraying, sewage treatment processes and the like. In addition, with the continuous development of the nuclear industry and the continuous popularization of nuclear energy application, the post-processing process of the spent fuel is attracting more and more attention. In the field of post-treatment of spent fuels, liquid electrolytes (aqueous solutions, ionic liquids, molten salts) play an important role as reaction media, both in aqueous post-treatment and dry post-treatment. Extraction and recovery of nuclear fuels such as uranium (U) and plutonium (Pu) remaining in a spent fuel in large quantities and separation and removal of Fission Products (FP) such as rare earth elements are required to be performed in various liquid electrolytes.
At present, the reaction processes in the liquid electrolyte all face a common problem, namely, no simple and universal method is available for judging the reaction endpoint. Taking the electrodeposition process in liquid electrolyte as an example, in industrial production, it is difficult for operators to visually monitor the ion concentration in the system, which makes it difficult to judge the degree of progress of the deposition process and whether to continue feeding. Therefore, there is a need for a simple and easy-to-operate device for determining the end point of the reaction in the liquid electrolyte and responding to the outside in time.
Disclosure of Invention
The invention aims to provide a reaction end point judgment and intelligent response device for a reaction process in a liquid electrolyte. The end point of the reaction is monitored by an electrochemical method, and visual feedback information is provided for the outside.
The purpose of the invention is realized as follows:
an intelligent response device for monitoring a reaction endpoint in a liquid electrolyte comprises a direct-current power supply 1, a voltage comparator module 2, an indicator lamp 5, a buzzer alarm 6, an independent power supply 7, an inert metal cathode 3 and a graphite anode 4; mainly divide into monitoring return circuit and response return circuit, monitoring return circuit includes: the device comprises a direct current power supply 1, a voltage comparator module 2, an inert metal cathode 3 and a graphite anode 4; the response loop comprises an indicator lamp 5, a buzzer alarm 6 and an independent power supply 7, and the two loops are connected through an overvoltage comparison module 2.
The device is suitable for aqueous solution, ionic liquid and molten salt systems;
an intelligent response method for monitoring a reaction endpoint in a liquid electrolyte comprises the following steps:
step (1): determining the oxidation-reduction potential of the target reactant ions and the decomposition voltage of the electrolyte, and adjusting the set voltage of the voltage comparator module between the two;
step (2): inserting the two electrodes into a liquid electrolyte, and switching on a power supply to monitor the constant current;
and (3): when the liquid electrolyte contains reactant ions, the voltage of the monitoring loop is close to the oxidation-reduction potential of the monitoring loop and is smaller than the set voltage of the voltage comparator module, the indicator light is not on, and the buzzer alarm does not sound;
and (4): when the reaction end point is reached, the voltage of the monitoring loop end point rises to the electrolyte decomposition voltage and is greater than the set voltage of the voltage comparator module, the indicator lamp is turned on, the buzzer alarm gives an alarm, and the judgment and the alarm response of the reaction end point are finished.
Compared with the prior art, the invention has the beneficial effects that:
1. the method and the device monitor the reaction process in the liquid electrolyte based on the electrochemical principle and automatically respond, do not introduce other elements into the liquid electrolyte system, and do not cause the pollution of the liquid electrolyte;
2. the device can be used for the reaction process of any reactant ion with the oxidation-reduction potential being positive to the decomposition voltage of the liquid electrolyte;
3. the application of the device is not limited to a specific liquid electrolyte, and the device can be suitable for most liquid electrolyte systems by adjusting the set voltage of the voltage comparator module;
4. compared with the prior art, the device can provide a clear visual signal for the outside to prompt the end point of the reaction in the liquid electrolyte;
5. the device has simple and reliable structure, convenient maintenance and low learning cost in the using process, and the operating process of the device can be mastered by one-line operators through simple training and can be applied in industrial production on a large scale.
Drawings
Fig. 1 is a schematic circuit diagram of the device, in which 1 is a power supply, 2 is a voltage comparator module, 3 is an inert metal cathode, 4 is a graphite anode, 5 is an indicator light, 6 is a buzzer alarm, 7 is an independent power supply, and 8 is a switch;
FIG. 2 is an interface for voltage calibration using a serial port connected computer in the embodiment;
FIG. 3 shows Pr-containing for determining potential in example3+Cyclic voltammogram of LiCl-KCl melt of ionic impurities.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The invention relates to an intelligent response method and device for monitoring a reaction endpoint in a liquid electrolyte. The application range of the invention includes but is not limited to the judgment of the chemical precipitation endpoint of the rare earth praseodymium ions in the molten salt system mentioned in the embodiment.
The circuit diagram of the device is shown in fig. 1, and the device main body comprises a direct current power supply 1, a voltage comparator module 2, an inert cathode 3, a graphite anode 4, an indicator lamp 5, a buzzer alarm 6 and an independent power supply 7.
The operation process of judging the reaction end point in the liquid electrolyte by using the device comprises the following steps:
(1) before applying the device, the redox potential of the reactant ions and the decomposition voltage of the liquid electrolyte were measured using an electrochemical workstation.
(2) And the voltage comparator module is connected with a computer through a serial port to carry out voltage calibration, so that the voltage deviation is accurate to +/-0.1V.
(3) The upper threshold of the voltage comparator module is set between the redox potential of the reactant ions and the decomposition voltage of the liquid electrolyte, and the lower threshold of the voltage comparator module is set below the redox potential of the reactant ions. The response mode of the voltage comparator module is set to an off-threshold response (i.e., when the voltage exceeds the upper threshold set voltage, the voltage comparator module responds to close the normally open switch).
(4) After setting, the inert cathode and the graphite anode of the device are inserted into the liquid electrolyte which is undergoing reaction, the power supply is started, and constant current is adopted for monitoring.
(5) When the liquid electrolyte contains reactant ions, the monitoring loop terminal voltage will stabilize near the redox potential of the reactant ions.
(6) When the reaction end point is reached, the consumption of reactant ions is almost exhausted, the terminal voltage quickly rises to the vicinity of the decomposition voltage of the liquid electrolyte and exceeds the set upper threshold, the device judges that the reaction end point is reached, and the indicator lamp emits light and buzzes for alarming.
The liquid electrolyte system can be most common aqueous solution, ionic liquid, common chloride or fluoride fused salt such as LiCl-KCl, NaCl-CsCl, NaCl-KCl, FLiNaK, FLiBe-KF and the like;
the reactant ions may be ions with redox potentials at the decomposition voltage of the liquid electrolyte, such as one or more of lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, lutetium, iron, cobalt, nickel, copper, lead, aluminum, zinc, tin, and the like.
The present invention is further described with reference to the following drawings and examples, which are for reference purposes and can be modified in various ways without departing from the scope of the invention.
An intelligent response method and device for monitoring a reaction end point in a liquid electrolyte are disclosed, wherein based on the difference of oxidation-reduction potentials of different ions, the monitoring of the reaction process in the liquid electrolyte is realized by monitoring the voltage change, the reaction end point is judged, a response such as light-on, buzzing alarm and the like is automatically sent out at the reaction end point, and a module can be added according to actual requirements to realize functions such as automatic feeding, automatic stopping and the like. This device mainly divide into monitoring return circuit and response circuit, and the monitoring return circuit includes: the device comprises a direct current power supply (1), a voltage comparator module (2), an inert metal cathode (3) and a graphite anode (4); the response loop comprises an indicator lamp (5), a buzzer alarm (6) and an independent power supply (7), the two loops are connected through an over-voltage comparison module (2), and other elements can be added to the response loop according to specific requirements in practical application, so that functions of automatic feeding, automatic stopping and the like are realized.
The device is used for monitoring reactant ions in the liquid electrolyte based on an electrochemical method, judging the reaction end point and responding, and is characterized in that:
step (1): determining the oxidation-reduction potential of the target reactant ions and the decomposition voltage of the electrolyte, and adjusting the set voltage of the voltage comparator module between the two;
step (2): inserting the two electrodes into a liquid electrolyte, and switching on a power supply to monitor the constant current;
and (3): when the liquid electrolyte contains reactant ions, the voltage of the monitoring loop is close to the oxidation-reduction potential of the monitoring loop and is smaller than the set voltage of the voltage comparator module, the indicator light is not on, and the buzzer alarm does not sound;
and (4): when the reaction end point is reached, the voltage of the monitoring loop end point rises to the electrolyte decomposition voltage and is greater than the set voltage of the voltage comparator module, the indicator lamp is turned on, the buzzer alarm gives an alarm, and the judgment and the alarm response of the reaction end point are finished.
By adjusting the set voltage of the voltage comparator module, the device is suitable for various common liquid electrolyte systems including aqueous solutions, ionic liquids and molten salt systems. The reactant ions may be one or more ions having an oxidation-reduction potential positive to the decomposition voltage of the system, including but not limited to rare earth ions: lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, lutetium, and other metal cations: zirconium, iron, cobalt, nickel, copper, lead, aluminum, zinc, tin, and the like.
When the reaction end point is reached, the device can send easily-perceived signal feedback to the outside.
Example (b):
taking the chemical precipitation process of rare earth praseodymium ions in a molten salt system as an example, the liquid electrolyte is LiCl-KCl molten salt (mass ratio is 38: 45), reactant ions in the molten salt are praseodymium ions (2.6 wt.%), sodium phosphate is added for precipitation, and the operation temperature is 773K. The reaction end point of the precipitation process is judged by using the device.
In the embodiment, the molten salt to be purified is LiCl-KCl eutectic salt, wherein LiCl is 38g, KCl is 45g, impurity ions in the molten salt are praseodymium ions (2.6 wt.%), and the purification method is a sodium phosphate precipitation method. The molten salt was dried in a muffle furnace at 473K for 72 hours to remove the water from the solvent salt initially before purification, and then transferred to a box-type resistance furnace in a vacuum glove box and heated to 773K to melt it. After the molten salt melts and stabilizes, purification is started.
Cyclic voltammetry tests were performed on the LiCl-KCl molten salt containing praseodymium ions using an electrochemical workstation before the reaction to determine the deposition potential of the praseodymium ions and the decomposition voltage of the LiCl-KCl solvent salt, and the obtained curves are shown in fig. 3. In the figure, the oxidation reduction peak A/A' is Li/Li+Redox peak, B/B' is Pr/Pr3+Redox peak. It can be seen from the figure that the oxidation-reduction potential of praseodymium ion is-3.2V (vs Cl)2/Cl-) The decomposition voltage of LiCl-KCl solvent salt was-3.6V.
The voltage comparator module is connected with a computer by a serial port and is subjected to voltage calibration by XCOM software, and an interface is shown in FIG. 2, so that the voltage deviation is not more than 0.1V.
The upper threshold of the voltage comparator block is set to-3.6V (vs Cl) based on the measured potential value of cyclic voltammetry2/Cl-) The lower threshold is set to 0V (vs Cl)2/Cl-) The response mode is set to an off-threshold response.
The cathode of the detection loop uses an inert tungsten electrode with a diameter of 1.0mm and a purity of 99.99%. The anode used a spectrally pure graphite rod with a diameter of phi (6.0 mm).
And adding the inert tungsten electrode and the graphite electrode which are subjected to cleaning treatment into LiCl-KCl molten salt containing praseodymium ions, wherein the cathode immersion depth is 1.0 cm.
The power supply is turned on, the monitoring loop is monitored by constant current of 8mA, and in the molten salt purification process, the monitoring loopThe terminal voltage is stabilized at praseodymium ion oxidation-reduction potential (-3.2V (vs Cl)2/Cl-) Near).
Sodium phosphate was added to the molten salt stepwise and allowed to stand for 30 minutes after each addition to allow the praseodymium ions to precipitate sufficiently. After a period of time, the praseodymium ions are nearly completely precipitated, the end voltage of the monitoring loop is increased to the decomposition voltage (-3.6V) of LiCl-KCl solvent salt, the chemical precipitation of the praseodymium ions is completed, the end voltage of the monitoring loop exceeds the upper threshold to set an alarm potential, the voltage comparator module responds, the normally open switch is closed, the indicator lamp is turned on, the buzzer alarms, and the chemical precipitation process of the praseodymium ions in the external molten salt is prompted to reach the end point.
When the reaction end point is reached, the power supply of the device is closed, the sodium phosphate is stopped being added, the molten salt supernatant is sampled for ICP test, and the result shows that the precipitation rate can reach 98.70%.
The invention provides a device for monitoring a reaction endpoint in a liquid electrolyte and responding, wherein a device main body comprises a direct-current power supply, a voltage comparator module, an indicator light, a buzzer alarm, an independent power supply, an inert metal cathode and a graphite anode. Constant current is conducted to two electrodes inserted into the liquid electrolyte, and terminal voltage change is monitored to judge whether a reaction terminal point is reached; when the reaction terminal point is reached, the indicator lamp of the device is turned on, the buzzer alarm gives an alarm, the external environment is fed back easily, and intelligent judgment and response of the reaction terminal point are realized. The device has wide application range, sensitive indication and simple structure, and can provide visual signal feedback to the outside.
In summary, the present invention provides an intelligent response method and apparatus for monitoring the reaction endpoint in liquid electrolyte. The voltage change is monitored through constant current electrolysis, the voltage comparator module is used for analyzing and judging the voltage, when the reaction end point is reached, the voltage comparator module sends out a response, and the indicating lamp and the buzzer alarm give an alarm to the outside. The invention converts the reaction condition in the liquid electrolyte into easily-perceived sound and light signals, and provides convenience for judging the end point of the reaction process in the liquid electrolyte. Meanwhile, the device has the advantages of simple structure, low cost, low requirement on the use environment, wide application range and suitability for commercial production.
Claims (3)
1. An intelligent response device for monitoring a reaction endpoint in liquid electrolyte is characterized by comprising a direct-current power supply (1), a voltage comparator module (2), an indicator lamp (5), a buzzer alarm (6), an independent power supply (7), an inert metal cathode (3) and a graphite anode (4); mainly divide into monitoring return circuit and response return circuit, monitoring return circuit includes: the device comprises a direct current power supply (1), a voltage comparator module (2), an inert metal cathode (3) and a graphite anode (4); the response loop comprises an indicator lamp (5), a buzzer alarm (6) and an independent power supply (7), and the two loops are connected through an overvoltage comparison module (2).
2. An intelligent response unit for monitoring the end point of a reaction in a liquid electrolyte as claimed in claim 1, wherein the unit is suitable for use in aqueous solutions, ionic liquids and molten salt systems.
3. An intelligent response method for monitoring a reaction endpoint in a liquid electrolyte, comprising the steps of:
step (1): determining the oxidation-reduction potential of the target reactant ions and the decomposition voltage of the electrolyte, and adjusting the set voltage of the voltage comparator module between the two;
step (2): inserting the two electrodes into a liquid electrolyte, and switching on a power supply to monitor the constant current;
and (3): when the liquid electrolyte contains reactant ions, the voltage of the monitoring loop is close to the oxidation-reduction potential of the monitoring loop and is smaller than the set voltage of the voltage comparator module, the indicator light is not on, and the buzzer alarm does not sound;
and (4): when the reaction end point is reached, the voltage of the monitoring loop end point rises to the electrolyte decomposition voltage and is greater than the set voltage of the voltage comparator module, the indicator lamp is turned on, the buzzer alarm gives an alarm, and the judgment and the alarm response of the reaction end point are finished.
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