CN112946046B - Online detection method for uranium content in fuel salt of molten salt reactor - Google Patents
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Abstract
The invention provides an online detection method for uranium content in molten salt reactor fuel salt, which comprises the following steps: 1) There is provided an electrochemical on-line detection device comprising: a working electrode, a counter electrode and a reference electrode respectively connected with the electrochemical workstation; 2) Pretreatment of fuel salt: filtering fuel salt through a sintered nickel filter element; 3) Electrochemical online detection: immersing a working electrode, a counter electrode and a reference electrode in fuel salt, applying a variable voltage through an electrochemical workstation, detecting current flowing through the working electrode, and scanning in a certain potential range by adopting square wave voltammetry to realize online detection, wherein the steps comprise two substeps: a. measuring a standard curve of the correspondence relation between uranium concentration and peak current density in fuel salt; b. and detecting the uranium content in the fuel salt to be detected. According to the invention, the real-time detection of the uranium concentration in the fuel salt in the operation process of the molten salt reactor can be realized, and the sampling, split charging, sample dissolving and detection under the strong radiation environment are avoided.
Description
Technical Field
The invention belongs to the technical field of electrochemical detection methods, and particularly relates to an online detection method for uranium content in molten salt reactor fuel salt.
Technical Field
The molten salt nuclear reactor (Molten Salt Reactor) is the only one of the six fourth generation nuclear energy systems internationally recognized at present, wherein liquid fluorine molten salt is used as fuel in a first loop, and liquid fluorine molten salt is also used as a second loop coolant. Compared with the current third-generation reactor in service, the operation is close to normal pressure, so that the inherent safety of the reactor is improved; the liquid fuel is convenient for on-line nuclear fuel post-treatment, and the cyclic utilization of the nuclear fuel is realized; high thermal power density, relatively simple core structure, convenient miniaturization and the like.
The molten salt reactor has higher safety, and adopts high-temperature liquid fluorine molten salt as nuclear fuel and also as heat carrier, and does not need to specially manufacture fuel components, thereby avoiding the occurrence of reactor core melting accidents; in addition, the low vapor pressure of the liquid fuel salt reduces the occurrence of core breach accidents, and even if the breach accidents occur, the liquid fuel salt can be quickly solidified at the ambient temperature, so that the accidents can be prevented from being further expanded.
The molten salt reactor liquid fuel mainly comprises FLiBeU, FLiBeUTh, FLiBeZrU, FLiBeZrUTh and the likeType, only the American oak-ridge national laboratory (ORNL) will fliBeZrU (LiF-BeF) 2 -ZrF 4 -UF 4 Prepared in a certain proportion) as a liquid fuel salt for Molten Salt Reactors (MSREs). The effect of Zr in FLiBeZrU is mainly to mask UO 2 If UO occurs during operation of the molten salt reactor 2 Precipitation may then cause nuclear critical safety accidents. Under high water-oxygen conditions, zr will preferentially react with O 2- Combine to form ZrO 2 Precipitation to avoid U and O 2- Combining to generate UO 2 Precipitation, but Zr pair inhibits UO 2 Is limited, it has been found that when the Zr/U molar ratio in the liquid fuel salt is below a certain value, the water-oxygen content in the environment increases and ZrO of the fuel salt occurs 2 -UO 2 The coprecipitation reaction simultaneously causes the reduction of uranium concentration in the liquid fuel, and threatens the safe operation of the reactor. Therefore, how to obtain the uranium concentration data in the fuel salt in real time in the operation process of the molten salt reactor, and to judge whether UO occurs 2 The precipitation reaction has great significance. The traditional liquid fuel salt uranium concentration detection is carried out in an online sampling and offline detection mode, the sampling process is complicated, the fuel salt sample taken out of the reactor core has strong radioactivity, ICP-AES or ICP-MS analysis is needed to be carried out in a hot chamber through a manipulator, and sample processing and detection process operation in the hot chamber are more difficult, so that a method capable of detecting the uranium concentration in the liquid fuel salt in real time in the operation process of the molten salt reactor is very needed, and the method is the problem to be solved.
Disclosure of Invention
The invention aims to provide an online detection method for the uranium content in molten salt reactor fuel salt, so as to solve the technical blank of the online detection method for the uranium content in high-temperature liquid fuel salt in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
the online detection method for uranium content in fuel salt of molten salt reactor comprises the following steps: 1) There is provided an electrochemical online detection apparatus comprising: respectively and electrochemically work withA working electrode, a counter electrode and a reference electrode which are connected by a station, wherein the reference electrode is Ni/NiF 2 A fuel salt reference electrode; 2) Pretreatment of fuel salt: filtering fuel salt through a sintered nickel filter core at 550-700 ℃ to remove insoluble matters in the fuel salt; 3) Electrochemical online detection: immersing the working electrode, the counter electrode and the reference electrode into liquid fuel salt, applying variable voltage to the working electrode and the counter electrode through an electrochemical workstation, detecting current flowing through the working electrode along with the change of the applied voltage, scanning in a certain potential range by adopting square wave voltammetry, and realizing on-line detection of uranium concentration in the liquid fuel salt, wherein the method comprises the following two sub-steps: a. determination of a standard curve of correspondence between uranium concentration and peak current density in fuel salt: heating fuel salts with known different uranium concentrations to a certain temperature for melting, and scanning by adopting a square wave voltammetry in a certain potential range to obtain a uranium reduction peak, thereby obtaining a corresponding relation standard curve of the uranium concentration and the peak current density; b, detecting uranium content in the fuel salt to be detected: and c, heating the fuel salt to be detected with unknown uranium concentration to a certain temperature for melting, detecting the peak current density of a uranium reduction peak in a certain potential range by adopting square wave voltammetry, and obtaining the uranium content in the fuel salt to be detected according to the corresponding relation standard curve of the uranium concentration and the peak current density obtained in the step a.
The Ni/NiF in step 1) 2 The preparation of the fuel salt reference electrode comprises the following steps: adding anhydrous FLiBeZr solid powder into a silicon nitride sleeve, and adding anhydrous NiF into the silicon nitride sleeve according to a certain proportion 2 Solid powder, anhydrous FLiBeZr and anhydrous NiF 2 Inserting nickel wires into the mixed solid powder of (a) and ensuring the connection of the nickel wires and the electrode rod to prepare Ni/NiF 2 A fuel salt reference electrode.
Wherein, the nickel wire is physically connected with the electrode rod to ensure conductivity, and anhydrous LiF-BeF with certain quality 2 -ZrF 4 After the solid powder (FLiBeZr) is added into the sleeve, the nickel wire is inserted into the bottom of the powder, so that the internal reference liquid can be conducted with the electrode rod after high-temperature melting.
Preferably, in step 1), anhydrous FLiBeZr and anhydrous NiF 2 Molar ratio of (3)Is (15-19) to 1.
Preferably, the Ni/NiF in step 1) 2 The side wall of the bottom end of the silicon nitride sleeve of the fuel salt reference electrode is polished to the thickness of 0.5-1.0 mm on the outer wall so as to ensure the Ni/NiF in the sleeve 2 The fuel salt is communicated with the fuel salt outside the sleeve.
Preferably, the working electrode in the step 1) is linear, the outer diameter is not more than 2mm, the material is one of Pt, pd, au, W and Mo, and the counter electrode is a cylindrical graphite electrode with the diameter not less than 40 mm.
Preferably, the on-line detection temperature of the fuel salt in both sub-step a and sub-step b in step 3) is 500-600 ℃.
It will be appreciated that in step 1) the silicon nitride sleeve is immersed in a fuel salt, and that in order to accelerate the passage of the silicon nitride sleeve between the internal reference salt and the fuel salt outside the sleeve, a suitable polishing thickness must be selected according to the measured temperature, typically at 500-600 c, the silicon nitride passage thickness being 0.5-1.0 mm.
Preferably, in step 2) the fuel salt is filtered by using a sintered nickel filter element, the pore diameter of the filter element is not more than 30 μm, the filtering temperature is not more than 700 ℃, and the Ni content in the filtered fuel salt is less than 50ppm, because the filtering step also comprises the step of filtering large-particle Ni in the fuel salt, thereby avoiding Ni 2+ And has influence on electrochemical detection.
Preferably, the online detection of the uranium concentration in the fuel salt by square wave voltammetry in substep a and substep b in step 3) uses a potential range of-1.4 to-1.1V within which U occurs 4+ Conversion to U 3+ Is a reduction reaction of (a).
Preferably, the frequency range adopted in the sub-step a and the sub-step b in the step 3) for online detection of the uranium concentration in the fuel salt by adopting square wave voltammetry is 5-50 Hz, and after the unidirectional square wave voltammetry scanning is finished, the cyclic voltammetry scanning can be carried out within the range of-0.8-0.1V for not less than 3 circles, so that U generated by reduction is reduced 3+ Reconversion to U 4+ 。
Preferably, steps 1) to 3) are all carried out in an environment having a water-oxygen content of less than 5 ppm.
Preferably, the Ni/NiF in step 1) 2 The anhydrous FLiBeZr solid powder used in the preparation of the fuel salt reference electrode is LiF-BeF 2 -ZrF 4 The fuel salt to be measured is LiF-BeF 2 -ZrF 4 -UF 4 。
The invention provides an online detection method for uranium content in molten salt reactor fuel salt, which comprises the following detection principles: filtering fuel salt with known U concentration, putting into an electric heating furnace with water-oxygen content less than 1ppm for melting, inserting three electrodes connected with an electrochemical workstation into liquid molten salt to form a measuring loop, and obtaining known different U concentrations and U4 by adopting square wave voltammetry + And finally, obtaining the U concentration of the fuel salt to be detected by measuring the current density of the unknown U concentration according to the corresponding relation curve of the reduction peak current density.
Compared with the prior art, the invention has the beneficial effects that: according to the electrochemical online detection method for the uranium concentration in the fuel salt of the molten salt reactor, provided by the invention, the uranium concentration in the fuel salt can be detected in real time in the running process of the molten salt reactor, and a series of complicated operations such as sampling, split charging, sample dissolving and detection in a strong radiation environment can be avoided; and obtaining a standard curve by adopting cold fuel salts with different uranium concentrations in advance through an electrochemical square wave voltammetry under the operation condition of the molten salt reactor, and then carrying out the temporary reactor detection of the uranium content in the fuel salts. Comparing the online detection method with the offline ICP analysis result, the error of the electrochemical online detection method is less than 5% in the range of 0.4-1.1 mol% of U concentration, and further proves the reliability of the online detection method for uranium concentration, which is significant for the safe operation of the high-temperature liquid molten salt reactor.
Drawings
FIG. 1 is a schematic diagram of an electrochemical online detection device for uranium concentration in fuel salt according to a preferred embodiment of the present invention;
FIG. 2 is a square wave voltammogram of example 1 for different U concentrations versus peak current densities;
FIG. 3 is a plot of the fit of different U concentrations to the corresponding peak current densities in example 1;
in the figure:
1. glove box 7, thermocouple
2. Sealing separator 8, reference electrode
3. Cooling water circulation 9, pure nickel crucible
4. Conductive electrode rod 10 and electric heating furnace
5. Working electrode 11, electrochemical workstation
6. Counter electrode
Detailed Description
The invention will be further illustrated with reference to specific examples. It should be understood that the following examples are illustrative of the present invention and are not intended to limit the scope of the present invention.
As shown in fig. 1, an electrochemical online detection device for uranium concentration in fuel salt according to a preferred embodiment of the present invention includes: the device comprises a glove box 1, a sealing partition plate 2, circulating cooling water 3, a conductive electrode rod 4, a working electrode 5, a counter electrode 6, a thermocouple 7, a reference electrode 8, a pure nickel crucible 9, an electric heating furnace 10 and an electrochemical workstation 11.
In the device, a glove box 1 is adopted to provide an anhydrous and anaerobic inert atmosphere environment, and U in fuel salt is very sensitive to water and oxygen, so UO is very easy to generate 2 The environment for detecting the concentration of U is precipitated, so that water and oxygen must be isolated in an inert atmosphere, and therefore, the environment with the water and oxygen content of less than 1ppm is preferably provided through the glove box 1 so as to meet the condition of on-line detection of the concentration of uranium. The sealing partition plate 2 is used for sealing the junction of the glove box 1 and the electric heating furnace 10. The pure nickel crucible 9 is arranged in the electric heating furnace 10 and is used for containing liquid molten salt, the lower ends of the working electrode 5, the counter electrode 6 and the reference electrode 8 are respectively immersed in the liquid molten salt, the upper ends of the working electrode 5, the counter electrode 6 and the reference electrode 8 are respectively connected with the electrochemical workstation 11 through the conductive electrode rod 4, the thermocouple 7 is used for measuring temperature, and the circulating cooling water 3 is used for cooling the junction of the glove box 1 and the electric heating furnace 10.
When the electrochemical on-line detection device shown in fig. 1 is used for electrochemical measurement, the working electrode 5, the counter electrode 6 and the reference electrode 8 are immersed in the liquid molten salt, respectively, to a depth of immersionThe three electrodes are connected with the electrochemical workstation 11 through the conductive electrode rod 4 and the scanning potential is applied to the electrodes through the electrochemical workstation 11 to enable the U concentration to correspond to the reduction peak current density, so that for fuel salt with unknown U concentration, only U needs to be measured 4+ To U (U) 3+ The U concentration value can be obtained through the reduction peak current density of the (C).
Example 1:
the bottom side wall of a silicon nitride sleeve of 2mm thickness was polished to 0.5mm, and then 5.5g of anhydrous LiF-BeF was added to the silicon nitride sleeve 2 -ZrF 4 (FLiBeZr) solid powder, and then adding anhydrous NiF in a molar ratio of 19:1 2 0.68g of pure nickel wire with the diameter of 1mm is inserted into the electrode rod, the pure nickel wire is connected with the electrode rod, and the Ni/NiF is prepared after encapsulation 2 A reference electrode.
And respectively placing fuel salt FLiBeZrU with the content of 100g U of 0.0%, 0.3%, 0.6%, 0.9% and 1.1% (mol%) in a sintered nickel filter core, wherein the pore diameter of the filter core is 20 mu m, and performing pressure filtration at 700 ℃ to obtain the fuel salt meeting electrochemical measurement. Loading fuel salts with different U contents into a pure nickel crucible, placing into a hearth with water-oxygen content less than 1ppm, heating to 600 ℃ for melting, respectively inserting W wires with outer diameter of 1mm into melted FLiBeZrU as working electrodes, respectively inserting spectral pure graphite rods with outer diameter of 4mm as counter electrodes, wherein the insertion depths of the working electrodes and the counter electrodes are 7mm, and Ni/NiF 2 The reference electrode insertion depth is 10mm, the three electrodes are connected with an electrochemical workstation, a reduction peak of U4 < + > is obtained by scanning in a range of-1.4 to-1.1V by adopting square wave voltammetry, square wave voltammetry curves with different U concentrations shown in figure 2 are obtained, and a relation curve of the U concentration and the peak current density (shown in figure 3) is obtained:
filtering fuel salt with unknown U concentration, and performing square wave voltammetry scanning under the same condition to obtain U 4+ The reduction peak current density of (C) was 45 mA.cm -3 The U concentration in the unknown fuel salt was found to be 0.59mol% by taking into account the above equation.
Example 2:
the bottom side wall of a silicon nitride sleeve of 2mm thickness was polished to 1mm, and then 6g of anhydrous LiF-BeF was added to the silicon nitride sleeve 2 -ZrF 4 (FLiBeZr) solid powder, and then adding anhydrous NiF in a molar ratio of 19:1 2 0.74g of pure nickel wire with the diameter of 1mm is inserted into the electrode rod, the pure nickel wire is connected with the electrode rod, and the Ni/NiF is prepared after encapsulation 2 A reference electrode.
The fuel salt FLiBeZrU with the content of 100g U of 0.2 percent, 0.4 percent, 0.7 percent, 1.0 percent and 1.1 percent (mol percent) is respectively put into a sintered nickel filter core, the pore diameter of the filter core is 30 mu m, and the fuel salt which accords with electrochemical measurement is obtained through pressurized filtration under the condition of 650 ℃. Loading fuel salts with different U contents into a pure nickel crucible, heating to 550 ℃ in a hearth with water-oxygen content less than 1ppm for melting, respectively inserting Mo wires with the outer diameter of 1mm into melted FLiBeZrU as working electrodes, respectively inserting a spectrum pure graphite rod with the outer diameter of 4mm as a counter electrode, wherein the insertion depths of the working electrode and the counter electrode are 9mm, and Ni/NiF 2 The reference electrode insertion depth is 12mm, the three electrodes are connected with an electrochemical workstation, and the U is obtained by scanning in the range of-1.4 to-1.1V by adopting square wave voltammetry 4+ Obtaining square wave volt-ampere curves with different U concentrations, and obtaining a relation curve of the U concentration and the peak current density:
filtering fuel salt with unknown U concentration, and performing square wave voltammetry scanning under the same condition to obtain U 4+ The reduction peak current density of (C) was 32 mA.cm -3 The U concentration in the unknown fuel salt was found to be 0.41mol% by taking into account the above equation.
Example 3:
according to the electrochemical online detection method for the uranium concentration in the molten salt reactor fuel salt, provided by the invention, the online detection method is compared with an offline ICP analysis result, and as shown in the following table 1, the error of the electrochemical online detection method is less than 5% within the range of 0.4-1.1 mol% of U concentration.
TABLE 1 comparison of electrochemical on-line analysis of U concentration in fuel salts with ICP-AES off-line analysis
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and various modifications can be made to the above-described embodiment of the present invention. All simple, equivalent changes and modifications made in accordance with the claims and the specification of the present application fall within the scope of the patent claims. The present invention is not described in detail in the conventional art.
Claims (7)
1. The online detection method for the uranium content in the fuel salt of the molten salt reactor is characterized by comprising the following steps of:
1) There is provided an electrochemical online detection apparatus comprising: a working electrode, a counter electrode and a reference electrode respectively connected with the electrochemical workstation, wherein the reference electrode is Ni/NiF 2 A fuel salt reference electrode, the Ni/NiF 2 The preparation of the fuel salt reference electrode comprises the following steps: adding anhydrous FLiBeZr solid powder into the silicon nitride sleeve with polished bottom side wall, and adding anhydrous NiF into the silicon nitride sleeve according to a certain proportion 2 Solid powder, anhydrous FLiBeZr and anhydrous NiF 2 The nickel wire is inserted into the mixed solid powder of (2) and is ensured to be connected with the electrode rod, and the internal reference liquid can be conducted with the electrode rod after high-temperature melting, thus preparing the Ni/NiF 2 A fuel salt reference electrode;
2) Pretreatment of fuel salt: liF-BeF 2 -ZrF 4 -UF 4 Filtering fuel salt through a sintered nickel filter core at 550-700 ℃ to remove insoluble matters in the fuel salt;
3) Electrochemical online detection: immersing the working electrode, the counter electrode and the reference electrode in a liquid fuel salt, applying a variable voltage across the working electrode and the counter electrode by an electrochemical workstation, and detecting the change in the applied voltage across the working electrodeIs scanned in a certain potential range by adopting square wave voltammetry to realize LiF-BeF 2 -ZrF 4 -UF 4 The on-line detection of uranium concentration in liquid fuel salt comprises the following two sub-steps:
a. determination of a standard curve of correspondence between uranium concentration and peak current density in fuel salt: taking LiF-BeF with known uranium concentrations 2 -ZrF 4 -UF 4 Heating fuel salt to a certain temperature for melting, and scanning by adopting square wave voltammetry in a certain potential range to obtain a uranium reduction peak, thereby obtaining a corresponding relation standard curve of uranium concentration and peak current density; and
b. detecting uranium content in fuel salt to be detected: taking LiF-BeF to be measured with unknown uranium concentration 2 -ZrF 4 -UF 4 Heating the fuel salt to a certain temperature for melting, detecting the peak current density of a uranium reduction peak in a certain potential range by adopting square wave voltammetry, and obtaining the uranium content in the fuel salt to be detected according to the corresponding relation standard curve of the uranium concentration and the peak current density obtained in the substep a;
in the substep a and the substep b, the frequency range adopted for online detection of the uranium concentration in the fuel salt by adopting square wave voltammetry is 5-50 Hz, and after unidirectional square wave voltammetry scanning is finished, cyclic voltammetry scanning can be carried out within the range of-0.8-0.1V for not less than 3 circles, so that U is formed 3+ Complete conversion to U 4+ 。
2. The online detection method according to claim 1, wherein in step 1), anhydrous FLiBeZr and anhydrous NiF are used 2 The mol ratio of (15-19) to 1.
3. The online detection method according to claim 2, wherein the Ni/NiF in step 1) is 2 The thickness of the bottom side wall of the silicon nitride sleeve of the fuel salt reference electrode is 0.5-1.0 mm so as to ensure the Ni/NiF in the sleeve 2 The fuel salt is communicated with the fuel salt outside the sleeve.
4. The online detection method according to claim 1, wherein the working electrode in step 1) is one of Pt, pd, au, W and Mo, and the counter electrode is a cylindrical graphite electrode having a diameter of not less than 40 mm.
5. The online detection method according to claim 1, wherein the online detection temperature of the fuel salt in sub-step a and sub-step b in step 3) is 500 to 600 ℃.
6. The online detection method according to claim 1, wherein steps 1) to 3) are performed in an environment where the water-oxygen content is less than 5 ppm.
7. The online detection method according to claim 1, wherein the Ni/NiF in step 1) 2 The anhydrous FLiBeZr solid powder used in the preparation of the fuel salt reference electrode is LiF-BeF 2 -ZrF 4 。
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