Experimental device and method for dissolution and chemical reaction process of material in liquid medium

Abstract

The invention provides an experimental device and an experimental method for dissolution and chemical reaction processes of a material in a liquid medium. The invention discloses an experimental device for dissolution and chemical reaction processes of a material in a liquid medium. The experimental device comprises a measuring assembly, a heating assembly, a reactor and a discharging assembly, the discharging assembly comprises a rod part, a first magnetic attraction part and a second magnetic attraction part, the solid sample is hung on the rod part, the second magnetic attraction part is arranged on the outer side of the top cover, and the second magnetic attraction part and the first magnetic attraction part are attracted so as to fix the solid sample above the reaction solution; when the parameters in the cylinder body meet the preset conditions, the second magnetic attraction part is controlled to be separated from the first magnetic attraction part, so that the solid sample is put into the reaction solution. The experimental device for the dissolution and chemical reaction process of the material in the liquid medium is established, and the dissolution process of different materials in the reaction medium, the complex chemical reaction process between the different materials and the complex chemical reaction process between the different materials and the reaction medium can be conveniently simulated under the specified temperature condition.

Description

Technical Field

[0001] The present invention relates to the field of simulation experiments, and in particular to an experimental device and an experimental method for the dissolution and chemical reaction process of a material in a liquid medium. Background Art

[0002] A loss-of-coolant accident (LOCA) in a reactor occurs when there is a large rupture in the primary circuit of the reactor. The coolant replenishment capacity is insufficient to compensate for the loss through the rupture, causing the core to gradually lose cooling, resulting in the fuel rod cladding heating up or even burning.

[0003] After a reactor loss of coolant (LOCA) accident, the containment vessel is exposed to a complex and harsh environment. Certain structural and insulation materials, such as those used in the reactor, corrode or decompose with the leaked coolant, reacting to form new compounds. When the ambient temperature changes, these compounds exceed their solubility limits and precipitate, adhering to the filter screen with the solution flow. This negatively impacts the filter screen's pressure drop and reduces the reliability of the circulating pumps in the safety injection and residual heat removal systems.

[0004] Chinese patent CN 111624297 A reports a bench test system and method for evaluating the chemical effects of nuclear power plant accidents. The system and method can provide test data on the dissolution and precipitation of materials in the containment under special water chemical conditions after the accident.

[0005] However, the devices currently used in China for conducting relevant tests all adopt the sequence of first mixing the test material and the reaction solution, and then increasing the temperature and pressure to the specified reaction conditions for testing. In actual engineering practice, the material and reaction solution after LOCA first react under high temperature and high pressure conditions, and then gradually cool down. Therefore, the current domestic test equipment cannot fully reproduce the actual LOCA process and cannot achieve the mixing of the test material and the reaction solution after reaching the specified temperature and pressure conditions. In order to more accurately evaluate the chemical effects of structural materials, insulation materials, and components in the containment after LOCA, how to build an experimental device for the dissolution and chemical reaction process of materials in liquid media has become a technical problem that needs to be solved urgently.

[0006] Therefore, technicians in this field are committed to developing an experimental device and experimental method for the dissolution and chemical reaction process of materials in liquid media to solve the problems existing in the prior art. Summary of the Invention

[0007] In view of the defects in the prior art, the purpose of the present invention is to provide an experimental device and an experimental method for the dissolution and chemical reaction process of a material in a liquid medium.

[0008] According to the present invention, an experimental device for the dissolution and chemical reaction process of a material in a liquid medium comprises a measuring component, a heating component, a reactor and a discharge component;

[0009] The reactor comprises a top cover and a barrel, wherein the barrel is used to hold the reaction solution and provide a chemical reaction space;

[0010] The measuring component is used to measure parameters inside the barrel;

[0011] The heating component is arranged in the barrel and is used to increase the temperature of the reaction solution in the barrel;

[0012] The discharge assembly includes a rod, a first magnetic component and a second magnetic component. The rod is connected to the first magnetic component and is arranged on the inner side of the top cover. The solid sample is suspended on the rod. The second magnetic component is arranged on the outer side of the top cover. The second magnetic component is attracted to the first magnetic component to fix the solid sample above the reaction solution. When the parameters in the cylinder body meet the preset conditions, the second magnetic component is controlled to separate from the first magnetic component to put the solid sample into the reaction solution.

[0013] Preferably, the parameter in the barrel includes a pressure value in the barrel, and the preset condition includes that the pressure value exceeds a preset pressure threshold; and / or

[0014] The temperature of the reaction solution in the cylinder body, the preset condition includes that the temperature value exceeds a preset temperature threshold.

[0015] Preferably, one end of the rod is tactilely connected to the top cover, and the other end is connected to the first magnetic element, and the solid sample is suspended on the rod by a wire;

[0016] When the second magnetic element is attracted to the first magnetic element, the rod remains horizontal to fix the solid sample above the reaction solution; when the second magnetic element is separated from the first magnetic element, the rod tilts to put the solid sample suspended on the rod into the reaction solution.

[0017] Preferably, the measuring component includes

[0018] a temperature sensor, the temperature sensor being electrically connected to the heating component and being used to measure the temperature of the reaction solution; and / or

[0019] A pressure gauge is used to measure the pressure inside the cylinder.

[0020] Preferably, it is characterized in that it further includes a cooling component and a support leg, the support leg is installed at the lower part of the barrel, one end of the cooling component is connected to the bottom end of the barrel, and the other end serves as an outlet for the liquid medium.

[0021] Preferably, one end of the cooling assembly is connected to the cylinder body through a control valve, and the other end is provided with a control valve.

[0022] Preferably, the first magnetic member is a rotatable magnetic sheet;

[0023] The second magnetic attraction component is a detachable magnetic attraction sheet or an electromagnet.

[0024] Preferably, the heating component is a thermocouple; and / or,

[0025] The cooling component is a condenser.

[0026] Preferably, the reaction solution is TSP or NaOH; and / or,

[0027] Solid samples are alkali-free glass cloth, pure zinc or low alloy steel.

[0028] According to the present invention, an experimental method based on the experimental device for the dissolution and chemical reaction process of the material in the liquid medium is provided, and the experimental method comprises the following steps:

[0029] S1, cleaning the reactor and injecting the reaction medium;

[0030] S2. Hanging the solid sample to be tested on the rod through a silk thread;

[0031] S3, disposing the second magnetic element on the outside of the top cover to engage with the first magnetic element on the inside of the top cover to suspend the solid sample to be tested above the reaction solution;

[0032] S4, controlling the heating component and the measuring component to operate, and when the measuring component measures that the parameters in the barrel meet a preset condition, removing the second magnetic element from the top cover, or disconnecting the second magnetic element from the power supply, so as to separate the first magnetic element from the second magnetic element, thereby placing the solid sample to be tested into the reaction solution for contact reaction therewith;

[0033] S5. After the specified reaction time is reached, samples are taken from the sampling port of the cooling component, and the chemical composition thereof is detected to obtain the element release rate curve of the test material, and to evaluate the interaction effects between the test material and the reaction medium, as well as between different test materials.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] 1. The present invention builds an experimental device for the dissolution and chemical reaction process of materials in liquid media, which can easily simulate the dissolution process of different materials in the reaction medium under specified temperature conditions, and the complex chemical reaction process between different materials and between them and the reaction medium.

[0036] 2. The present invention can simulate and accurately study the behavior of elements released from representative materials in the containment after LOCA.

[0037] 3. The present invention designs experimental equipment and experimental steps to address the defect that the types and compositions of compounds formed after the reaction of different materials under high temperature conditions are still unclear. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Other features, objects and advantages of the present invention will become more apparent upon reading the detailed description of non-limiting embodiments with reference to the following drawings:

[0039] Figure 1 It is a structural schematic diagram of the present invention;

[0040] The figure shows:

[0041] DETAILED DESCRIPTION

[0042] The present invention will be described in detail below with reference to specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that, for those skilled in the art, several changes and improvements can be made without departing from the scope of the present invention. These all fall within the scope of protection of the present invention.

[0043] The present invention provides an experimental device for the dissolution and chemical reaction process of materials in liquid media, which is used to simulate the dissolution process of different materials in reaction media under specified temperature conditions, and the complex chemical reaction processes between different materials and between different materials and reaction media. The experimental device for the dissolution and chemical reaction process of materials in liquid media includes a measuring component, a heating component, a reactor, and a discharge component. The reactor includes a top cover 42 and a barrel 41. The top cover 42 is detachably mounted on the top of the barrel 41. The barrel 41 is used to hold a reaction solution and provide a chemical reaction space. The measuring component is used to measure parameters within the barrel 41. The heating component is located within the barrel 41 and is used to increase the temperature of the reaction solution within the barrel 41. The discharge component includes a rod 6, a first magnetic element, and a second magnetic element. The rod 6 is connected to the first magnetic element and is located inside the top cover 42. The solid sample is suspended on the rod 6. The second magnetic element is located outside the top cover 42 and engages with the first magnetic element to fix the solid sample above the reaction solution. When the parameters within the barrel 41 meet preset conditions, the second magnetic element is controlled to separate from the first magnetic element to allow the solid sample to be dropped into the reaction solution. When using this device, the operator can discharge the material without lifting the cover, which will not disrupt the environment within the barrel.

[0044] Specifically, the parameters in the barrel 41 include the pressure value in the barrel 41, and the preset conditions include the pressure value exceeding the preset pressure threshold; and / or the temperature of the reaction solution in the barrel 41, and the preset conditions include the temperature value exceeding the preset temperature threshold. For example, in some embodiments, when the measuring component measures that the pressure value in the barrel 41 exceeds the preset pressure threshold, or measures that the temperature of the reaction solution in the barrel 41 exceeds the preset temperature threshold, the second magnetic component is controlled to separate from the first magnetic component to put the solid sample into the reaction solution. In addition, in some embodiments, when the measuring component measures that the pressure value in the barrel 41 exceeds the preset pressure threshold, and the temperature of the reaction solution in the barrel 41 exceeds the preset temperature threshold, the second magnetic component is controlled to separate from the first magnetic component to put the solid sample into the reaction solution.

[0045] Furthermore, in some embodiments, the measuring component may include a temperature sensor, which is electrically connected to the heating component and is used to measure the temperature of the reaction solution.

[0046] In some embodiments, the measuring assembly may include a pressure gauge 1 for measuring the pressure in the barrel 41. It should be noted that in some embodiments, the measuring assembly may also include other pressure measuring components for measuring the pressure in the barrel 41, such as a pressure gauge, a pressure sensor, etc., which are not limited here.

[0047] The discharge assembly includes a rod 6, a first magnetic element, and a second magnetic element. One end of the rod 6 is drivably connected to the top cover 42, and the other end is connected to the first magnetic element. The solid sample is suspended from the rod 6 by a thread. When the second magnetic element engages with the first magnetic element, the rod 6 remains horizontal, securing the solid sample above the reaction solution. When the second magnetic element separates from the first magnetic element, the first magnetic element tilts and rotates about the rod 6, releasing the suspended solid sample into the reaction solution.

[0048] In some embodiments, the first magnetic member is a rotatable magnetic sheet 7, and the second magnetic member is a detachable magnetic sheet or an electromagnet. The rotatable magnetic sheet 7 is a magnetic sheet that can rotate relative to the top cover 42 along with the rotation of the rod 6;

[0049] The detachable magnetic sheet is a magnetic sheet that can be installed on the outside of the top cover 42 by manual or mechanical structures, and can also be removed from the outside of the top cover 42 by manual or mechanical structures. Specifically, initially, the second magnetic member is installed on the outside of the top cover 42, and the first magnetic member is fixed to the top cover by magnetic attraction with the second magnetic member. At this time, the first magnetic member is horizontal and can fix the suspended sample, and the sample is in a state where it does not fall into the reaction solution. When the preset conditions are met, the second magnetic member is removed. At this time, the first magnetic member can no longer be fixed to the top cover due to separation from the second magnetic member. Under the action of gravity, the first magnetic member tilts and rotates with the rod 6 as the axis, and the sample falls into the reaction solution, completing the unloading action. Wherein, when the preset conditions are met, the operator can be prompted to manually remove the second magnetic member with the help of a sensor and an audible and visual alarm, or the second magnetic member can be automatically removed by the robot with the help of the cooperation of the sensor and the manipulator.

[0050] In some embodiments, the second magnetic member can also be an electromagnet. In this case, the second magnetic member can be attracted and separated from the first magnetic member by turning the electromagnet on and off. Specifically, when the second magnetic member is energized, the second magnetic member has magnetism and can be attracted to the first magnetic member. At this time, the first magnetic member can be fixed to the top cover by magnetic force. At this time, the first magnetic member is horizontal and can fix the suspended sample, and the sample is in a state where it does not fall into the reaction solution; when the power is turned off, the second magnetic member loses its magnetism, and the first magnetic member cannot be fixed to the top cover. Under the action of gravity, the first magnetic member tilts and rotates with the rod 6 as the axis, and the sample falls into the reaction solution, completing the unloading action; wherein, when the preset conditions are met, the electromagnet can be de-energized with the help of a sensor and a controller.

[0051] The experimental device for the dissolution and chemical reaction of materials in a liquid medium also includes a cooling assembly and a support leg 5. The support leg 5 is mounted below a barrel 41. One end of the cooling assembly 3 is connected to the bottom end of the barrel 41, and the other end serves as an outlet for the liquid medium. One end of the cooling assembly 3 is connected to the barrel 41 via a control valve, and the other end is provided with a control valve.

[0052] The heating component is a thermocouple 2, and / or the cooling component is a condenser 3. The reaction solution is TSP (i.e., Na3PO4) or NaOH, and / or the solid sample is alkali-free glass cloth, pure zinc, or low-alloy steel.

[0053] The present invention also provides an experimental method, the core of which is to determine the reaction characteristics of different substances in Na₃PO₄ and NaOH solutions by varying reaction conditions and reactants. The experimental method utilizes an experimental apparatus for the dissolution and chemical reaction of materials in liquid media, and includes experimental steps. The principles of the experimental steps are as follows: heating allows alkali-free glass cloth, pure zinc, and low-alloy steel to react with the solution; controlling the pH and temperature to influence the reaction outcomes; and sampling the solution to detect the solute composition and calculate the extent of the reaction.

[0054] The specific operation is to electrically heat the reactor 4 using a heater 2, and to maintain a stable temperature in the reactor 4 by means of a temperature sensor linked to the heater 2. After reaching the specified temperature, alkali-free glass cloth, pure zinc, low-alloy steel, and Na3PO4 or NaOH solution are mixed. During sampling, the reaction solution is cooled by a cooling assembly and sampled at the sampling port.

[0055] The specific steps include:

[0056] S1. Clean the reactor 4 and inject Na3PO4 or NaOH solution. More specifically, rinse the inside of the reactor 4 3-4 times with ultrapure water.

[0057] S1.1. Sample Preparation: Weigh the samples. The experimental solution volume is 1 L. The amount of alkali-free glass cloth can be 2g, 5g, 10g, 20g, or 30g. The number of low-alloy steel samples can be 2 pieces, and the number of pure zinc samples can be 4 pieces. Use alkali-resistant cotton thread to make hanging pieces of the samples and fix them to the top of the reactor through the discharge assembly.

[0058] S1.2. Inject 1L of Na3PO4 or NaOH solution into reactor 4; the Na3PO4 or NaOH solution can be a solution whose pH value has been adjusted by a pH buffer. The pH buffer is: when a certain amount of acid and base are added to certain solutions, it has the effect of hindering the change of the solution's pH value, which is called buffering effect. Such a solution is also called a buffer solution.

[0059] S2. Hang the solid sample to be tested on the rod through a silk thread;

[0060] S3, disposing a second magnetic element on the outside of the top cover 42 to engage with the first magnetic element on the inside of the top cover 42 to suspend the solid sample to be tested above the reaction solution;

[0061] S4. Control the operation of the heating component and the measuring component. When the measuring component measures that the parameters in the barrel 41 meet the preset conditions, the second magnetic component is removed from the top cover 42, or the second magnetic component is powered off to separate the first magnetic component from the second magnetic component, so that the solid sample to be tested is placed into the reaction solution for contact reaction.

[0062] Specifically, the heater and temperature sensor operate simultaneously to control the reaction temperature, and the sample is added. More specifically, the reactor 4 heats up. When the temperature of the reactor reaches 150°C and stabilizes for 5 minutes, the second magnetic plate is controlled to cause the discharge assembly to drop the sample and suspend it in the solution, and the time is recorded.

[0063] S5. After the specified reaction time has elapsed, samples are taken from the cooling assembly's sampling port and their chemical composition is tested to obtain an element release rate curve for the test material. This allows for evaluation of the interaction between the test material and the reaction medium, as well as between different test materials. More specifically, regular sampling can be performed: 10 mL of water samples are taken at 10, 20, 30, 60, and 90 minutes for elemental analysis by ICP-OES (inductively coupled plasma optical emission spectrometry). This allows analysis of the element release rate of the sample under simulated accident conditions.

[0064] This paper designs an experimental device for studying the dissolution and chemical reaction processes of materials in liquid media, taking into account environmental conditions such as pressure, temperature, and pH within the containment vessel or other space behind a LOCA. This device can simulate the media conditions within the containment vessel or other space behind a LOCA, and study the release behavior of Zn, Ca, Si, and P from representative materials (e.g., alkali-free glass cloth, pure zinc, and low-alloy steel). Combined with dissolution and chemical reaction test data, this device supports modeling of chemical effect analysis.

[0065] The overall experiment simulates actual working conditions, with multiple temperatures and various water chemistry conditions (different pH values), and analyzes the release rate of major elements and the composition of sediments from representative samples of flooded materials (e.g., alkali-free glass cloth, pure zinc, and low-alloy steel) within the containment or other spaces after a LOCA accident.

[0066] The present invention designs an experimental device and experimental steps to address the following defects: the current situation is that it is impossible to mix materials and liquid media under specified temperature and pressure conditions; the reaction characteristics of different substances in high-temperature liquid media are not studied in depth; the relationship between the reaction results and reaction conditions of substances such as alkali-free glass cloth, pure zinc, and low-alloy steel with Na3PO4 or NaOH solutions under high temperature conditions has not been established; and the type and composition of precipitates formed after the reaction of substances such as alkali-free glass cloth, pure zinc, and low-alloy steel under high temperature conditions are still unclear.

[0067] This study simulated a reactor loss-of-coolant accident (LOCA) condition, collected extensive data on the dissolution behavior of three representative materials: alkali-free glass cloth, zinc metal, and low-alloy steel, and analyzed their precipitation behavior after dissolution. Summarizing the various experiments, the following conclusions were drawn:

[0068] 1. E-glass cloth dissolves in Na3PO4 solution. The main dissolved elements include Si, Na, Ca, and Mg. Among them, Si and Na dissolve significantly, while Ca and Mg dissolve less. The dissolution rates of Si and Na increase with increasing temperature and pH, and the relationship formulas of the dissolution rates of Si and Na with temperature and pH are obtained respectively. The dissolution rates of Si and Na decrease with increasing addition amount, which is related to the morphology of E-glass cloth in water.

[0069] 2. Precipitates are generated in the dissolving solution of alkali-free glass cloth, mainly Ca3(PO4)2 and Mg(OH)2;

[0070] 3. Low alloy steel and zinc did not dissolve in Na3PO4 solution, and no precipitate was generated.

[0071] In the description of this application, it should be understood that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on this application.

[0072] The above describes specific embodiments of the present invention. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art may make various changes or modifications within the scope of the claims, which do not affect the essence of the present invention. The embodiments of this application and the features in the embodiments may be combined with each other in any manner unless there is a conflict.

Claims

1. An experimental device for the dissolution and chemical reaction process of a material in a liquid medium, characterized in that: It includes a measuring component, a heating component, a reactor (4) and a discharge component; The reactor (4) comprises a top cover (42) and a barrel (41), wherein the barrel (41) is used to contain a reaction solution and provide a chemical reaction space; The measuring component is used to measure parameters in the barrel (41); The heating component is arranged in the barrel (41) and is used to increase the temperature of the reaction solution in the barrel (41); The discharge assembly includes a rod (6), a first magnetic component and a second magnetic component, wherein the rod (6) is connected to the first magnetic component and is arranged on the inner side of the top cover (42), and the solid sample is suspended on the rod (6), and the second magnetic component is arranged on the outer side of the top cover (42). The second magnetic component is attracted to the first magnetic component to fix the solid sample above the reaction solution; when the parameters in the barrel (41) meet the preset conditions, the second magnetic component is controlled to separate from the first magnetic component to put the solid sample into the reaction solution.

2. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to claim 1, characterized in that: The parameter in the barrel (41) includes a pressure value in the barrel (41), and the preset condition includes the pressure value exceeding a preset pressure threshold; and / or The temperature of the reaction solution in the barrel (41), the preset condition includes that the temperature value exceeds a preset temperature threshold.

3. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to claim 1, characterized in that: One end of the rod (6) is tactilely connected to the top cover (42), and the other end is connected to the first magnetic attraction member, and the solid sample is suspended on the rod (6) via a wire; When the second magnetic element is attracted to the first magnetic element, the rod (6) remains horizontal to fix the solid sample and suspend it above the reaction solution; when the second magnetic element is separated from the first magnetic element, the rod (6) tilts to put the solid sample suspended on the rod into the reaction solution.

4. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to claim 1, characterized in that: The measuring component includes a temperature sensor, the temperature sensor being electrically connected to the heating component and being used to measure the temperature of the reaction solution; and / or A pressure gauge (1) is used to measure the pressure inside the cylinder (41).

5. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to any one of claims 1 to 4, characterized in that: It also includes a cooling component and a support leg (5), wherein the support leg (5) is installed at the lower part of the barrel (41), one end of the cooling component (3) is connected to the bottom end of the barrel (41), and the other end serves as a liquid medium outlet.

6. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to claim 5, characterized in that: One end of the cooling assembly (3) is connected to the barrel (41) via a control valve, and the other end is provided with a control valve.

7. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to any one of claims 1 to 4, characterized in that: The first magnetic attraction member is a rotatable magnetic attraction sheet (7); The second magnetic attraction component is a detachable magnetic attraction sheet or an electromagnet.

8. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to any one of claims 1 to 4, characterized in that: The heating component is a thermocouple (2); and / or, The cooling component is a condenser (3).

9. The experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to any one of claims 1 to 4, characterized in that: The reaction solution is TSP or NaOH; and / or, Solid samples are alkali-free glass cloth, pure zinc or low alloy steel.

10. An experimental method based on the experimental device for the dissolution and chemical reaction process of a material in a liquid medium according to any one of claims 1 to 9, characterized in that: The experimental method comprises the following steps: S1, cleaning the reactor (4) and injecting the reaction medium; S2. Hanging the solid sample to be tested on the rod through a silk thread; S3, arranging the second magnetic element on the outside of the top cover (42) to engage with the first magnetic element on the inside of the top cover (42) to suspend the solid sample to be tested above the reaction solution; S4, controlling the operation of the heating component and the measuring component, and when the measuring component measures that the parameters in the barrel (41) meet the preset conditions, removing the second magnetic component from the top cover (42), or disconnecting the power supply of the second magnetic component, so as to separate the first magnetic component from the second magnetic component, thereby putting the solid sample to be tested into the reaction solution for contact reaction therewith; S5. After the specified reaction time is reached, samples are taken from the sampling port of the cooling component, and the chemical composition thereof is detected to obtain the element release rate curve of the test material, and to evaluate the interaction effects between the test material and the reaction medium, as well as between different test materials.

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