A dissolution kinetic reaction device resistant to acid corrosion and its experimental method

Abstract

The present invention discloses an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof, which relates to the field of analytical detection technology, and includes: a reaction container and a container cover; the container cover is used to seal the opening of the reaction container, and the container cover is provided with a temperature measuring port, a gas phase channel port and a adding / sampling port; the temperature measuring port is connected to a temperature measuring device; the gas phase channel port is connected to a condensation reflux device. By adopting this scheme, during the sample dissolution reaction process, by sampling and analyzing the solution in the reaction container at different time points, the dissolution law and dissolution kinetic behavior of the doped uranium dioxide microspheres that are not easily soluble can be studied.

Description

Technical Field

[0001] The invention relates to the technical field of analysis and detection, and in particular to an acid corrosion-resistant dissolution kinetics reaction device and an experimental method thereof. Background Art

[0002] Nuclear fuel doped with metal oxides has important applications in the field of nuclear energy. Other matrices are added to uranium dioxide microspheres during the production process, and ceramic-like doped fuel microspheres are formed after high-temperature sintering. Compared with pure uranium dioxide microspheres, doped uranium dioxide microspheres face the problem of difficult dissolution in sample pretreatment. According to industry requirements, when conducting chemical composition testing on doped uranium dioxide microspheres, 36 elements such as U need to be quantitatively analyzed. Understanding the dissolution law and dissolution kinetics of doped uranium dioxide microspheres in the HNO3-HF system is a prerequisite for establishing a pretreatment method for doped fuel microspheres, and is the basis for ensuring the complete extraction and accurate quantitative analysis of the elements to be measured.

[0003] At present, there are no public reports abroad on the research of pretreatment technology and chemical composition detection technology of doped uranium dioxide microspheres, there is very little reference material, and the research is difficult. Summary of the invention

[0004] The purpose of the present invention is to provide an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof. By adopting this scheme, during the sample dissolution reaction process, by sampling and analyzing the solution in the reaction container at different time points, the dissolution law and dissolution kinetic behavior of the poorly soluble doped uranium dioxide microspheres can be studied.

[0005] The present invention is achieved through the following technical solutions:

[0006] A dissolution kinetic reaction device resistant to acid corrosion comprises: a reaction container and a container cover; the container cover is used to seal the opening of the reaction container, and the container cover is provided with a temperature measuring port, a gas phase channel port and a adding / sampling port; the temperature measuring port is connected to a temperature measuring device; the gas phase channel port is connected to a condensation reflux device.

[0007] Compared with the prior art, there is no research on the pretreatment technology and chemical composition detection technology of doped uranium dioxide microspheres, there is very little reference material, and the research is difficult. The present scheme provides an acid-corrosion-resistant dissolution kinetic reaction device. In the specific scheme, it includes a reaction container and a container cover. The reaction container is used to hold the reaction solution and conduct a solid dissolution test. The container cover is located in the middle part of the device and is used to seal the reaction container. Three ports are respectively opened on the container cover, namely a temperature measurement port, a gas phase channel port and a sampling port, wherein the sampling port is used to add a sample to the reaction container or take out the solution after the reaction; the temperature measurement port is provided with a temperature measurement device, which is used to measure the internal temperature of the reaction container. The sample can be added to react only when the acid solution is heated to a given temperature; wherein the gas phase channel port is used to discharge the steam inside the reaction container, and a condensation reflux device is connected to the gas phase channel port, so that after the steam enters the condensation reflux device, it can be condensed and refluxed into the reaction container, thereby reducing the influence of heating on the volume of the acid solution in the reaction container.

[0008] Further optimization is that a plug with a threaded sealing connection is provided at the addition / sampling port; wherein the plug and the addition / sampling port are threadedly sealed and connected to seal the addition / sampling port while achieving a detachable connection to facilitate taking out a certain volume of solution at any time.

[0009] Further optimization is that the condensation reflux device adopts a condenser tube, and cooling water flows through the condenser tube to facilitate condensation reflux.

[0010] Further optimization is that a first connector with a threaded sealing connection is provided at the gas phase channel opening, a first through hole is opened on the first connector, the condenser is inserted into the first through hole through a bottom hose and is connected to the interior of the reaction container; for realizing a detachable connection.

[0011] Further optimized, the temperature measuring device includes a temperature sensor and a temperature sensor sleeve, the temperature sensor is placed in the temperature sensor sleeve, and the temperature sensor sleeve extends from the temperature measurement port to below the liquid level of the reaction acid solution in the reaction container; it is used to accurately measure the temperature of the solution inside the reaction container and protect the temperature sensor from acid corrosion.

[0012] Further optimization, the temperature measuring port is provided with a second connector with a threaded sealing connection, the second connector is provided with a second through hole, and the temperature sensor sleeve extends into the reaction container from the second through hole; for realizing a detachable connection.

[0013] Further optimization is that the temperature sensor sleeve is injected with heat transfer oil; the solution temperature is transferred to the heat transfer oil, and the temperature sensor displays the temperature of the reaction acid solution, thereby improving the detection accuracy.

[0014] Further optimized, the container cover and the reaction container are threadedly sealed and connected to achieve a detachable connection.

[0015] Further optimization, the reaction container adopts a cylindrical translucent container; it is used to hold the acid solution, conduct the dissolution kinetics test, and observe the reaction phenomenon; wherein the reaction container, the container cover, the condensation reflux device, the temperature sensor sleeve, the first connector, the second connector and the plug are all made of corrosion-resistant materials, such as fusible polytetrafluoroethylene (PFA), polytetrafluoroethylene (PTFE) and other materials, to ensure the corrosion resistance of the dissolution kinetics reaction device in the acid solution.

[0016] Further optimized, an experimental method for an acid corrosion resistant dissolution kinetic reaction device, the method comprising the following steps:

[0017] Step 1: prepare an acid solution, transfer the acid solution into a reaction vessel, and assemble a dissolution kinetic reaction device;

[0018] Step 2: placing the dissolution kinetics reaction device in a constant temperature oil bath, heating the acid solution to a specified temperature, measuring the temperature of the acid solution by the temperature measuring device, then adding the sample into the reaction container, and starting timing;

[0019] Step 3: At certain time intervals, a certain volume of solution is drawn through the adding / sampling port, and an equal volume of acid solution is added at the same time;

[0020] Step 4: Dilute the solution absorbed each time to a certain volume, and use relevant instruments to quantitatively analyze the ions in the solution to obtain the dissolution information of the solid sample.

[0021] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0022] 1. The present invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof. By adopting this scheme, during the sample dissolution reaction process, by sampling and analyzing the solution in the reaction container at different time points, the dissolution law and dissolution kinetic behavior of the poorly soluble doped uranium dioxide microspheres can be studied.

[0023] 2. The present invention provides an acid-corrosion-resistant dissolution kinetics reaction device and an experimental method thereof, which adopts corrosion-resistant materials (PFA, PTFE) as the main material of the corrosion device to ensure the corrosion resistance of the dissolution kinetics reaction device in various acid solutions, and can meet the requirements of carrying out dissolution kinetics experiments in a corrosive environment.

[0024] 3. The present invention provides an acid corrosion-resistant dissolution kinetic reaction device and an experimental method thereof, which adopts a condenser structure to quickly condense the water vapor generated in the container to ensure a constant volume of the acid liquid in the reaction container.

[0025] 4. The present invention provides an acid corrosion resistant dissolution kinetics reaction device and an experimental method thereof, which adopts a temperature sensor sleeve setting to ensure that the measured temperature reflects the temperature of the acid solution in the reaction container.

[0026] 5. The present invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof, and is provided with a adding / sampling port, which is convenient for adding samples after the acid solution is heated to a specified temperature, and is also convenient for sampling the acid solution and replenishing the acid solution. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and should not be regarded as limiting the scope. For those of ordinary skill in the art, other relevant drawings can be obtained based on these drawings without creative work. In the drawings:

[0028] Figure 1 A schematic diagram of the structure of an embodiment provided by the present invention;

[0029] Figure 2 A top view of a container closure according to an embodiment of the present invention.

[0030] Marks and corresponding parts names in the attached drawings:

[0031] 1-container cover, 2-second connector, 3-first connector, 4-plug, 5-reaction container, 6-condensation reflux device, 7-cooling water inlet, 8-cooling water outlet, 9-temperature sensor sleeve. DETAILED DESCRIPTION

[0032] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with embodiments and drawings. The exemplary embodiments of the present invention and their description are only used to explain the present invention and are not intended to limit the present invention.

[0033] Embodiment 1

[0034] like Figure 1 and Figure 2 As shown, this embodiment 1 provides an acid-corrosion-resistant dissolution kinetic reaction device, comprising: a reaction container 5 and a container cover 1; the container cover 1 is used to seal the opening of the reaction container 5, and the container cover 1 is provided with a temperature measuring port, a gas phase channel port and a adding / sampling port; the temperature measuring port is connected to a temperature measuring device; the gas phase channel port is connected to a condensation reflux device.

[0035] Compared with the prior art, there is no research on the pretreatment technology and chemical composition detection technology of doped uranium dioxide microspheres, there are very few reference materials, and the research is difficult. This scheme provides an acid-corrosion-resistant dissolution kinetic reaction device. In the specific scheme, it includes a reaction container 5 and a container cover 1. The reaction container 5 is used to hold the reaction solution and perform a solid dissolution test. The container cover 1 is located in the middle part of the device and is used to seal the reaction container 5. Three ports are respectively opened on the container cover 1, namely, a temperature measurement port, a gas phase channel port and a sampling port, wherein The adding / sampling port is used to add samples to the reaction container 5 or take out the solution after the reaction; the temperature measuring port is provided with a temperature measuring device, which is used to measure the internal temperature of the reaction container 5. The sample can only be added to make it react when the acid solution is heated to a given temperature; the gas phase channel port is used to discharge the steam inside the reaction container 5. A condensation reflux device is connected to the gas phase channel port, and the condensation reflux device is located above the container cover 1, so that after the steam enters the condensation reflux device, it can condense and reflux into the reaction container 5, thereby reducing the impact of heating on the volume of the acid solution in the reaction container 5.

[0036] The above scheme aims to achieve: allowing the acid solution and the sample to react continuously in the reaction container 5. During the reaction, the solution in the reaction container 5 can be taken out at different time points through the sampling port, and sampling and analysis can be carried out, so as to realize the study of the dissolution law and dissolution kinetic behavior of the insoluble doped uranium dioxide microspheres; wherein the condensation reflux device can condense and reflux the steam to the reaction container 5, so as to reduce the effect of heating on the volume of the acid solution in the reaction container 5, and ensure that the volume of the acid solution in the reaction container 5 is constant.

[0037] For further solutions, see Figure 2 The adding / sampling port is provided with a plug 4 with a threaded sealing connection; wherein the plug 4 is threadedly sealed to the adding / sampling port, which is used to seal the adding / sampling port while realizing a detachable connection, so as to facilitate taking out a certain volume of solution at any time.

[0038] See also Figure 1 As a specific implementation method for condensation reflux, it is configured as follows: the condensation reflux device adopts a condenser tube, and cooling water flows through the condenser tube.

[0039] In the above scheme, the condensation reflux device adopts a condenser, and the condenser is preferably a straight condenser, a cooling water inlet 7 is provided below the side of the condenser, and a cooling water outlet 8 is provided above the side of the condenser, so that cooling water can be introduced to achieve cooling.

[0040] See also Figure 2As an implementation method for realizing detachable connection, it is configured as follows: a first connector 3 with threaded sealing connection is provided at the gas phase channel opening, a first through hole is opened on the first connector 3, the condenser is inserted into the first through hole through a bottom hose, and is connected to the interior of the reaction container 5;

[0041] In the above scheme, the first connector 3 is threadedly sealed to the gas phase channel opening, wherein the first through hole and the hose at the bottom of the condenser are matched in size, and the hose is inserted into the first through hole and fixed, so that the condenser and the reaction container 5 can be connected to each other.

[0042] See also Figure 1 As a specific embodiment for accurately measuring the temperature of the solution inside the reaction container 5, it is set as follows: the temperature measuring device includes a temperature sensor and a temperature sensor sleeve 9, the temperature sensor is placed in the temperature sensor sleeve 9, and the temperature sensor sleeve 9 extends from the temperature measuring port to below the liquid level of the reaction acid solution in the reaction container 5; in this scheme, the temperature measuring device includes a temperature sensor, the temperature sensor is placed in the temperature sensor sleeve 9, and the temperature sensor and the acid solution are isolated by the temperature sensor sleeve 9, so as to prevent the temperature sensor from chemically reacting with the acid, thereby protecting the temperature sensor from acid corrosion and preventing the components of the acid solution from being contaminated; wherein the temperature sensor sleeve 9 extends from the temperature measuring port into the reaction container 5 and can be inserted below the liquid level of the reaction acid solution, so as to measure the temperature of the reaction acid solution.

[0043] See also Figure 2 As an implementation method for realizing detachable connection, the temperature measuring port is provided with a second connector 2 with threaded sealing connection, the second connector 2 is provided with a second through hole, and the temperature sensor sleeve 9 extends into the reaction container 5 from the second through hole; in this scheme, the second connector 2 and the temperature measuring port are sealed and threadedly connected, wherein the sizes of the second through hole and the temperature sensor sleeve 9 are matched, and the temperature sensor sleeve 9 is inserted into the reaction container 5 from the second through hole and placed below the liquid level of the reaction acid solution, so that the temperature of the reaction acid solution can be accurately measured.

[0044] As a redundant solution, the temperature sensor sleeve 9 is injected with heat transfer oil; the solution temperature is transferred to the heat transfer oil, and the temperature sensor displays the temperature of the reaction acid solution, thereby improving the detection accuracy.

[0045] As an implementation method for achieving a detachable connection, the container cover 1 and the reaction container 5 are threadedly sealed and connected to achieve a detachable connection.

[0046] A further solution is: the reaction container 5 adopts a cylindrical translucent container; it is used to hold the acid solution, conduct the dissolution kinetics test, and observe the reaction phenomenon; wherein the reaction container 5, the container cover 1, the condensation reflux device, the temperature sensor sleeve 9, the first connector 3, the second connector 2 and the plug 4 are all made of corrosion-resistant materials, such as fusible polytetrafluoroethylene (PFA), polytetrafluoroethylene (PTFE) and other materials, to ensure the corrosion resistance of the dissolution kinetics reaction device in the acid solution.

[0047] Embodiment 2

[0048] This embodiment 2 is further limited on the basis of embodiment 1, and provides an experimental method for a dissolution kinetic reaction device resistant to acid corrosion, the method comprising the following specific steps:

[0049] Step 1: Before the test, prepare an acid solution according to the test requirements, and place the acid solution in a clean reaction container 5; and weigh the solid sample prepared according to the test requirements before the experiment.

[0050] Step 2: Transfer a certain volume of acid solution to the reaction container 5, then connect the reaction container 5 to the container cover 1, and connect the container cover 1 to the condenser. Connect the sleeve with the temperature sensor and the addition / sampling port to the container cover 1, and pass cooling water through the condenser.

[0051] (3) Place the dissolution kinetics reaction device in a constant temperature oil bath to raise the temperature of the acid solution to a specified temperature; add the sample into the reaction vessel 5 through the sampling port, and start recording the time.

[0052] (4) At every certain time interval, a certain volume of solution is drawn through the adding / sampling port, and an equal volume of acid solution is added at the same time to ensure that the volume of the acid solution is basically constant.

[0053] (5) Dilute the absorbed solution to a certain volume, and use relevant instruments to quantitatively analyze the ions in the solution to obtain the dissolution information of the solid sample.

[0054] (6) After the sample collection is completed, the switch of the constant temperature oil bath is turned off, and after the oil bath is cooled to room temperature, the dissolution kinetic reaction device is taken out, the acid solution in the reaction container 5 is recovered, and the device is cleaned.

[0055] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A dissolution kinetic reaction device resistant to acid corrosion, characterized in that: include: A reaction container (5) and a container cover (1); the container cover (1) is used to seal the opening of the reaction container (5), and the container cover (1) is provided with a temperature measuring port, a gas phase channel port, and a adding / sampling port; the temperature measuring port is connected to a temperature measuring device, and the gas phase channel port is connected to a condensing reflux device (6); The temperature measuring device comprises a temperature sensor and a temperature sensor sleeve (9), wherein the temperature sensor is placed in the temperature sensor sleeve (9), and the temperature sensor sleeve (9) extends from the temperature measuring port to below the liquid level of the reaction acid solution in the reaction container (5); The reaction container (5) is made of soluble polytetrafluoroethylene material, the container cover is made of polytetrafluoroethylene material, and the temperature sensor sleeve (9) is made of corrosion-resistant material; The dissolution kinetics reaction device is used to sample the dissolution reaction process of the doped uranium dioxide microsphere solid sample to obtain the dissolution law of the doped uranium dioxide microsphere.

2. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The adding / sampling port is provided with a plug (4) which is threaded and sealed.

3. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The condensation reflux device (6) adopts a condenser tube, and cooling water flows through the condenser tube.

4. The acid corrosion resistant dissolution kinetic reaction device according to claim 3, characterized in that: A first connector (3) with a threaded sealing connection is provided at the gas phase channel opening. A first through hole is provided on the first connector (3). The condenser is inserted into the first through hole through a bottom hose and is connected to the interior of the reaction container (5).

5. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The temperature measuring port is provided with a second connector (2) with a threaded sealing connection, the second connector (2) is provided with a second through hole, and the temperature sensor sleeve (9) extends into the reaction container (5) from the second through hole.

6. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The temperature sensor sleeve is injected with heat-conducting oil.

7. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The container cover (1) and the reaction container (5) are threadedly sealed.

8. The acid corrosion resistant dissolution kinetic reaction device according to claim 1, characterized in that: The reaction container (5) is a cylindrical translucent container.

9. The experimental method of an acid corrosion resistant dissolution kinetic reaction device according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: Step 1: prepare acid solution; Step 2: Transfer the acid solution to a reaction vessel (5) and assemble a dissolution kinetic reaction device; Step 3: placing the dissolution kinetics reaction device in a constant temperature oil bath, heating the acid solution to a specified temperature, measuring the temperature of the acid solution by the temperature measuring device, then adding the sample to the reaction container (5), and starting the timing; Step 4: At certain time intervals, a certain volume of solution is drawn through the adding / sampling port, and an equal volume of acid solution is added at the same time; Step 5: Dilute the solution absorbed each time to a certain volume, and use relevant instruments to quantitatively analyze the ions in the solution to obtain the dissolution information of the solid sample.

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