Device for measuring purification effect of high-temperature radioactive gas

Abstract

The utility model discloses a device for measuring the purification effect of a material on volatile radionuclides such as I, Cs and Te generated in a nuclear fission process. The device provided by the utility model comprises an experimental gas generating device, an adsorption device, a pressure control device and a tail gas purifying device which are communicated with one another, pipelines, communicating pipelines and communicating devices which are communicated with the devices, valves arranged on the related pipelines, and heating and heat preservation devices. The experimental gas generation device and the adsorption device are both arranged in the heating and heat preservation device, and the device for measuring the purification effect of the material on the high-temperature radioactive gas is completely isolated from the outside in an airtight manner. According to the utility model, the adsorption performance of various volatile radionuclides generated in the nuclear fission process under different materials under severe working conditions can be determined and relatively high, and a favorable tool is provided for solving the problem of volatile radionuclides generated in the nuclear fission process.

Description

Technical Field

[0001] The utility model relates to a testing device, more specifically a device for determining the purification effect of a certain material on high-temperature radioactive gas, especially volatile radionuclides such as I, Cs, Te, etc. produced in the nuclear fission process. Background Art

[0002] There are many materials and devices for adsorbing radionuclides in the patents disclosed so far, such as the composite microsphere adsorption material and its preparation method and application disclosed in CN113877549A, but it is not clear whether similar materials and methods can treat high-temperature radioactive gases and their effects. To adsorb and purify high-temperature radioactive gases, it is first necessary to determine the adsorption effect of specific materials on different high-temperature radioactive gases. However, there is no device in the prior art that can be used to determine the purification effect of materials on high-temperature radioactive gases. Summary of the invention

[0003] The utility model provides a device which can be used to measure the purification effect of materials on high-temperature radioactive gas.

[0004] The utility model discloses a device for determining the purification effect of a material on high-temperature radioactive gas, comprising: an experimental gas generating device, an adsorption device, a pressure control device and an exhaust gas purification device which are interconnected, a pipeline connecting the aforementioned devices and valves arranged on the relevant pipelines, and a heating and heat preservation device, wherein the experimental gas generating device and the adsorption device are both arranged inside the heating and heat preservation device.

[0005] Preferably, the pressure control device in the device for measuring the purification effect of a material on high-temperature radioactive gas of the utility model is composed of a vacuum pump and a pressure controller.

[0006] Preferably, the experimental gas generating device in the device for determining the purification effect of materials on high-temperature radioactive gases of the utility model is composed of an experimental carrier gas source, an experimental carrier gas heating device, a mass flow controller and a volatilization device for the experimental substance under test.

[0007] Preferably, the tail gas purification device in the device for measuring the purification effect of a material on high-temperature radioactive gas of the utility model is a cold trap.

[0008] Preferably, in the device for determining the purification effect of a material on high-temperature radioactive gas of the utility model, the carrier gas source adopts an inert gas, and the experimental carrier gas heating device is composed of a muffle furnace and a metal coil placed therein.

[0009] Preferably, the experimental substance volatilization device in the device for determining the purification effect of materials on high-temperature radioactive gases of the utility model is composed of an outer shell with a cavity inside and a connecting tube, a sample dish placed in the cavity of the outer shell, a quartz boat placed in the sample dish with the test volatile material, and an upper cover with a ventilation pipeline and can be sealed and fixed to the outer shell, and a ventilation hole is opened in the part of the sample dish located outside the quartz boat.

[0010] Preferably, the adsorption device of the device for determining the purification effect of a material on high-temperature radioactive gas of the utility model is composed of a static adsorption device and a dynamic adsorption device, wherein:

[0011] The static adsorption device is composed of a shell with a cavity inside, a static adsorption dish placed in the shell cavity, and an upper cover with a connecting flange that can be sealed and fixed to the shell by bolts. The static adsorption dish is provided with at least one adsorption hole in which the adsorption material can be filled, and a small hole for ventilation is opened at the bottom of the adsorption hole;

[0012] The dynamic adsorption device consists of a tubular shell, a plurality of dynamic adsorption dishes stacked in the tubular shell, and a cover with a flange thereon. A ventilation hole is opened at the bottom of each dynamic adsorption dish, and the adsorption material to be tested is placed in the dynamic adsorption dish.

[0013] Preferably, the heating and heat preservation device of the device for determining the purification effect of materials on high-temperature radioactive gases of the utility model is composed of two heating and heat preservation devices made of heat preservation material, which are hinged to each other and can be locked and opened, and an area for placing the test substance volatilization device, static adsorption device or / and dynamic adsorption device is provided therein, and the heating and heat preservation device is located in the area of ​​the test substance volatilization device, static adsorption device or / and dynamic adsorption device, and a heating device and a temperature measuring device such as a thermocouple are provided.

[0014] Preferably, in the heating and heat preservation device of the device for determining the purification effect of materials on high-temperature radioactive gases of the utility model, the heating devices of the three areas where the experimental substance volatilization device, the static adsorption device and / or the dynamic adsorption device are placed are respectively provided with independent temperature control units, which can realize the determination of the purification capacity of the adsorption material under different experimental conditions and obtain the corresponding process parameters.

[0015] More preferably, in the device for determining the purification effect of materials on high-temperature radioactive gases, the connecting device between the experimental substance volatilization device, the static adsorption device and / or the dynamic adsorption device is a flange with a knife edge and a soft metal gasket, which is sealed by the knife edge of the soft gasket.

[0016] The device of the utility model uses heated carrier gas to carry the heated and volatilized experimental substances, such as I, Cs, Te and other gases, into adsorption devices in different states and fully interact with the adsorption materials in the adsorption devices, wherein the pressure control device ensures the stable volatilization of the experimental substances to complete the adsorption experiment. During the experiment, the gaseous experimental substances that are not completely purified are introduced into the cold trap for condensation in real time, and are discharged after harmless treatment by the adsorbent set at the outlet of the vacuum pump. During the experiment, the gaseous experimental substances are in a negative pressure system and are completely isolated from the outside world, and will not escape and have a negative impact on the outside world.

[0017] In the device of the utility model, the experimental substance volatilization device, the static adsorption device and / or the dynamic adsorption device are sealed by the knife edge of the soft gasket. This structure can completely ensure the airtightness of the device and ensure that the experimental gas is isolated from the atmosphere.

[0018] The tail gas purification device in the device of the utility model comprises a stainless steel cold trap and a heat preservation container to which liquid nitrogen can be added and the stainless steel cold trap is placed. This design can condense the tested radioactive gas that is not adsorbed by the material in real time, thereby fundamentally preventing the leakage of the experimental gas from affecting the outside world.

[0019] The utility model provides a favorable tool for solving the problem of volatile radionuclides produced in the nuclear fission process, and provides a method for determining and comparing the adsorption performance of various volatile radionuclides produced in the nuclear fission process under different materials under severe working conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a schematic diagram of the overall structure of the best embodiment of the utility model;

[0021] Figure 2 It is a schematic diagram of a device for volatilizing experimental substances built in the device of the utility model. Figure 4 It is a half-section view;

[0022] Figure 3 yes Figure 2 Schematic diagram of the middle AA direction;

[0023] Figure 4 It is a semi-sectional schematic diagram of a static adsorption device in the device of the utility model;

[0024] Figure 5 for Figure 4 Schematic diagram of the middle BB section;

[0025] Figure 6 2 is a semi-sectional schematic diagram of a dynamic adsorption device in the device of the utility model;

[0026] Figure 7This is a schematic diagram of the utility model device in the open state of the heating device, the right side of the figure is partially half-sectioned;

[0027] Figure 8 It is the airtightness performance diagram of the device of the utility model;

[0028] Fig. 9 This is the adsorption capacity curve of the functionalized inorganic particle material to gaseous Te in a static state during the test of the embodiment of the utility model;

[0029] Fig.10 This is the adsorption capacity curve of functionalized inorganic particle material for gaseous Te under dynamic conditions.

[0030] In the figure: 1-experimental gas generating device, 2-adsorption device, 3-exhaust gas purification device, 4-carrier gas source, 5-carrier gas heating device, 6-tested experimental substance volatilization device, 7-static adsorption device, 8-dynamic adsorption device, 9-pressure control device, 10-container with activated carbon, 11-vacuum pump, 12-capping of dynamic adsorption device, 13-tested adsorption material, 14-dynamic adsorption dish, 15-dynamic adsorption device housing, 16-dynamic adsorption device fixing screw, 17-static adsorption device flange, 18-cavity for placing the test adsorption material, 19-static adsorption device housing, 20-bolts and nuts, 21-device for heating the dynamic adsorption device, 22-dynamic adsorption device, 23-device for heating the static adsorption device, 24-static adsorption device 25-a device for heating the experimental substance volatilization device, 26-a device for volatilizing the experimental substance, 27-a heating and heat preservation device on the right side of the device of the utility model, 28-a hinge, 29-a heating and heat preservation device on the left side of the device of the utility model, 30-a pipeline connected to the exhaust gas treatment device, 31-a device for heating the dynamic adsorption device on the left side, 33-a cavity for placing the dynamic adsorption device on the left side, 32-a device for heating the dynamic adsorption device on the left side, 34-a cavity for placing the static adsorption device on the left side, 35-a device for heating the experimental substance volatilization device on the left side, 36-a cavity for placing the experimental substance volatilization device on the left side, 37-a housing of the experimental substance volatilization device, 38-experimental substance, 39-a quartz boat, 40-a carrier gas flow hole, 41-a carrier gas output pipe, 42-a carrier gas input pipe, 43-static adsorption dish, 44-adsorption hole (44a-44h are adsorption holes respectively filled with different adsorption materials), 45-bottom of adsorption hole with small holes, 46-handle of adsorption dish, 47-handle hole of adsorption dish, 48-flow controller, 49-pressure controller, 50-pressure guide tube, 51-sample dish, 52-housing. DETAILED DESCRIPTION

[0031] The present invention is described in detail with reference to the preferred embodiments given in the accompanying drawings.

[0032] See also Figure 1 The utility model is composed of an experimental gas generating device 1, an adsorption device 2, an exhaust gas purification device 3 and a pressure control device 9 which are sequentially connected to each other. The devices are connected by a gas pipeline, and valves are provided at appropriate positions of the gas pipeline.

[0033] The experimental gas generating device 1 in the device for determining the purification effect of materials on high-temperature radioactive gases of the utility model is composed of a carrier gas source 4, a carrier gas heating device 5, a test material volatilization device 6 and a mass flow controller 48. The flow controller 48 is placed between the outlet of the carrier gas source 4 and the carrier gas heating device 5, and the content of the radioactive gas input into the dynamic adsorption device is regulated by the mass flow controller 48. In the embodiment of the utility model, the carrier gas source 4 is an inert gas in a gas bottle, and the experimental material volatilization device 6 is composed of an outer shell 52 with a cavity therein and a connecting pipe 42, a sample dish 51 placed in the cavity of the outer shell, a quartz boat 39 placed in the sample dish 51 and containing the test volatilization material, and an upper cover 41 with a ventilation pipeline and can be sealed and fixed to the outer shell 52, see Figure 2 The portion of the sample dish 51 outside the quartz boat 39 is provided with a vent hole 40, see Figure 3 When the utility model is working, the test substance in the quartz boat 39 is heated and volatilized by the heating device, and the heated inert gas carrier passes through the hole 40 to introduce the volatilized test substance gas into the adsorption device 2 through the pipeline to realize the adsorption experiment.

[0034] The adsorption device 2 of the utility model is composed of a static adsorption device 7 and a dynamic adsorption device 8. The static adsorption device 7 and the dynamic adsorption device are connected through a pipeline.

[0035] The static adsorption device 7 is composed of a shell 19 with a cavity 18, an adsorption dish 43 placed therein, and an upper cover 17 with a connecting flange that can be sealed and fixed to the shell 19 by bolts. The adsorption dish 43 is provided with a plurality of adsorption holes 44 into which adsorption materials can be filled, see Figure 4 Each adsorption hole bottom 45 is provided with a small hole for ventilation. In this embodiment, eight adsorption holes are provided. Figure 5 The adsorption dish 43 is also provided with an adsorption dish handle 46, and a handle hole 47 is provided at the end of the handle 46 to facilitate the placement or removal of the adsorption dish 43 during the experiment. The carrier gas and volatile experimental substances introduced during the experiment are brought into different adsorption materials through the small holes on the bottom 45 of the adsorption holes. Since different adsorption materials can be filled in each adsorption hole, static adsorption experiments can be carried out on different materials at the same time.

[0036] The dynamic adsorption device 8 is composed of a tubular housing 15, a plurality of adsorption dishes 14 stacked in the housing, and a cover 12 with a flange on the housing. The adsorption material to be tested is placed in the adsorption dish 14. Figure 6 The bottom of each adsorption dish 14 is provided with a ventilation hole, and its structure is similar to the bottom 45 of the adsorption hole of the static adsorption device.

[0037] The experimental gas comes into contact with the tested adsorption material through the ventilation holes to carry out dynamic adsorption experiment.

[0038] The experimental substance volatilization device 6 and the adsorption device 2 of the present utility model embodiment are both placed in a lockable and openable two-door heating and heat preservation device, see Figure 7 The left and right heating and heat preservation devices are connected by a hinge 28 and can be opened or locked. The two heating and heat preservation devices are respectively provided with cavities for placing the experimental material volatilization device 6, the dynamic adsorption device and the adsorption device. The experimental device can be easily placed before and after the experiment, or the adsorption material to be tested can be taken out for related tests. This structure can ensure the smooth progress of the experiment process. The areas where the experimental material volatilization device, the static adsorption device or / and the dynamic adsorption device are placed are respectively provided with heating devices and temperature measuring devices such as thermocouples to achieve heating and temperature control of different areas during the experiment.

[0039] In the utility model, the experimental gas outlet is connected to the exhaust gas purification device 3 and the pressure control device composed of the pressure controller 49 and the vacuum pump 11 through a pipeline with a control valve thereon, and a pressure-leading pipe 50 is connected between the experimental gas outlet and the pressure controller 49. Figure 1 In the specific embodiment of the present invention, the gas outlet of the dynamic adsorption device is connected to the exhaust gas purification device 3. The container 10 containing activated carbon is connected to the gas outlet of the vacuum pump 11. The utility model is provided with a pressure controller to adjust the volatilization amount of the radioactive gas in the experimental gas generating device to ensure normal measurement operation; the pressure lead pipe 50 is provided mainly for real-time detection and control of the absolute pressure in the adsorption device. The exhaust gas purification device in the device of the utility model is a cold trap, which is composed of an insulated container to which liquid nitrogen can be added and the cold trap is placed. When the device of the utility model is conducting experimental operations, the gas containing the test substance discharged through the experimental gas outlet is cooled into a solid by the cold trap, so that no exhaust gas pollution is generated, and the container 10 containing activated carbon can adsorb the gas formed in the vacuum pump 11 system, and there is no problem of leakage of pollutants.

[0040] The device of this embodiment is made of stainless steel material, especially a stainless steel cold trap.

[0041] In this embodiment, the experimental substance volatilization device 6 and the adsorption device 2 are connected to each other by flanges. A knife edge is provided on the flanges. When connected to each other, a soft gasket of a certain thickness is filled between the flanges. A soft metal gasket can also be used. The sealing is achieved by squeezing the knife edge. According to actual measurements, the whole device has good airtightness and can maintain 0 hPa within 300 min. See Figure 8 , so that the experimental gas can be completely isolated from the outside world.

[0042] The following is the process of conducting material experiments using the device of the utility model:

[0043] 1. Static adsorption experiment

[0044] For the static adsorption process: put the experimental substance into the quartz boat 39. The test substance used in this example is 0.1g amorphous single substance Te. Then put the quartz boat 39 into the experimental substance volatilization device. Put the tested adsorbent material 20, such as functionalized inorganic granular material / inorganic granular material, into the cavity 18 of the static adsorption device. This embodiment successively uses the tested adsorbent materials as functionalized inorganic granular material and inorganic granular material adsorption to conduct experiments, tests and compare the adsorption effects. After installing a soft gasket between the connecting flanges to squeeze and seal, put it into the heating and heat preservation device, connect the experimental pipeline, close and lock the two heating and heat preservation devices, and then turn on the carrier gas, vacuum pump, mass flow controller and pressure controller. After replacing the air in the stainless steel sealed container for 2 hours, turn off the carrier gas, mass flow controller, pressure controller, high temperature resistant vacuum needle valves at the front and rear ends of the stainless steel sealed container and the vacuum pump. The temperature of the static adsorption zone is set by the temperature controller and after reaching 20 min, the temperature of the gas generation zone is set. After the functionalized inorganic particle material / inorganic particle adsorption material has been in contact with the gaseous Te for a certain period of time, the stainless steel cold trap is cooled with liquid nitrogen, and the vacuum pump, carrier gas, mass flow controller, pressure controller, and high-temperature vacuum needle valves at the front and back ends are turned on to purge the unabsorbed gaseous Te and condense it in the cold trap. When the temperature of the device drops to room temperature, turn off the vacuum pump. When the air pressure in the device reaches atmospheric pressure, turn off the carrier gas, mass flow controller, and pressure controller. Turn on the two heating and heat preservation devices to take out the static adsorption device, and then take out the inorganic particle material / inorganic particle material after adsorbing the gaseous Te. The adsorbed Te is eluted with acid and its concentration is measured. The experimental results are as follows: Fig. 9 As shown, the functionalized inorganic particle material exhibits excellent adsorption and purification ability compared with the unfunctionalized inorganic particle material.

[0045] (II) Dynamic adsorption experiment

[0046] In the dynamic adsorption process, 0.1 g of single substance Te is placed in the quartz boat 39 of the experimental material volatilization device 6, and the adsorbed material to be tested is placed in multiple adsorption dishes 14 at the same time, and then the adsorption dishes 14 are placed in the dynamic adsorption device. In this embodiment, ten layers of adsorption dishes are used for adsorption experiments. The dynamic adsorption device is placed in two heating and heat preservation devices and closed and locked. Soft gaskets are placed in each blade of the connecting flange, and the screws are tightened before placing it in the carrier gas heating furnace. The vacuum pump, carrier gas, carrier gas heating furnace, mass flow controller and pressure controller are turned on, and the absolute pressure and carrier gas flow rate in the device are adjusted to a certain value. The air in the device is replaced, and the test gas contacts the adsorbed material to be tested through the vents at the bottom of each layer of adsorption dishes 14 to conduct a dynamic adsorption experiment. The temperature of the dynamic adsorption zone of the heating furnace is adjusted and maintained for one hour, and then the temperature of the gas generation zone is adjusted. After a period of reaction, the heating furnace is cooled, the carrier gas heating furnace is turned off, and the vacuum pump is turned off after the temperature drops to room temperature. After the device pressure reaches atmospheric pressure, the carrier gas, mass flow controller and pressure controller are turned off. The functionalized inorganic particle materials with different numbers of layers were taken out, and the amount of gaseous Te adsorbed by each layer of the functionalized inorganic particle materials was measured. Fig.10 The distribution curve of gaseous Te shows that the third layer can completely purify the volatilized gaseous Te, indicating that the purification material has a good purification ability for the flowing high-temperature gaseous Te.

[0047] Since the test gas is cooled into a solid by the cold trap, the device of the utility model has no possibility of radioactive gas contamination.

[0048] In summary, the device of the utility model can simulate the static and dynamic adsorption experiments of the test adsorption material on the high-temperature volatilized radioactive test gas in a static or flowing state, and obtain the adsorption performance of the test adsorption material under different states. During the experiment, the experimental gas is completely isolated from the outside world, and after the experiment, the test gas can be completely condensed into a solid state through the action of the cold trap, and there is no negative impact of the escape of the test gas on the outside world.

Claims

1. A device for measuring the purification effect of high-temperature radioactive gas, characterized in that The device includes an experimental gas generating device, an adsorption device, a pressure control device and an exhaust gas purification device which are interconnected in sequence, pipelines connecting the aforementioned devices and valves arranged on the relevant pipelines, a heating and heat preservation device and the experimental gas generating device and the adsorption device are all arranged inside the heating and heat preservation device.

2. The device according to claim 1, characterized in that The pressure control device consists of a vacuum pump and a pressure controller.

3. The device according to claim 2, characterized in that The experimental gas generating device is composed of an experimental carrier gas source, an experimental carrier gas heating device, a mass flow controller and a volatilization device for the experimental substance under test.

4. The device according to claim 3, characterized in that The exhaust gas purification device is a cold trap.

5. The device according to claim 4, characterized in that The carrier gas source is an inert gas, and the experimental carrier gas heating device consists of a muffle furnace and a metal coil placed therein.

6. The device according to claim 5, characterized in that The experimental substance volatilization device is composed of an outer shell with a cavity inside and a connecting pipe, a sample dish placed in the outer shell cavity, a quartz boat placed in the sample dish and containing the tested volatilized material, and an upper cover with a ventilation pipeline and sealably fixed to the outer shell, and a ventilation hole is opened on the part of the sample dish located outside the sample dish.

7. The device according to any one of claims 1 to 6, characterized in that The adsorption device is composed of a static adsorption device and a dynamic adsorption device, wherein: The static adsorption device is composed of a shell with a cavity inside, a static adsorption dish placed in the shell cavity, and an upper cover with a connecting flange that can be sealed and fixed to the shell by bolts. The static adsorption dish is provided with at least one adsorption hole in which the adsorption material can be filled, and a small hole for ventilation is opened at the bottom of the adsorption hole; The dynamic adsorption device consists of a tubular shell, a plurality of dynamic adsorption dishes stacked in the tubular shell, and a cover with a flange thereon. A ventilation hole is opened at the bottom of each dynamic adsorption dish, and the adsorption material to be tested is placed in the dynamic adsorption dish.

8. The device for measuring the purification effect of high-temperature radioactive gas according to claim 7, characterized in that The heating and heat preservation device is made of heat preservation material and is composed of two heating and heat preservation devices which are hinged and can be locked and opened. An area is provided in which a volatilization device, a static adsorption device or / and a dynamic adsorption device for the experimental substance to be tested can be placed. The heating and heat preservation device is provided with a heating device in the area of ​​the volatilization device, the static adsorption device or / and the dynamic adsorption device.

9. The device for measuring the purification effect of high-temperature radioactive gas according to claim 8, characterized in that The heating devices of the three areas where the experimental substance volatilization device, the static adsorption device and / or the dynamic adsorption device are placed in the heating and heat preservation device are respectively provided with independent temperature control units.

10. The device for measuring the purification effect of high-temperature radioactive gas according to claim 9, characterized in that The connection device between the tested experimental substance volatilization device, the static adsorption device and / or the dynamic adsorption device is a flange with a knife edge and a soft metal gasket, which is sealed by the knife edge of the soft gasket.

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