An activation system for activating hydrogen storage materials
By designing an activation system including the main airflow path, quantitative container, air pressure detection part, isolation valve, temperature regulation device and activation container group, the automation and efficiency of the activation treatment of hydrogen storage materials are solved, and efficient and consistent activation effects are achieved.
Patent Information
- Application Number
- CN202310004669.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-01-03
- Publication Date
- 2025-05-30
- Estimated Expiration
- 2043-01-03
AI Technical Summary
Hydrogen storage materials need to be activated before use to remove surface oxide films and impurities and improve their performance of absorbing and discharging hydrogen isotopes, but the prior art lacks an automated and efficient activation system.
An activation system including an airflow main path, a quantitative container, a pressure detector, an isolation valve, a temperature regulating device and an activation container group is provided. The quantitative circulation of the activation gas is realized through the airflow main path between the quantitative container and the activation container group, and the activation process is accurately controlled by the temperature regulating device and the control device to improve activation efficiency and consistency.
The efficient activation of multiple activation containers is achieved, the consistency of activation efficiency and effect is improved, the influence of human factors is reduced, and the degree of automation and versatility of the system is enhanced.
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Figure CN115973997B_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of hydrogen storage material activation, and particularly relates to an activation system for activating hydrogen storage materials. Background Art
[0002] Hydrogen storage materials can achieve reversible hydrogen isotope absorption and release. Compared with traditional hydrogen storage methods, they have advantages such as safety, high efficiency, and high density. Since the surface of hydrogen storage materials is prone to form oxide films or adsorb other impurities, which will greatly affect the normal hydrogen isotope absorption and release of hydrogen storage materials. Therefore, hydrogen storage materials need to be activated before use to obtain better performance. Summary of the Invention
[0003] In view of this, the present application expects to provide an activation system for activating hydrogen storage materials.
[0004] To achieve the above object, an embodiment of the present application provides an activation system for activating hydrogen storage materials, including an air flow main path, a quantitative container, a first air pressure detection component, a first isolation valve, a temperature adjustment device, and an activation container group. The activation container group includes a plurality of activation containers. The quantitative container is used to store activation gas. The activation containers contain hydrogen storage materials. The activation containers are provided with access valves. The temperature adjustment device is used to adjust the temperature of the activation containers. The activation container group is connected to the quantitative container through the air flow main path. The first isolation valve is arranged on the pipeline of the air flow main path between the quantitative container and the activation container group. The first isolation valve can selectively conduct or cut off the air flow main path. The first air pressure detection component is arranged on the air flow main path.
[0005] In some embodiments, the activation system includes an exhaust main valve, a vacuum pumping device, and a vacuum branch. The vacuum branch is connected to the pipeline of the air flow main path between the quantitative container and the activation container group. The exhaust main valve and the vacuum pumping device are both arranged on the vacuum branch. The exhaust main valve is used to selectively conduct or cut off the vacuum branch.
[0006] In some embodiments, the vacuum pumping device includes a rough vacuum pump, a fine vacuum pump, and a diversion pipe. The inlets of the rough vacuum pump and the fine vacuum pump are both connected to the vacuum branch. The diversion pipe connects the outlet of the fine vacuum pump and the inlet of the rough vacuum pump.
[0007] In some embodiments, the temperature adjustment device includes an electric heater. The electric heater is formed with a heating groove. The heating groove is used to place at least one of the activation containers.
[0008] In some embodiments, the electric heater includes a temperature control element, a temperature measuring element, and a heating jacket. The heating jacket is formed with the heating groove. The temperature measuring element is configured to detect the temperature of the heating jacket. Both the temperature measuring element and the heating jacket are electrically connected to the temperature control element, and the temperature control element controls the heating jacket according to the temperature detected by the temperature measuring element.
[0009] In some embodiments, the temperature regulating device includes a placement container and a cooler. The placement container is formed with a cooling groove and a cooling chamber. The cooling groove is configured to place at least one of the activation containers. The cooling chamber is located on the outer periphery of the cooling groove. The cooling chamber communicates with the cooler. The cooler is configured to cool the refrigerant, and the cooling chamber is configured to circulate the refrigerant from the cooler.
[0010] In some embodiments, the activation system includes an activation gas source, a second air pressure detection component, a second isolation valve, and a gas supply pipeline. The activation gas source communicates with the metering container through the gas supply pipeline. The second air pressure detection component is disposed on the gas supply pipeline. The second isolation valve is disposed on the pipeline of the gas supply pipeline between the metering container and the second air pressure detection component.
[0011] In some embodiments, the activation system includes a cleaning gas source and a cleaning gas pipeline. The cleaning gas source communicates with the cleaning gas pipeline, and the cleaning gas pipeline communicates with the gas supply pipeline.
[0012] In some embodiments, the activation system includes an airtightness detection gas source and an airtightness gas pipeline. The airtightness detection gas source communicates with the airtightness gas pipeline, and the airtightness gas pipeline communicates with the gas supply pipeline.
[0013] In some embodiments, the activation system includes a main isolation valve, a flow isolation valve, a flow controller, a flow branch, a first isolation valve, at least one flow branch pipe, and a plurality of second isolation valves. The main isolation valve is disposed on the pipeline of the main air flow path between the first air pressure detection component and the activation container group. The first isolation valve is disposed on the pipeline of the main air flow path between the main isolation valve and the activation container group. Two of the second isolation valves are disposed between adjacent two of the activation containers. One flow branch pipe is disposed between adjacent two of the second isolation valves. The flow branch pipe communicates with the flow branch. The flow branch communicates with the pipeline of the main air flow path between the main isolation valve and the first isolation valve. Both the flow controller and the flow isolation valve are disposed on the flow branch.
[0014] In some embodiments, the activation system includes a processing device and a control device. The processing device, the first air pressure detection component, the first isolation valve, and the temperature regulating device are all communicatively connected to the control device.
[0015] In some embodiments, the main air flow path adopts a stainless steel pipe.
[0016] In some embodiments, the inner surface of the stainless steel pipe is treated by electrolytic polishing.
[0017] On the one hand, the activation system provided by the embodiments of the present application can activate multiple activation containers with high activation efficiency. On the other hand, the activation gas circulates between any one of the quantitative container and the activation containers in the activation container group. The quantitative container can be used to enable the hydrogen storage material in the activation container to adsorb or desorb the activation gas, so as to realize the quantitative activation of the quantitative container. The operation is simple, and the activation efficiency of the activation container and the consistency of the activation effect can be greatly improved. Description of the Drawings
[0018] Figure 1 It is a schematic diagram of the activation system in an embodiment of the present application.
[0019] Description of the Reference Numerals
[0020] Quantitative container 1; inlet valve 11 of quantitative container 1; first air pressure detection member 2; first air pressure detection valve 201; first pressure sensor 202; first isolation valve 3; activation container group 4; activation container 41; access valve 42; hand valve 43; exhaust main valve 5; vacuum pumping device 6; rough pumping pump 61; fine pumping pump 62; diversion pipe 63; first inlet pipe 64; second inlet pipe 65; first path valve 66; second path valve 67; third path valve 68; second air pressure detection member 7; second air pressure detection valve 71; second pressure sensor 72; second isolation valve 8; total isolation valve 9; flow isolation valve 10; flow controller 11; first isolation valve 12; second isolation valve 13; main second isolation valve 13a; sub-second isolation valve 13b; vacuum gauge 14; vacuum gauge valve 15; vacuum valve 16; atmosphere isolation valve 17; first filter 18; first gas source valve 19; second filter 20; second gas source valve 21; third filter 22; third gas source valve 23; circulation isolation valve 24; quantitative isolation valve 25;
[0021] Main air flow path 100; vacuum branch 200; gas supply path 300; cleaning gas path 400; airtight gas path 500; flow branch 600; flow branch pipe 700; detection pipe 800; atmosphere gas path 900; circulation branch 1000; quantitative branch 1100; Detailed Embodiments
[0022] It should be noted that, without conflict, the embodiments in the present application and the technical features in the embodiments can be combined with each other. The detailed description in the detailed embodiments should be understood as an explanatory illustration of the purpose of the present application and should not be regarded as an improper limitation of the present application.
[0023] The present application will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. The descriptions such as "first" and "second" in the embodiments of the present application are only for descriptive purposes and cannot be construed as indicating or implying their relative importance or implicitly including at least one feature. In the description of the embodiments of the present application, the meaning of "a plurality" is at least two, such as two, three, etc., unless otherwise specifically defined.
[0024] Please refer to Figure 1 , the present application provides an activation system for activating hydrogen storage materials. The activation system includes an air flow main path 100, a quantitative container 1, a first air pressure detection component 2, a first isolation valve 3, a temperature adjustment device, and an activation container group 4. The activation container group 4 includes a plurality of activation containers 41.
[0025] The quantitative container 1 is used to store the activation gas. The volume of the quantitative container 1 is quantified, that is to say, the volume of the quantitative container 1 is known. Exemplarily, the quantitative container 1 has a containing cavity for storing the activation gas, and the volume of the containing cavity is known. In this way, the set volume of the activation gas that can be stored in the quantitative container 1 is known.
[0026] Specifically, the quantitative container 1 has an inlet valve, and the quantitative container 1 is selectively opened or closed through the inlet valve 11 of the quantitative container 1. The inlet valve 11 of the quantitative container 1 is opened so that the activation gas can enter and exit the quantitative container 1. The inlet valve 11 of the quantitative container 1 is closed, and the activation gas cannot enter and exit the quantitative container 1.
[0027] The activation gas is hydrogen and its isotope gases. Isotopes of hydrogen include deuterium and tritium.
[0028] The activation container 41 contains a hydrogen storage material. The hydrogen storage material is usually solid. The hydrogen storage material can adsorb or desorb the activation gas. The reaction between the activation gas and the hydrogen storage material is a reversible reaction. The activation container 41 has an access valve 42. The access valve 42 of the activation container 41 is used to selectively open or close the activation container 41 where it is located. The access valve 42 of the activation container 41 is opened so that the activation gas can enter and exit the activation container 41. The access valve 42 of the activation container 41 is closed, and the activation gas cannot enter and exit the activation container 41.
[0029] The temperature adjustment device is used to adjust the temperature of the activation container 41. The temperature adjustment device can independently adjust the temperature of each activation container 41. That is to say, the temperature adjustment device can selectively increase or decrease the temperature of each activation container 41.
[0030] The activation container group 4 is connected to the quantitative container 1 through the air flow main path 100. That is to say, the activation gas can flow between the quantitative container 1 and each activation container 41 through the air flow main path 100.
[0031] The first isolation valve 3 is arranged on the pipeline of the main air flow path 100 between the metering container 1 and the activation container group 4. The first isolation valve 3 can selectively conduct or cut off the main air flow path 100. In other words, by closing the first isolation valve 3, the main air flow path 100 is in a cut-off state, and the activation gas in the main air flow path 100 cannot flow between the metering container 1 and all the activation containers 41. By opening the first isolation valve 3, the main air flow body is in a conducting state, and the activation gas can flow between the metering container 1 and any one of the activation containers 41.
[0032] The first air pressure detection component 2 is arranged on the main air flow path 100. The first air pressure detection component 2 is used to detect the air pressure of the main air flow path 100. Exemplarily, the first air pressure detection component 2 is arranged on the pipeline of the main air flow path 100 between the first isolation valve 3 and the activation container group 4. In this way, the air pressure of the activation gas in the metering container 1 can be obtained through the first air pressure detection component 2.
[0033] Activation includes the adsorption and desorption of the activation gas. The activation system has a metering container 1 activation mode. In the metering container 1 activation mode, the activation gas flows between the metering container 1 and any one of the activation containers 41 in the activation container group 4. Through the metering container 1, the hydrogen storage material in the activation container 41 can adsorb or desorb the activation gas to realize the quantitative activation of the metering container 1.
[0034] Taking the adsorption of the activation gas by one activation container 41 as an example, first open the first isolation valve 3 and the inlet valve 11 of the metering container 1. The first air pressure detection component 2 detects that the air pressure is the air pressure of the activation gas in the metering container 1. Since the volume of the metering container 1 is known, the initial volume of the activation gas is known. Then open the access valve 42 of one activation container 41. The activation gas in the metering container 1 enters the activation container 41 through the main air flow path 100. As the hydrogen storage material in the activation container 41 absorbs the activation gas, the air pressure detected by the first air pressure detection component 2 decreases to the first target air pressure, such as zero. Then the access valve 42 of the activation container 41, the first isolation valve 3 and the inlet valve 11 of the metering container 1 can be closed. In this way, the adsorption process is completed. Since the volume of the metering container 1 is known, the remaining volume of the remaining activation gas in the metering container 1 can be obtained through the first target air pressure, and the volume of the activation gas adsorbed by the activation container 41 can be calculated according to the gas state equation to realize quantitative adsorption.
[0035] It should be noted that the adsorption process can be completed through multiple adsorption steps. Exemplarily, as the hydrogen storage material in the activation container 41 absorbs the activation gas, the rate of decrease in the air pressure detected by the first air pressure detector 2 is relatively low. For example, during the quantitative activation process of the quantitative container 1, if the rate of decrease in the air pressure detected by the first air pressure detector 2 is less than 20 Pa / s (Pascal per second), the access valve 42 of the activation container 41, the first isolation valve 3, and the inlet valve 11 of the quantitative container 1 can be closed to complete one adsorption step. The quantitative capacity of the single quantitative container 1 is calculated based on the change in the air pressure value of the first air pressure detector 2 through the gas state equation. The above adsorption steps can be repeated until the adsorption is completed. For example, depending on the volume of the quantitative container 1 and the different hydrogen storage materials in the activation container 41, the above adsorption steps can be repeated as needed until adsorption saturation, and the cumulative adsorption amount of the activation gas can be used to obtain the saturated adsorption capacity of the activation container 41.
[0036] It can be understood that since a large amount of heat is released during the process of the hydrogen storage material adsorbing the activation gas, the temperature of the activation container 41 can be reduced by a temperature control device and left standing at room temperature, such as around 20 °C, to ensure complete adsorption.
[0037] Taking the desorption of the hydrogen storage material in the activation container 41, that is, the release of the activation gas, as an example, when there is no activation gas in the quantitative container 1, the activation container 41 can be heated by a temperature control device first to make the activation gas escape from the hydrogen storage material, and then the access valve 42 of the heated activation container 41 is opened, and the activation gas in the hydrogen storage material is completely desorbed and released into the quantitative container 1. In this way, the adsorption process is completed.
[0038] It should be noted that the adsorption process can be completed through multiple desorption steps. Exemplarily, as the activation gas in the hydrogen storage material in the activation container 41 gradually decreases, the rate of increase in the air pressure detected by the first air pressure detector 2 gradually decreases until the rate of increase in the air pressure detected by the first air pressure detector 2 is relatively slow. For example, to ensure safety, when the air pressure value detected by the first air pressure detector 2 does not exceed 35 kPa (kilo-Pascal), heating of the activation container 41 is stopped, and the access valve 42 of the heated activation container 41 is closed. The air pressure value of the first air pressure detector 2 at this time can be recorded to complete one desorption, that is, release process. The above release process can be repeated, and through multiple releases until complete release. The specific amount of the activation gas released in each release process is calculated according to the corresponding gas state equation, and the cumulative amount of the activation gas released in each release process can be used to obtain the total release amount of the activation container 41.
[0039] It should be noted that before the desorption of the activation container 41, if there is activation gas in the quantitative container 1, the activation gas in the quantitative container 1 needs to be emptied to keep the inside of the quantitative container 1 free of activation gas.
[0040] It can be understood that by controlling the heating temperature of the temperature regulating device, the activation gas can be released more smoothly to ensure safety.
[0041] On the one hand, the activation system provided by the embodiment of the present application can activate multiple activation containers 41 with high activation efficiency. On the other hand, the activation gas circulates between any one of the quantitative container 1 and the activation container group 4, i.e., the activation container 41. Through the quantitative container 1, the hydrogen storage material in the activation container 41 can adsorb or desorb the activation gas, so as to realize the quantitative activation of the quantitative container 1. The operation is simple, and the activation efficiency and the consistency of the activation effect of the activation container 41 can be greatly improved.
[0042] Exemplarily, in some embodiments, the temperature regulating device can heat the activation container 41 to a range between 100°C and 700°C. In this way, the activation gas in the hydrogen storage material can be desorbed.
[0043] The hydrogen storage material is made of metal. Exemplarily, the hydrogen storage material includes but is not limited to LaNi 4.25 Al 0.75 (lanthanum nickel aluminum), ZrCo (zirconium cobalt), U (uranium), etc. The hydrogen storage material can improve the reliability and safety of storing hydrogen and its isotope gases.
[0044] In one embodiment, please refer to Figure 1 , the first air pressure detection component 2 includes a first air pressure detection valve 201 and a first pressure sensor 202. Opening the first air pressure detection valve 201 allows the activation gas in the main air flow path 100 to contact the first pressure sensor 202, or closing the first air pressure detection valve 201 isolates the activation gas in the main air flow path 100 from the first pressure sensor 202. In this way, it is convenient to open the first air pressure detection valve 201 when the first pressure sensor 202 is needed to detect the air pressure. When the first pressure sensor 202 is not needed to detect the air pressure, the first air pressure detection valve 201 is closed.
[0045] In related technologies, the activation treatment of hydrogen storage materials is mostly in the laboratory stage, and no automatic treatment device has been seen. Most of the activation operations, data recording, and analysis are manually completed. The operation sequence, time interval, heating temperature, and temperature holding time are all manually controlled. The efficiency is low and the consistency is difficult to guarantee. The performance of the hydrogen storage container after activation depends largely on manual operation, resulting in great uncertainty. In view of this, in some embodiments, the activation system includes a processing device and a control device. The processing device, the first air pressure detection component 2, the first isolation valve 3, and the temperature control device are all communicatively connected to the control device. The control device can collect data of the activation system, such as temperature, air pressure, and mass flow of the mass flow controller 11, and control the operation of the first air pressure detection component 2, the first isolation valve 3, the temperature control device, etc. according to the above data. The processing device is used for operations such as data calculation and storage. Through the processing device and the control device, precise control of the activation operation can be achieved, the influence of human factors can be reduced, the labor input can be reduced, the consistency of the performance of the hydrogen storage material after activation can be guaranteed, and automation can be realized. The activation system provided by this application has the characteristics of high automation, strong versatility, and simple and convenient operation.
[0046] The processing device includes, but is not limited to, a computer.
[0047] The control device includes a controller, a serial communication gateway, a data acquisition communication data link, a signal acquisition circuit, and an execution circuit. The data acquisition part can collect temperature, the mass flow of the mass flow controller 11, air pressure, and vacuum degree. The controller can control the process gas transmission and transportation functions of each functional valve of the system, control the temperature control function, timing, interval, etc. of the temperature control device, so as to realize the activation of the hydrogen storage material in the activation container 41, and output the absorption and release capacity under different conditions.
[0048] The controller can be a Programmable Logic Controller (PLC). As a real-time controller, the PLC collects all information and is used for control instruction output and timing logic control. The software program of the processing device, such as a computer, operates automatically according to the set steps and operation timing, can generate data records, and can automatically generate activation process record documents.
[0049] In some embodiments, the volumes of the respective activation containers 41 are equal. In this way, a quantitative container 1 can be adopted, thereby reducing the operation of replacing the quantitative container 1.
[0050] It should be understood that in some embodiments, the volumes of at least two activation containers 41 are not equal.
[0051] In one embodiment, the activation container 41 is provided with a manual valve 43, which can be manually opened or closed to activate the container 41. In this way, on the one hand, safety can be improved, and on the other hand, it is convenient to use the activated activation container 41, for example, in production or living occasions.
[0052] In some embodiments, the main gas flow path 100 is made of a stainless steel pipe. The stainless steel pipe can avoid the radiation damage caused by radioactive hydrogen isotopes, and not only has a long service life, but also has high safety.
[0053] The types of stainless steel pipes include but are not limited to 316 stainless steel, 316L stainless steel, 304 stainless steel, or 304L stainless steel, etc.
[0054] In some embodiments, the inner surface of the stainless steel pipe is treated by electrolytic polishing. This can avoid the adsorption and residue of various gases, such as activation gases, on the inner surface of the stainless steel pipe.
[0055] The pipe joints in the main gas flow path 100 can be sealed with a sealing material or sealed by argon arc welding. The materials of the sealing material include but are not limited to stainless steel or pure nickel, etc. In this way, the radiation damage caused by radioactive hydrogen isotopes can be avoided from damaging the sealing performance and causing the leakage of radioactive substances.
[0056] In some embodiments, the activation system includes a temperature detector for detecting the temperature of the activation gas in the metering container 1. Exemplarily, a part of the temperature detector extends into the accommodation cavity to detect the temperature in the accommodation cavity. In this way, the absorbed amount of the activation gas can be calculated by the gas state equation.
[0057] In one embodiment, please refer to Figure 1 , the activation system includes an exhaust main valve 5, a vacuum pumping device 6, and a vacuum branch 200. The vacuum branch 200 communicates with the pipeline of the main gas flow path 100 between the metering container 1 and a plurality of activation containers 41. The exhaust main valve 5 and the vacuum pumping device 6 are both arranged on the vacuum branch 200. The exhaust main valve 5 is used to selectively conduct or cut off the vacuum branch 200. Specifically, in the air flow direction of vacuum pumping, the exhaust main valve 5 is located upstream of the vacuum pumping device 6. The vacuum pumping device 6 is used to pump the activation system to a vacuum.
[0058] For example, before activating the hydrogen storage material, the vacuum degree can be made to reach a target value, such as 10 - 4 Pa magnitude, by the vacuum pumping device 6.
[0059] Exemplarily, before performing the activation operation, the activation system is evacuated first. The evacuation step before the activation treatment includes: first opening the inlet valve 11 of the metering container 1, the first isolation valve 3, and the access valve 42 of the activation container 41 to be activated, and then opening the evacuation device 6 to make the pressure drop below the target value. Taking the target value of 10 -4 Pa as an example, it can be evacuated until the pressure value shown by the first air pressure detector 2 reaches 10 -4 Pa or below.
[0060] In one embodiment, please refer to Figure 1 , the activation system includes a detection tube 800, a vacuum gauge 14, and a vacuum gauge valve 15. The detection tube 800 communicates with the vacuum branch 200 and the air flow main path 100. The vacuum gauge 14 and the vacuum gauge valve 15 are both arranged on the detection tube 800. The vacuum gauge valve 15 is used to conduct or cut off the detection tube 800. The vacuum gauge 14 can be used for low-pressure measurement, that is, for vacuum measurement below atmospheric pressure. Opening the vacuum gauge valve 15 enables the vacuum gauge 14 to detect the vacuum degree between the vacuum branch 200 and the air flow main path 100, or closing the vacuum gauge valve 15 isolates both the vacuum branch 200 and the air flow main path 100 from the vacuum gauge 14. In this way, it is convenient to open the vacuum gauge valve 15 when it is necessary to use the vacuum gauge 14 to detect the vacuum degree. When it is not necessary to use the vacuum gauge 14 to detect the vacuum degree, the vacuum gauge valve 15 is closed.
[0061] Exemplarily, in one embodiment, since there is generally a slightly positive pressure protective gas in the activation container 41, after the activation container 41 is connected to the air flow main path 100, the access valve 42 of the activation container 41 can be opened first, and the activation container 41 is evacuated to an appropriate pressure at room temperature, for example, 20°C, and then the vacuum gauge valve 15 is opened until the reading of the vacuum gauge 14 is less than 2.0 Pa. Then the activation container 41 is heated, and evacuation is continued to remove the adsorbed impurities. The control device can control the temperature regulating device to rise to the required temperature and maintain it. Since the release amount of the impurity gas varies with the temperature range, during this period, the on-off state of the vacuum gauge 14 needs to be adjusted according to the released gas pressure to protect the vacuum gauge 14. In this way, the protective gas and part of the adsorbed impurities in the activation container 41 can be removed.
[0062] The protective gas includes, but is not limited to, inert gases such as helium, neon, argon, or krypton.
[0063] In one embodiment, please refer to Figure 1, the vacuum pumping device 6 includes a roughing pump 61, a fine pumping pump 62, and a diversion pipe 63. The inlets of both the roughing pump 61 and the fine pumping pump 62 are connected to the vacuum branch 200, and the diversion pipe 63 connects the outlet of the fine pumping pump 62 and the inlet of the roughing pump 61. Rough pumping is achieved through the roughing pump 61 to reduce the pressure value displayed by the first pressure detection component 2 to a first preset value, and then fine pumping is achieved through the fine pumping pump 62 to reduce the pressure value displayed by the first pressure detection component 2 from the first preset value to a target value. For example, the target value can be 10 -4 Pa or less.
[0064] Exemplarily, first, turn on the roughing pump 61. If it is the initial activation of the entire activation system, the exhaust main valve 5, the first isolation valve 3, and the inlet valve 11 of the metering container 1 need to be turned on in sequence for rough pumping; when the pressure value displayed by the first pressure detection component 2 drops below a first preset value, for example, 5.0 Pa; start the fine pumping pump 62 to perform fine pumping on the system. When the system pressure drops to the target value, for example, 10 -4 Pa or less, close the exhaust main valve 5, the first isolation valve 3, and the inlet valve 11 of the metering container 1 to stop vacuum pumping.
[0065] The roughing pump 61 includes, but is not limited to, a vortex pump.
[0066] The fine pumping pump 62 includes, but is not limited to, a molecular pump.
[0067] In one embodiment, please refer to Figure 1 , the vacuum pumping device 6 includes a first inlet pipe 64, a second inlet pipe 65, a first path valve 66, a second path valve 67, and a third path valve 68. The first inlet pipe 64 connects the vacuum branch 200 and the inlet of the roughing pump 61, and the first path valve 66 is arranged on the first inlet pipe 64 to selectively conduct or cut off the first inlet pipe 64. The second inlet pipe 65 connects the vacuum branch 200 and the inlet of the fine pumping pump 62, and the second path valve 67 is arranged on the second inlet pipe 65 to selectively conduct or cut off the second inlet pipe 65. The third path valve 68 is arranged on the diversion pipe 63 to selectively conduct or cut off the diversion pipe 63. During rough pumping, the first path valve 66 can be opened to conduct the first inlet pipe 64, and the second path valve 67 and the third path valve 68 can be closed. During fine pumping, the first path valve 66 can be closed to cut off the first inlet pipe 64, and the second path valve 67 and the third path valve 68 can be opened to conduct the second inlet pipe 65 and the diversion pipe 63.
[0068] In one embodiment, please refer to Figure 1, the activation system includes a vacuum valve 16, an atmospheric isolation valve 17, and an atmospheric gas path 900 communicating with the atmosphere. The vacuum valve 16 is disposed on the pipeline of the vacuum branch 200 between the exhaust main valve 5 and the vacuum pumping device 6. The atmospheric gas path 900 communicates with the pipeline of the vacuum branch 200 between the exhaust main valve 5 and the vacuum valve 16. The atmospheric isolation valve 17 is disposed on the atmospheric gas path 900. The atmospheric isolation valve 17 is used to conduct or cut off the atmospheric gas path 900. When there is a need, the atmospheric isolation valve 17 can be opened to conduct the atmospheric gas path 900, and the atmospheric gas path 900 is used to discharge the hydrogen gas in the activation system to the outside of the system.
[0069] In one embodiment, the temperature regulating device includes an electric heater. The electric heater forms a heating tank, and the heating tank is used to place at least one of the activation containers 41. The electric heater can convert electrical energy into heat energy. By placing at least one of the activation containers 41 in the heating tank, the electric heater transfers heat energy to the hydrogen storage material in the activation container 41 through heat conduction to increase the temperature of the hydrogen storage material. In this way, when the hydrogen storage material needs to release the activation gas, that is, hydrogen isotopes, the electric heater can heat the activation container 41. The electric heater can quickly increase the temperature in a short time, which is convenient for increasing the temperature of the hydrogen storage material in a short time.
[0070] In one embodiment, the electric heater includes a temperature control element, a temperature measuring element, and a heating sleeve. The heating sleeve forms a heating tank. The temperature measuring element is used to detect the temperature of the heating sleeve. Both the temperature measuring element and the heating sleeve are electrically connected to the temperature control element, and the temperature control element controls the heating sleeve according to the temperature detected by the temperature measuring element. The temperature control element is convenient for automatically controlling the heating temperature of the heating sleeve, so as to be able to effectively and continuously adjust the temperature of the activation container 41. By controlling the heating temperature, the effective release and recycling of hydrogen and its isotope gases are realized, and the safety and efficiency are improved.
[0071] The temperature measuring element can be a temperature sensor.
[0072] In one embodiment, the temperature regulating device includes a placement container and a cooler. The placement container forms a cooling tank and a cooling chamber. The cooling tank is used to place at least one of the activation containers 41. The cooling chamber is located on the outer periphery of the cooling tank. The cooling chamber communicates with the cooler. The cooler is used to cool the refrigerant, and the cooling chamber is used to circulate the refrigerant from the cooler. Specifically, the cooling chamber is isolated from the cooling tank. That is to say, the refrigerant in the cooling chamber will not enter the cooling tank. Through the circulation of the refrigerant, the heat of the hydrogen storage material in the activation container 41 is transferred to the refrigerant through heat exchange, thereby reducing the temperature of the hydrogen storage material. Using the refrigerant method can achieve mild and rapid cooling, ensuring the adsorption rate and safety of the hydrogen storage material.
[0073] The types of the refrigerant include but are not limited to water liquid or cooling oil, etc.
[0074] In one embodiment, please refer toFigure 1 , the activation system includes an activation gas source, a second air pressure detector 7, a second isolation valve 8, and a gas supply line 300. The activation gas source is connected to the metering container 1 through the gas supply line 300. The second air pressure detector 7 is disposed on the gas supply line 300, and the second isolation valve 8 is disposed on the pipeline of the gas supply line 300 between the metering container 1 and the second air pressure detector 7. The activation gas source is used to provide activation gas. The second isolation valve 8 is used to selectively conduct or cut off the gas supply line 300. The second air pressure detector 7 can detect the air supply pressure of the activation gas source. The activation gas source can timely supplement the activation gas in the metering container 1.
[0075] In one embodiment, please refer to Figure 1 , the activation system includes a first filter 18 and a first gas source valve 19. The first filter 18 is disposed on the pipeline of the gas supply line 300 between the activation gas source and the second air pressure detector 7, and the first gas source valve 19 is disposed on the pipeline of the gas supply line 300 between the first filter 18 and the second air pressure detector 7. The first filter 18 is used to filter the activation gas from the activation gas source to prevent impurities from entering the gas supply line 300. The first gas source valve 19 is used to selectively open or close the activation gas source.
[0076] In one embodiment, please refer to Figure 1 , the second air pressure detector 7 includes a second air pressure detection valve 71 and a second pressure sensor 72. Opening the second air pressure detection valve 71 allows the activation gas in the gas supply line 300 to contact the second pressure sensor 72, or closing the second air pressure detection valve 71 isolates the activation gas in the gas supply line 300 from the second pressure sensor 72. In this way, it is convenient to open the second air pressure detection valve 71 when the second pressure sensor 72 is needed to detect the air pressure. When the second pressure sensor 72 is not needed to detect the air pressure, the second air pressure detection valve 71 is closed.
[0077] It can be understood that the first pressure sensor 202 and the second pressure sensor 72 can be two high-pressure pressure gauges with different ranges. The first pressure sensor 202 and the second pressure sensor 72 are used for pressure monitoring and recording during the hydrogen absorption or release process. By opening and closing the first air pressure detection valve 201 and the second air pressure detection valve 71, the first pressure sensor 202 and the second pressure sensor 72 can measure the pressures in the metering container 1 and the multiple activation containers 4.
[0078] In one embodiment, please refer to Figure 1 , the activation system includes a cleaning gas source and a cleaning gas line 400. The cleaning gas source is connected to the cleaning gas line 400, and the cleaning gas line 400 is connected to the gas supply line 300. The cleaning gas source is used to provide cleaning gas. The cleaning gas is used to clean the activation system to remove the residual activation gas in the activation system.
[0079] The cleaning gas includes, but is not limited to, inert gases such as helium, neon, argon, krypton, or xenon.
[0080] In one embodiment, please refer to Figure 1 , the activation system includes a second filter 20 and a second gas source valve 21. The second filter 20 is disposed on the cleaning gas path 400, and the first gas source valve 19 is disposed on the pipeline of the cleaning gas path 400 downstream of the second filter 20. The second filter 20 is used to filter the cleaning gas from the cleaning gas source to prevent impurities from entering the main gas flow path 100. The second gas source valve 21 is used to selectively open or close the cleaning gas path 400.
[0081] In some embodiments, please refer to Figure 1 , the connection point between the cleaning gas path 400 and the gas supply path 300 may be located between the second pressure detection member 7 and the second isolation valve 8.
[0082] In one embodiment, please refer to Figure 1 , the activation system includes an airtightness detection gas source and an airtight gas path 500. The airtightness detection gas source is communicated with the airtight gas path 500, and the airtight gas path 500 is communicated with the gas supply path 300. The airtightness detection gas source is used to provide airtightness detection gas to detect the airtightness of the activation system.
[0083] In one embodiment, please refer to Figure 1 , the activation system includes a third filter 22 and a third gas source valve 23. The third filter 22 is disposed on the airtight gas path 500, and the third gas source valve 23 is disposed on the pipeline of the airtight gas path 500 downstream of the third filter 22. The third filter 22 is used to filter the airtightness detection gas from the airtightness detection gas source to prevent impurities from entering the main gas flow path 100. The third gas source valve 23 is used to selectively open or close the airtight gas path.
[0084] In some embodiments, please refer to Figure 1 , the connection point between the airtight gas path 500 and the gas supply path 300 may be located between the second pressure detection member 7 and the second isolation valve 8.
[0085] In one embodiment, please refer to Figure 1 , the activation system includes a main isolation valve 9, a flow isolation valve 10, a flow controller 11, a flow branch 600, a first isolation valve 12, at least one flow branch pipe 700, and a plurality of second isolation valves 13.
[0086] The main isolation valve 9 is provided on the pipeline of the main gas flow path 100 between the first air pressure detection component 2 and multiple activation containers 41. The first isolation valve 12 is provided on the pipeline of the main gas flow path 100 between the main isolation valve 9 and multiple activation containers 41. Two second isolation valves 13 are provided between two adjacent activation containers 41. A flow branch pipe 700 is provided between two adjacent second isolation valves 13. The flow branch pipe 700 communicates with a flow branch path 600. The flow branch path 600 communicates with the pipeline of the main gas flow path 100 between the main isolation valve 9 and the first isolation valve 12. The flow controller 11 and the flow isolation valve 10 are both provided on the flow branch path 600.
[0087] The flow isolation valve 10 is used to selectively conduct or cut off the flow branch path 600.
[0088] The flow controller 11 is used to control the instantaneous flow value of the activation gas flowing through the flow branch path 600.
[0089] Exemplarily, one of the multiple second isolation valves 13 is opened, and the remaining second isolation valves 13 are closed, so that the activation gas from the flow branch path 600 can enter one of the multiple activation containers 41.
[0090] Exemplarily, the main isolation valve 9 can selectively conduct or cut off the main gas flow path 100 and the flow branch path 600. In this way, the activation gas from the activation gas source can enter the flow branch path 600.
[0091] The first isolation valve 12 can prevent the activation gas from flowing back to the flow branch path 600. For example, when the first isolation valve 12 is closed, the activation gas in the flow branch path 600 flows to the activation container 41 and cannot flow back to the flow branch path 600 anymore.
[0092] In one embodiment, please refer to Figure 1 , the activation system has a flow control activation mode. In the flow control activation mode, the activation gas flows through the flow branch path 600, the flow controller 11, and the flow branch pipe 700 and enters each activation container 41. The instantaneous flow value of the activation gas is controlled by the flow controller 11. In this way, in the flow control activation mode, quantitative activation is achieved through the flow controller 11. Specifically, by setting the instantaneous flow value of the flow controller 11, the activation gas flows through the flow controller 11 and enters and exits the activation container 41. The operation of the flow controller 11 is terminated according to the set conditions, and the cumulative flow of the flow controller 11 is recorded, so as to achieve quantitative activation. The quantitative value of quantitative activation is the cumulative flow, and the quantitative value is taken from the mass flow controller 11.
[0093] Exemplarily, in the flow control activation mode, the specific steps of adsorption may include: first, set the instantaneous flow rate value of the flow controller 11 to a preset value, adjust the pressure of the activation gas source to a preset pressure, then successively open the first isolation valve 3, the second isolation valve 8, the main isolation valve 9, the flow isolation valve 10, the access valve 42 of the activation container 41 and the corresponding second isolation valve 13, and close the first isolation valve 12 and the remaining second isolation valves 13. When the instantaneous flow rate value of the flow controller 11 reaches the preset value, terminate the operation of the flow controller 11, and successively close the flow isolation valve 10, the corresponding second isolation valve 13, the access valve 42 of the activation container 41 and the inlet valve of the activation gas source, and record the cumulative flow rate of the flow controller 11. In this way, quantitative activation can be achieved through the cumulative flow rate of the flow controller 11.
[0094] It can be understood that since a large amount of heat is released during the process of the hydrogen storage material adsorbing hydrogen isotopes, the activation container 41 can be circulated and cooled to room temperature, such as 20°C, through a temperature control device, such as a placement container and a cooler, to ensure complete adsorption.
[0095] Exemplarily, in the flow control activation mode, the specific steps of desorption may include: first, set the instantaneous flow rate value of the flow controller 11 to a preset value, heat the activation container 41 to a temperature between 100°C and 700°C through a temperature control device, and wait for a certain period of time to allow the heat to be fully transferred to the hydrogen storage material. Then successively open the first isolation valve 3, the inlet valve 11 of the metering container 1, the main isolation valve 9, the flow isolation valve 10, the corresponding second isolation valve 13 and the inlet valve of the activation container 41, and close the first isolation valve 12. When the instantaneous flow rate value of the flow controller 11 is less than the preset value, terminate the operation of the flow controller 11. In this way, the activation gas in the activation container 41 can enter the metering container 1 to reduce the external emission of the activation gas.
[0096] In some embodiments, during the desorption process, the exhaust main valve 5 can also be opened, and the vacuum pumping device 6 can be started to accelerate the desorption of the activation gas in the hydrogen storage material.
[0097] The preset value can be 0.05 SLM (Standard Liter per Minute).
[0098] Compared with the flow control activation mode, if the quantitative container 1 activation mode is adopted for quantitative activation, it is possible to choose not to pass through the flow controller 11. A quantitative container 1 with a known volume is used to accurately calibrate each part of the volume, and then the standard intake pressure of the quantitative container 1 is set according to the type of hydrogen storage material in the activation container 41. The valves of the main gas flow path 100 can be continuously cycled to open to realize the adsorption process of the activation container 41. The adsorption process records the number of times the access valve 42 of the activation container 41 is opened and closed, as well as the pressure after the valve is closed and the temperature data of the quantitative container 1. The specific activation adsorption capacity is calculated based on the gas state equation and the recorded pressure and temperature data of the quantitative container 1. The high-temperature desorption process is similar to the adsorption process, except that the opening and closing states of each valve are controlled to form a release path. Those skilled in the art can understand the release path according to the solution disclosed in this application, and will not be elaborated here.
[0099] In one embodiment, please refer to Figure 1 , the activation system has a cyclic activation mode. In the cyclic activation mode, the activation gas circulates between any two activation containers 41 through the flow branch 600, the flow controller 11, and the flow branch pipe 700, and the instantaneous flow value of the activation gas is controlled by the flow controller 11. In this way, in the cyclic activation mode, quantitative activation is achieved through the flow controller 11. In the cyclic activation mode, the quantitative container 1 can be isolated from the activation container group 4 by closing the first isolation valve 3, and cyclic activation can be performed between multiple activation containers 41 in the activation container group 4, with the flow count of the flow controller 11 as the quantitative standard. By selecting an appropriate adsorption / desorption path, the activation gas can be recycled between two activation containers 41 for activation operations, realizing the effective utilization of the activation gas. Especially for deuterium gas with a relatively high price, it has a relatively significant cost savings.
[0100] Taking two activation containers 41 as an example, one of the activation containers 41 is defined as the first activation container 41a, and the other activation container 41 is defined as the second activation container 41b. Among the two second isolation valves 13 between the first activation container 41a and the second activation container 41b, the second isolation valve 13 close to the first activation container 41a is the main second isolation valve 13a, and the second isolation valve 13 close to the second activation container 41b is the auxiliary second isolation valve 13b. Taking the desorption of the activation gas in the first activation container 41a to the adsorption of the second activation container 41b as an example: set the instantaneous flow value of the flow controller 11, set the heating temperature of the first activation container 41a between 100°C and 700°C through the temperature adjustment device, wait for a certain period of time for the heat to transfer to the hydrogen storage material inside the first activation container 41a, and establish a gas flow path: sequentially open the access valve 42 of the second activation container 41b, the auxiliary second isolation valve 13b, the flow isolation valve 10, the first isolation valve 12, and the access valve 42 of the first activation container 41a. The activation gas released in the first activation container 41a, that is, hydrogen and its isotope gas, enters the second activation container 41b for adsorption. Gradually increase the heating temperature of the first activation container 41a until the preset release end temperature is reached, and the pressure between the first activation container 41a and the second activation container 41b reaches equilibrium. Terminate the operation of the flow controller 11 and record the cumulative flow of the flow controller 11, which is the adsorption amount of the second activation container 41b during this adsorption process. When the second activation container 41b desorbs the activation gas to the first activation container 41a, each valve can be opened in reverse. Those skilled in the art can reasonably obtain according to the above solution and will not be elaborated here.
[0101] It should be noted that in the description of the gas flow path in this application, if not otherwise specified, the relevant valves can be in a closed state.
[0102] In some embodiments where the number of activation containers 41 is two, please refer to Figure 1 , the activation system includes a circulation branch 1000 and a circulation isolation valve 24. One end of the circulation branch 1000 is connected to the pipeline of the flow branch 600 between the flow isolation valve 10 and the flow controller 11, the other end of the circulation branch 1000 is connected to the second activation container 41b, and the circulation isolation valve 24 is arranged on the circulation branch 1000 to conduct or cut off the circulation branch 1000. The circulation branch 1000 facilitates the desorption of the activation gas in the second activation container 41b to the first activation container 41a.
[0103] When the second activation container 41b desorbs the activation gas to the first activation container 41a, the heating temperature of the second activation container 41b can be set between 100°C and 700°C through the temperature control device. Wait for a certain period of time for the heat to transfer to the hydrogen storage material inside the second activation container 41b, and establish a gas flow path: successively open the access valve 42 of the first activation container 41a, the circulation isolation valve 24, the flow controller 11, the main second isolation valve 13a, and the access valve 42 of the second activation container 41b, and close the secondary second isolation valve 13b, the flow isolation valve 10, and the first isolation valve 12. Set the instantaneous flow control value of the flow controller 11. The second activation container 41b gradually releases the adsorbed activation gas, and gradually increases the heating temperature of the first activation container 41a until the preset release end temperature is reached. The pressure between the first activation container 41a and the second activation container 41b is balanced, the operation of the flow controller 11 is terminated, and the cumulative flow of the flow controller 11 is recorded, which is the adsorption capacity of the first activation container 41a during this adsorption process.
[0104] It can be understood that in the cyclic activation mode, since the flow controller 11 is used intermittently for the two activation containers 41, the cumulative flow of the flow controller 11 needs to be cleared before each use, and the single flow is cumulatively calculated for each to obtain the saturated adsorption capacity.
[0105] The number of activation containers 41 is two. In some embodiments, please refer to Figure 1 , the activation system includes a quantitative branch 1100 and a quantitative isolation valve 25. One end of the quantitative branch 1100 is connected to the pipeline of the air flow main path 100 between the first pressure detection member 2 and the main isolation valve 9, and the other end of the quantitative branch 1100 is connected to the pipeline of the air flow main path 100 between the main second isolation valve 13a and the secondary second isolation valve 13b. The quantitative isolation valve 25 is arranged on the quantitative branch 1100 to conduct or cut off the quantitative branch 1100. During the process of activating the first activation container 41a and the second activation container 41b in the quantitative container 1 mode, the activation gas can flow between the quantitative container 1 and the first activation container 41a, and between the quantitative container 1 and the second activation container 41b through the quantitative branch 1100, and no longer needs to pass through valve components such as the main isolation valve 9 and the first isolation valve 12. In this way, the activation gas passes through fewer valve components, the air flow path is simpler, and the valve operation steps are further simplified. The first activation container 41a and the second activation container 41b can perform air inlet and outlet operations without affecting each other, and can also read the pressure under different range pressure gauges.
[0106] In some embodiments, all pipelines of the activation system can be made of stainless steel pipes, and the inner surface of the stainless steel pipes is treated by electrolytic polishing. The pipe joints of all pipelines of the activation system can be sealed with sealing materials or sealed by argon arc welding. The materials of the sealing materials include, but are not limited to, stainless steel or pure nickel, etc.
[0107] In some embodiments, all valves of the activation system can be pneumatic valves connected to solenoid valves through air pipes. The on-off state of the solenoid valve is controlled by a transistor drive board, which is connected to the digital output port of the data acquisition card. The signal output ends of the pressure sensor and the temperature sensor are both connected to the signal input end of the data acquisition card. The mass flow controller 11 exchanges data with the data acquisition card, and the data acquisition card is connected to a processing device such as a computer through a signal cable. By automatically controlling each valve through the control device, the accuracy and efficiency of activation are improved.
[0108] In some embodiments, all parts of the activation system that come into contact with the activation gas, such as valves, seals, and joint gaskets, etc., can be made of metals such as stainless steel.
[0109] In some embodiments, the activation system can be used for the activation and performance measurement of activation gases. The activation system can also include a radioactive activity monitoring instrument, which is connected to the main gas flow path 100. A hydrogen concentration monitoring instrument and a gas tritium concentration monitor can be arranged in the atmospheric environment where the activation system is located. In this way, the activation and performance tests using hydrogen and its isotope gases as activation gases can be measured through the above three devices.
[0110] The radioactive activity monitoring instrument includes, but is not limited to, a tritium gas ionization chamber.
[0111] The number of activation containers 41 is not limited. Exemplarily, the number of activation containers 41 is two. The following takes two activation containers 41 as an example to show the specific use of the activation system of the present application. The two activation containers 41 are respectively defined as the first activation container 41a and the second activation container 41b, and the specific description is as follows:
[0112] Vacuum pumping treatment step before activation:
[0113] Step 1: Connect the first activation container 41a and the second activation container 41b that need to be activated to the main gas flow path 100.
[0114] Step 2: Vacuum pump each part through the vacuum pump 6 to ensure that the vacuum degree of the evacuated part reaches 10 -4 Pa magnitude.
[0115] Step 3: First, close the vacuum gauge valve 15 to isolate the vacuum gauge 14. Open the manual valve 43 of the activation container 41, evacuate the activation container 41 at room temperature, open the vacuum gauge valve 15 when the pressure is appropriate, until the reading of the vacuum gauge 14 is less than 2.0 Pa.
[0116] Step 4: Heat the activation container 41, continue to evacuate to remove adsorbed impurities, program-control the temperature rise to the required temperature and maintain it. Since the impurity release amount varies with the temperature range, during this period, it is necessary to adjust the on-off state of the vacuum gauge 14 according to the released gas pressure to protect the vacuum gauge 14, and timely adjust the type of working pump connected to the system.
[0117] Step 5: After degassing at high temperature, from the activation container 41 to the vacuum pumping port, close each valve on the path in turn, turn off the electric heater, and cool the activation container 41 to room temperature.
[0118] The specific process includes: Before performing the activation operation, first, the activation system needs to be evacuated: First, open the roughing pump 61, such as an oil-free scroll pump, and the first path valve 66. If it is an initial activation, it is necessary to open the vacuum valve 16, the evacuation main valve, the main isolation valve 9, the flow isolation valve 10, the access valve 42 of the first activation container 41a, the main second isolation valve 13a, the quantitative isolation valve 25, the circulation isolation valve 24, the secondary second isolation valve 13b, the vacuum gauge valve 15, the first air pressure detection valve 201, the first isolation valve 3, the second isolation valve 8, the inlet valve 11 of the quantitative container 1, and the second air pressure detection valve 71 in sequence to rough-pump the system; when the system pressure drops below 5.0 Pa, open the third path valve 68 in sequence, start the fine pumping pump 62, such as a molecular pump, close the first path valve 66, open the second path valve 67, and fine-pump the system. When the system pressure drops below 10 -4 Pa, stop the roughing pump 61 and the fine pumping pump 62, and close the above valve parts.
[0119] Before the activation treatment, set the temperature of the cooling water in the chiller to about 20 °C.
[0120] The activation step can select one of the following three quantitative activation methods:
[0121] I. Flow control activation mode
[0122] Taking the operation of the first activation container 41a as an example, set the instantaneous flow rate value of the flow controller 11. Under the condition of ensuring the stable supply of the gas source in the front-end gas supply pipeline 300, adjust the supply pressure of the activation gas source to the required level. Then, successively open the inlet valve of the activation gas source, the second gas pressure detection valve 71, the second isolation valve 8, the first isolation valve 3, the first gas pressure detection valve 201, the main isolation valve 9, the flow isolation valve 10, the main second isolation valve 13a, and the access valve 42 of the first activation container 41a. Run the flow controller 11 according to the set result. When the instantaneous flow rate value of the flow controller 11 < 0.05 SLM, terminate the operation of the flow controller 11 and record the cumulative flow rate of the flow controller 11. Close the flow isolation valve 10, the main second isolation valve 13a, the access valve 42 of the first activation container 41a, and the inlet valve of the activation gas source. Since the hydrogen storage material adsorbs the activation gas and releases a large amount of heat, a cooler and a cooling container can be used to cool and let the first activation container 41a stand still until it reaches about room temperature to ensure complete adsorption.
[0123] Similar to the above method, the main isolation valve 9, the flow isolation valve 10, the secondary second isolation valve 13b, and the access valve 42 of the second activation container 41b can be successively opened to achieve the saturated adsorption of the second activation container 41b.
[0124] When the flow control method is used for activation desorption, the process is similar to the adsorption process. Taking the desorption of the second activation container 41b as an example, set the instantaneous flow rate value of the flow controller 11. First, set the heating temperature between 100°C and 700°C through the temperature control device and wait for a certain time for the heat to transfer to the hydrogen storage material in the second activation container 41b. Then, successively open the vacuum valve 16, the evacuation main valve, the first isolation valve 3, the inlet valve 11 of the metering container 1, the first gas pressure detection valve 201, the main isolation valve 9, the first isolation valve 12, the main second isolation valve 13a, the circulation isolation valve 24, and the access valve 42 of the second activation container 41b. When the instantaneous flow rate value of the flow controller 11 < 0.05 SLM, terminate the operation of the flow controller 11 and record the cumulative flow rate of the flow controller 11. Close the access valve 42 of the second activation container 41b. Stop heating the second activation container 41b and cool it to room temperature.
[0125] II. Activation Mode of the Metering Container
[0126] First, the dosing container 1 can be filled with gas using the gas supply line 300. The volume of each part can be accurately calibrated through the dosing container 1 with a known volume. Then, the intake pressure of the dosing volume can be set according to the type of hydrogen storage material. Taking the first activation container 41a as an example, the inlet valve of the activation gas source, the second pressure detection valve 71, the second isolation valve 8, and the inlet valve 11 of the dosing container 1 are opened in sequence. The pressure of the activation gas source is adjusted to the required level, and then the inlet valve of the activation gas source, the second pressure detection valve 71, and the second isolation valve 8 are closed. The first isolation valve 3, the first pressure detection valve 201, the main isolation valve 9, and the first isolation valve 12 are opened in sequence, and the pressure value of the first pressure detection element and the temperature data of the dosing container 1 are recorded. The access valve 42 of the first activation container 41a is opened, and adsorption starts until the reading rate of the pressure value of the first pressure detection element drops below 20 Pa / s. Then, the access valve 42 of the first activation container 41a is closed, and the pressure value of the first pressure detection element and the temperature data of the dosing container 1 are recorded to complete one adsorption process. The specific amount of adsorbed hydrogen isotope is calculated based on the change in the chamber pressure before and after adsorption, the temperature data of the dosing container 1, and the state equation of the corresponding gas. According to the volume of the dosing container 1 and the different materials filled in the container to be activated 41, the above adsorption steps can be repeated as needed until adsorption saturation, and the saturated adsorption capacity of the activation container 41 can be obtained by accumulating the adsorbed hydrogen isotope amounts. Similarly, a large amount of heat is released during the adsorption of hydrogen isotopes, and it is necessary to cooperate with the circulating cooling device to stand still until the temperature reaches around room temperature to ensure complete adsorption.
[0127] During desorption by the volumetric dosing method, the dosing container 1 needs to be emptied first. The specific operation is as follows: The vacuum valve 16, the evacuation main valve, the first isolation valve 12, the main isolation valve 9, the first pressure detection valve 201, the first isolation valve 3, and the inlet valve 11 of the dosing container 1 are opened in sequence, and it is evacuated to a relatively low pressure close to vacuum in sequence. Then, the evacuation main valve and the vacuum valve 16 are closed, and the pressure value of the first pressure detection element and the temperature data of the dosing container 1 are recorded. The heating temperature is adjusted between 100 °C and 700 °C through the temperature control device. After waiting for a certain time for the heat to transfer to the hydrogen storage material, the main isolation valve 9, the first isolation valve 12, and the access valve 42 of the first activation container 41a are opened, and the hydrogen isotope gas is released into the dosing container 1 until the pressure rising speed becomes relatively slow. For example, to ensure safety, the pressure value of the first pressure detection element does not exceed 35 kPa. Then, the access valve 42 of the first activation container 41a is closed, and the pressure value of the first pressure detection element and the temperature data of the dosing container 1 are recorded to complete one release process. The specific amount of released hydrogen isotope is calculated based on the state equation of the corresponding gas, and the total release amount of the activation container 41 can be obtained by accumulating the released hydrogen isotope amounts. When releasing hydrogen isotopes, it is necessary to carefully control the heating state of the container to be activated 41 to ensure that the hydrogen isotope gas can be released smoothly to ensure safety.
[0128] III. Cyclic activation mode
[0129] Taking the desorption of the activation gas in the first activation container 41a and the adsorption in the second activation container 41b as an example: Set the instantaneous flow rate value of the flow controller 11, set the heating temperature between 100°C and 700°C through the temperature control device, wait for a certain time for the heat to transfer to the hydrogen storage material, and successively open the access valve 42 of the second activation container 41b, the secondary second isolation valve 13b, the flow isolation valve 10, the first isolation valve 12, and the access valve 42 of the first activation container 41a. The hydrogen isotope gas released from the first activation container 41a is adsorbed into the second activation container 41b. Gradually increase the heating temperature of the first activation container 41a until the preset release end temperature is reached, and the pressure between the first activation container 41a and the second activation container 41b reaches equilibrium. Terminate the operation of the flow controller 11 and record the cumulative flow of the flow controller 11, which is the adsorption capacity of the second activation container 41b during this adsorption process. When the second activation container 41b desorbs gas into the first activation container 41a, establish a gas flow path: the access valve 42 of the first activation container 41a, the circulation isolation valve 24, the flow controller 11, the main second isolation valve 13a, and the access valve 42 of the second activation container 41b. Set the instantaneous flow rate value of the flow controller 11, gradually increase the heating temperature of the first activation container 41a until the preset release end temperature is reached, and the pressure between the first activation container 41a and the second activation container 41b reaches equilibrium. Terminate the operation of the flow controller 11 and record the cumulative flow of the flow controller 11, which is the adsorption capacity of the first activation container 41a during this adsorption process.
[0130] It can be understood that for a specific activation container 41, a single adsorption and desorption of the activation gas may not achieve the best adsorption performance, that is, complete activation. Therefore, the number of adsorption and desorption cycles, that is, the number of times of the above various activation processes, can be determined according to the differences in specific hydrogen storage materials and usage conditions. When the last activation is completed, the activation gas adsorbed by the activation container 41 needs to be exhausted as much as possible. Therefore, while completing the above release process, it is necessary to evacuate through the vacuum device 6. Exemplarily, successively open the vacuum valve 16, the evacuation main valve, the main isolation valve 9, the first isolation valve 12, the main second isolation valve 13a, the secondary second isolation valve 13b, the access valve 42 of the first activation container 41a, and the access valve 42 of the second activation container 41b, and evacuate the residual activation gas in the first activation container 41a and the second activation container 41b until the reading of the vacuum gauge 14 is less than 5.0 Pa and the pressure at the inlet end of the molecular pump is less than 10 -3 Pa.
[0131] Post-activation treatment steps:
[0132] The activated container 41 after activation treatment has good activity and is easily oxidized by oxygen in the air and poisoned by other impurity gases. If it is not for immediate use, it is best to fill the activated container 41 with a cleaning gas, that is, an inert gas for preservation to prevent air from leaking into the activated container 41 and reducing its performance. The operating steps for filling an inert gas into the activated container 41 that has been desorbed and cooled to room temperature are as follows: successively open the vacuum valve 16, the evacuation main valve, the main isolation valve 9, the first isolation valve 12, the main second isolation valve 13a, the access valve 42 of the first activated container 41a, the secondary second isolation valve 13b, the access valve 42 of the second activated container 41b, the vacuum gauge valve 15, the first air pressure detection valve 201, the first isolation valve 3, the second isolation valve 8, and conduct rough pumping and fine pumping on the system in sequence. When the reading of the vacuum gauge 14 is less than 2.0 Pa and the pressure at the inlet end of the molecular pump is less than 10 -4 Pa, close the vacuum gauge valve 15, the evacuation main valve, and the vacuum valve 16, and open the inlet valve of the cleaning gas source. Adjust the inflation pressure of the first activated container 41a and the second activated container 41b to the required value, and close the hand valve 43 of the first activated container 41a and the hand valve 43 of the second activated container 41b, that is, the filling of the protective gas is completed.
[0133] As described above, it is only the preferred embodiment of the present application and is not used to limit the present application. For those skilled in the art, various changes and modifications can be made to the present application. Any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present application are all included in the protection scope of the present application.
Claims
1. An activation system for activating hydrogen storage materials, characterized in that, it includes an air flow main path, a metering container, a first air pressure detection component, a first isolation valve, a temperature regulating device and an activation container group. The activation container group includes a plurality of activation containers. The metering container is used for storing activation gas. The activation containers contain hydrogen storage materials. The activation containers are provided with access valves. The temperature regulating device is used for regulating the temperature of the activation containers. The activation container group is connected to the metering container through the air flow main path; the first isolation valve is arranged on the pipeline of the air flow main path between the metering container and the activation container group. The first isolation valve can selectively conduct or cut off the air flow main path; the first air pressure detection component is arranged on the air flow main path; the volume of the metering container is quantified; the activation system includes a main isolation valve, a flow isolation valve, a flow controller, a flow branch, a first isolation valve, at least one flow branch pipe and a plurality of second isolation valves. The main isolation valve is arranged on the pipeline of the air flow main path between the first air pressure detection component and the activation container group. The first isolation valve is arranged on the pipeline of the air flow main path between the main isolation valve and the activation container group. Two of the second isolation valves are arranged between adjacent two of the activation containers. One flow branch pipe is arranged between adjacent two of the second isolation valves. The flow branch pipe is connected to the flow branch. The flow branch is connected to the pipeline of the air flow main path between the main isolation valve and the first isolation valve. The flow controller and the flow isolation valve are both arranged on the flow branch; the activation container group includes a first activation container and a second activation container. The second isolation valve close to the first activation container is the main second isolation valve, and the second isolation valve close to the second activation container is the auxiliary second isolation valve; the activation system includes a circulation branch and a circulation isolation valve. One end of the circulation branch is connected to the pipeline of the flow branch between the flow isolation valve and the flow controller. The other end of the circulation branch is connected to the second activation container. The circulation isolation valve is arranged on the circulation branch to conduct or cut off the circulation branch; the activation system has a circulation activation mode. In the circulation activation mode, the activation gas circulates between the first activation container and the second activation container through the flow branch, the flow controller and the flow branch pipe; the activation system includes a metering branch and a metering isolation valve. One end of the metering branch is connected to the pipeline of the air flow main path between the first air pressure detection component and the main isolation valve. The other end of the metering branch is connected to the pipeline of the air flow main path between the main second isolation valve and the auxiliary second isolation valve. The metering isolation valve is arranged on the metering branch to conduct or cut off the metering branch.
2. The activation system according to claim 1, characterized in that, The activation system includes an exhaust main valve, a vacuum pumping device, and a vacuum branch. The vacuum branch communicates with the pipeline of the main gas flow between the metering container and the activation container group. The exhaust main valve and the vacuum pumping device are both arranged on the vacuum branch, and the exhaust main valve is used to selectively conduct or cut off the vacuum branch.
3. The activation system according to claim 2, wherein, the vacuum pumping device includes a roughing pump, a fine pumping pump, and a diversion pipe. The inlets of the roughing pump and the fine pumping pump are both connected to the vacuum branch, and the diversion pipe connects the outlet of the fine pumping pump and the inlet of the roughing pump.
4. The activation system according to claim 1, wherein, the temperature regulating device includes an electric heater which forms a heating tank for placing at least one of the activation containers.
5. The activation system according to claim 4, wherein, the electric heater includes a temperature control element, a temperature measuring element, and a heating jacket. The heating jacket forms the heating tank. The temperature measuring element is used to detect the temperature of the heating jacket. The temperature measuring element and the heating jacket are both electrically connected to the temperature control element, and the temperature control element controls the heating jacket according to the temperature detected by the temperature measuring element.
6. The activation system according to claim 1, wherein, the temperature regulating device includes a placement container and a cooler. The placement container forms a cooling tank and a cooling chamber. The cooling tank is used to place at least one of the activation containers. The cooling chamber is located on the outer periphery of the cooling tank and communicates with the cooler. The cooler is used to cool the refrigerant, and the cooling chamber is used to circulate the refrigerant from the cooler.
7. The activation system according to claim 1, wherein, the activation system includes an activation gas source, a second air pressure detection component, a second isolation valve, and a gas supply pipeline. The activation gas source is connected to the metering container through the gas supply pipeline. The second air pressure detection component is arranged on the gas supply pipeline, and the second isolation valve is arranged on the pipeline of the gas supply pipeline between the metering container and the second air pressure detection component.
8. The activation system according to claim 7, wherein, the activation system includes a cleaning gas source and a cleaning gas pipeline. The cleaning gas source is connected to the cleaning gas pipeline, and the cleaning gas pipeline is connected to the gas supply pipeline.
9. The activation system according to claim 7, wherein, the activation system includes an airtightness detection gas source and an airtightness gas pipeline. The airtightness detection gas source is connected to the airtightness gas pipeline, and the airtightness gas pipeline is connected to the gas supply pipeline.
10. The activation system according to any one of claims 1 to 9, wherein, the activation system includes a processing device and a control device. The processing device, the first air pressure detection component, the first isolation valve, and the temperature regulating device are all communicatively connected to the control device.
11. The activation system according to any one of claims 1 to 9, wherein, the main gas flow pipeline is made of stainless steel pipe.
12. The activation system according to claim 11, It is characterized in that the inner surface of the stainless steel pipe is treated by electrolytic polishing.
Citation Information
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