High-pressure container for hydride preparation

Abstract

The utility model relates to the technical field of hydride preparation, and discloses a high-pressure container for hydride preparation, which comprises a high-pressure tank body, the upper part of the high-pressure tank body is of an opening structure, a sealing cover is assembled at the opening, and a material loading disc capable of being taken out is placed at the lower part of an inner cavity of the high-pressure tank body; a plurality of small chambers capable of being correspondingly and adaptively inserted with small-sized graphite crucibles are formed in the top of the material carrying disc, high-temperature-resistant metal sheets are fixed to the positions, corresponding to the small chambers, of the bottom face of the material carrying disc, and the high-temperature-resistant metal sheets can support the graphite crucibles located in the small chambers; an air inlet is formed in the upper portion of the outer side wall of the high-pressure tank and externally connected with an air supply assembly. An exhaust valve communicated with the inner cavity of the high-pressure tank body is arranged on the sealing cover, and a heating assembly is arranged outside the high-pressure tank body. According to the utility model, magnesium hydride powder is not easy to drift away from the crucible, and negative pressure airflow around the exhaust valve and the magnesium hydride powder are also isolated, so that the flying loss of the magnesium hydride powder is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of hydride preparation, and more specifically, to a high-pressure container for hydride preparation. Background Art

[0002] In exploring the synthesis of nano-magnesium hydride powders, researchers have adopted a variety of techniques, including mechanical ball milling, liquid-phase impregnation, vapor-phase synthesis, and arc heating. Arc heating involves placing magnesium metal in a specialized arc-heated container. Within this environment, the metal undergoes chemical changes in an argon and hydrogen atmosphere. Through a precise collection system, high-quality nano-magnesium hydride powder can ultimately be obtained.

[0003] Traditional arc heating technology involves loading magnesium metal powder into a graphite crucible and placing the crucible inside an arc heating device. This process involves using a high-pressure gas pump to compress argon and hydrogen, which are then fed into the arc heating chamber. The magnesium metal powder then reacts with the hydrogen under the heating of the arc, producing magnesium hydride powder. After the reaction is complete, the excess gas in the arc heating chamber is removed.

[0004] However, in the process of producing magnesium hydride powder by the arc heating method, the compressed gas is fed into the arc heating chamber from below and discharged from above. In addition, the opening of the graphite crucible inside the arc heating chamber is relatively large. As a result, the generated magnesium hydride powder is not adequately protected during the gas flow in the arc heating chamber. Some of the powder may drift onto the inner wall of the arc heating device and the exhaust duct, thereby increasing the difficulty of the collection operation.

[0005] To this end, we propose a high-pressure container for hydride preparation to solve the above technical problems. Utility Model Content

[0006] In view of this, the present invention proposes a high-pressure container for hydride preparation, and its specific technical solution is as follows:

[0007] A high-pressure container for preparing hydrides, comprising a high-pressure tank body, the upper portion of which is an open structure and is equipped with a sealing cover at the opening; a removable loading tray is placed in the lower portion of the inner cavity of the high-pressure tank body; the top of the loading tray is provided with a plurality of small chambers that can be adapted to insert and insert small graphite crucibles; a high-temperature resistant metal sheet is fixed to the bottom surface of the loading tray at a position corresponding to each of the small chambers, and the high-temperature resistant metal sheet can support the graphite crucible located in the small chamber; an air inlet is provided on the upper portion of the outer wall of the high-pressure tank body, and the air inlet is externally connected to an air supply assembly; the sealing cover is provided with an exhaust valve connected to the inner cavity of the high-pressure tank body, and a heating assembly is provided on the outside of the high-pressure tank body.

[0008] Preferably, the loading tray is circular and has a detachable hook installed on the top.

[0009] Preferably, two hooks are provided and are symmetrically mounted on both sides of the top of the loading tray.

[0010] Preferably, the lower end of the hook is threadedly connected to the top of the loading tray.

[0011] Preferably, a flexible baffle is integrally provided on the bottom surface of the loading tray, and the high-temperature resistant metal sheet is placed above the baffle.

[0012] Preferably, the high-pressure tank body and the sealing cover are connected using a serrated flange gasket.

[0013] Preferably, the gas supply assembly includes a compressor arranged outside the high-pressure tank body, the exhaust end of the compressor is connected to the air inlet, and the intake end of the compressor is connected to the hydrogen tank and the argon tank respectively.

[0014] Preferably, the upper portion of the outer side wall of the high-pressure tank body is connected to an air intake pipe inclined upward and away from the high-pressure tank body, and the upper end of the air intake pipe is the air inlet.

[0015] Preferably, the sealing cover is further provided with a pressure gauge and a temperature sensor which are in communication with the inner cavity of the high-pressure tank.

[0016] Preferably, the heating assembly includes a heating furnace fixed to the lower part of the high-pressure tank body and a furnace bottom temperature sensor, and the temperature sensor is arranged at the center of the bottom of the heating furnace and contacts the bottom center of the high-pressure tank body.

[0017] Compared with the prior art, the high-pressure container for hydride preparation of the utility model has the following beneficial effects:

[0018] 1. The utility model sets the air inlet on the upper part of the outer wall of the high-pressure tank and provides an exhaust valve on the sealing cover, so that the gas injected into the high-pressure tank flows above the crucible, which helps to isolate the negative pressure airflow around the exhaust valve from the magnesium hydride powder, thereby reducing the flying loss of the magnesium hydride powder.

[0019] 2. The utility model also replaces a large crucible adapted to the inner cavity of the high-pressure tank with several small crucibles placed on the loading tray. By reducing the size of the crucible and narrowing the opening of the crucible, the magnesium hydride powder is not easy to float out of the crucible.

[0020] 3. The utility model sets a high-temperature resistant metal sheet at the bottom of each small chamber on the loading tray. By pushing the high-temperature resistant metal sheet upward, the crucible placed in the small chamber can be easily taken out.

[0021] 4. The loading tray of the present invention can be extracted through a hook provided thereon, and the hook can be disassembled from the loading tray to avoid affecting the reaction process and the collection of magnesium hydride powder in the crucible after the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0023] Figure 1 This is a schematic diagram of the overall structure of a high-pressure container for hydride preparation according to the present invention.

[0024] Figure 2 This is a structural schematic diagram of a gas supply assembly connected to a high-pressure container for hydride preparation according to the present invention.

[0025] Figure 3 This is a schematic diagram of the internal structure of the medium and high pressure tank body of the utility model.

[0026] Figure 4 This is a structural diagram of the loading tray in the utility model.

[0027] In the figure: 1-high-pressure tank, 2-sealing cover, 3-loading tray, 4-graphite crucible, 5-small chamber, 6-air inlet, 7-gas supply assembly, 8-exhaust valve, 9-hook, 10-compressor, 11-hydrogen tank, 12-argon tank, 13-inlet pipe, 14-pressure gauge, 15-temperature sensor. DETAILED DESCRIPTION

[0028] The following describes in detail embodiments of the present invention, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to explain the present invention, and should not be construed as limiting the present invention.

[0029] In the description of the present invention, it should be understood that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they should not be understood as limitations on the present invention.

[0030] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature specified as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of this utility model, "plurality" means two or more, unless otherwise specifically defined.

[0031] Example:

[0032] See Figures 1-4 The present embodiment provides a high-pressure container for preparing hydrides, comprising a high-pressure tank body 1; the upper portion of the high-pressure tank body 1 is an open structure and a sealing cover 2 is installed at the opening; a removable loading tray 3 is placed at the lower portion of the inner cavity of the high-pressure tank body 1; the top of the loading tray 3 is provided with a plurality of small chambers 5 that can be adapted to insert and insert small graphite crucibles 4; the graphite crucibles 4 are preferably in the shape of circular grooves; high-temperature resistant metal sheets are fixed at positions corresponding to each small chamber 5 on the bottom surface of the loading tray; the high-temperature resistant metal sheets can support the graphite crucibles 4 located in the small chambers 5; an air inlet 6 is provided at the upper portion of the outer wall of the high-pressure tank body 1, and the air inlet 6 is externally connected to a gas supply component 7; an exhaust valve 8 communicating with the inner cavity of the high-pressure tank body 1 is provided on the sealing cover 2, and a heating component is provided on the outside of the high-pressure tank body 1.

[0033] In this embodiment, the volume of the high-pressure tank 1 needs to be no less than 100 ml, which is sufficient to accommodate containers such as the loading tray 3 and a smaller graphite crucible 4 .

[0034] The present embodiment provides a high-pressure container for preparing hydrides. Before use, the high-pressure tank body 1, the loading tray 3 and the graphite crucible 4 must all be cleaned. When in use, a fixed amount of magnesium metal powder is first placed in the graphite crucible 4 and flattened. After flattening, the thinner magnesium metal powder can increase the contact area with hydrogen. Then, the graphite crucible 4 is placed into the high-pressure tank body 1 from the upper opening and seated on the loading tray 3. The upper opening of the high-pressure tank body 1 is closed, the exhaust valve 8 is opened, and the gas supply component 7 is started to first introduce excess argon gas to squeeze out the air in the high-pressure tank body 1, and then a fixed amount of hydrogen is introduced to empty the argon. At this time, the exhaust valve 8 and the gas supply component 7 are synchronously closed. After the internal pressure of the high-pressure tank body 1 rises to 2-5 MPa, the heating component is started. The temperature of the magnesium metal powder inside the high-pressure tank body is heated in a hydrogen environment to >350°C, so that part of the hydrogen Under high temperature and high pressure environment, it reacts with magnesium metal powder to form magnesium hydride powder. Finally, the heating component is controlled to stop heating and slowly cool down, the exhaust valve 8 and the air supply component 7 are opened, and argon is introduced into the high-pressure tank body 1 again to squeeze out the hydrogen and discharge it along the exhaust valve 8. This process helps to isolate the negative pressure airflow around the exhaust valve 8 from the magnesium hydride powder, thereby reducing the flying loss of the magnesium hydride powder; the above-emitted waste gas is collected by the drainage method. After the pressure relief operation is completed, the high-pressure tank body 1 is cooled to room temperature, the upper opening of the high-pressure tank body is opened, and the loading tray 3 is lifted and removed with the help of the detachable hook 9, and the high-temperature resistant metal sheet at the lower end of each small chamber 5 is pushed from the bottom of the loading tray 3 to eject the graphite crucible 4, which can conveniently remove and collect the magnesium hydride powder in the crucible, and clean the crucible to facilitate subsequent work.

[0035] In a further specific embodiment, the material loading tray 3 is circular and a detachable hook 9 is also installed on the top. Furthermore, two hooks 9 are provided and symmetrically installed on both sides of the material loading tray 3 top.

[0036] In this embodiment, the two symmetrically arranged detachable hooks 9 on the loading tray 3 and the several evenly distributed small chambers 5 on the tray body for placing high-temperature resistant metal sheets can facilitate the stable and horizontal placement of the graphite crucible 4.

[0037] More specifically, the lower end of the hook 9 is threadedly connected to the top of the loading tray 3. By setting the hook 9 as a detachable structure, the hook can be removed during the reaction to prevent it from affecting the reaction process. After the reaction is completed and the loading tray 3 is removed, the hook 9 can also be removed first to facilitate the removal of the crucible and the collection of the magnesium hydride powder in the crucible.

[0038] In a further specific embodiment, a flexible baffle is integrally provided on the bottom surface of the loading tray 3, and a high-temperature resistant metal sheet is placed above the baffle.

[0039] In a further embodiment, the sealing cover 2 is equipped with a turntable. The forward rotation of the turntable can lock the sealing cover 2 at the opening of the high-pressure tank body 1, and the reverse rotation of the turntable can open the sealing cover 2. At the same time, to further ensure the sealing effect, the high-pressure tank body 1 and the sealing cover 2 are connected using a serrated flange gasket.

[0040] In this embodiment, the gas supply assembly 7 includes a compressor 10 arranged on the outside of the high-pressure tank body 1. The compressor 10 can be a DJ series fixed compressor. The exhaust end of the compressor 10 is connected to the air inlet 6, and the intake end of the compressor 10 is connected to the hydrogen tank 11 and the argon tank 12 respectively. A hydrogen control valve is provided on the hydrogen tank 11, and an argon control valve is provided on the argon tank 12. The argon control valve and the hydrogen control valve are used for the passage and blocking of argon and hydrogen respectively.

[0041] By independently opening the hydrogen tank 11 or the argon tank 12, the system can deliver the required gas to the high-pressure vessel. After starting the compressor 10, the gas is pressurized, and the pressure can be adjusted between 2 MPa and 5 MPa. When the hydrogenation reaction is complete, the compressor 10 is turned off and the pressure is gradually released.

[0042] An air storage tank, a pre-filter, a dryer, a post-filter and a precision filter are sequentially connected between the exhaust end of the compressor 10 and the air inlet 6. This technical solution is a prior art and is not shown in the figure.

[0043] The upper portion of the outer wall of the high-pressure tank body 1 is connected to an air intake pipe 13 that is inclined upward and away from the high-pressure tank body, and the upper end of the air intake pipe 13 is an air inlet 6.

[0044] The sealing cover 2 is also provided with a pressure gauge 14 and a temperature sensor 15 which are in communication with the inner cavity of the high-pressure tank 1, so as to realize the visual display of the pressure and temperature parameters during the reaction process, so as to accurately control the reaction process.

[0045] In this embodiment, the heating assembly includes a heating furnace fixed to the lower portion of the high-pressure tank 1 and a furnace bottom temperature sensor (not shown). The temperature sensor is located at the exact center of the furnace bottom and contacts the center of the bottom of the high-pressure tank 1. During heating, the power is turned on, and the heating furnace is set to heat the high-pressure tank 1 at a heating rate. Heat is then transferred to the magnesium metal powder in the graphite crucible 4, concentrating the heat there and achieving the required reaction temperature.

[0046] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. Reference can be made to the common and similar parts between the various embodiments. For the devices disclosed in the embodiments, since they correspond to the methods disclosed in the embodiments, the description is relatively simple, and the relevant parts can be referred to the method description.

[0047] The above description of the disclosed embodiments will enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A high-pressure container for preparing hydrides, characterized in that: It includes a high-pressure tank body, the upper part of the high-pressure tank body is an open structure and a sealing cover is installed at the opening, a removable loading tray is placed at the lower part of the inner cavity of the high-pressure tank body, and the top of the loading tray is provided with a plurality of small chambers that can be adapted to insert small graphite crucibles, and high-temperature resistant metal sheets are fixed at the positions corresponding to each of the small chambers on the bottom surface of the loading tray, and the high-temperature resistant metal sheets can support the graphite crucibles located in the small chambers; an air inlet is provided on the upper part of the outer wall of the high-pressure tank body, and the air inlet is connected to the outside of the air supply component; an exhaust valve connected to the inner cavity of the high-pressure tank body is provided on the sealing cover, and a heating component is provided on the outside of the high-pressure tank body.

2. A high-pressure container for hydride preparation according to claim 1, characterized in that: The loading tray is circular and a detachable hook is installed on the top.

3. A high-pressure container for hydride preparation according to claim 2, characterized in that: There are two hooks, which are symmetrically installed on both sides of the top of the loading tray.

4. A high-pressure container for hydride preparation according to claim 2, characterized in that: The lower end of the hook is threadedly connected to the top of the loading tray.

5. A high-pressure container for hydride preparation according to claim 1, characterized in that: A flexible baffle is integrally provided on the bottom surface of the loading tray, and the high-temperature resistant metal sheet is placed above the baffle.

6. A high-pressure container for hydride preparation according to claim 1, characterized in that: The high-pressure tank body and the sealing cover are connected by a serrated flange gasket.

7. A high-pressure container for hydride preparation according to claim 1, characterized in that: The gas supply assembly includes a compressor arranged outside the high-pressure tank body, the exhaust end of the compressor is connected to the air inlet, and the intake end of the compressor is connected to the hydrogen tank and the argon tank respectively.

8. A high-pressure container for hydride preparation according to claim 1 or 7, characterized in that: The upper portion of the outer side wall of the high-pressure tank body is connected to an air intake pipe which is inclined upward and away from the high-pressure tank body, and the upper end of the air intake pipe is the air inlet.

9. A high-pressure container for hydride preparation according to claim 1, characterized in that: The sealing cover is also provided with a pressure gauge and a temperature sensor which are in communication with the inner cavity of the high-pressure tank.

10. The high-pressure container for preparing hydrides according to claim 1, characterized in that: The heating assembly includes a heating furnace fixed at the lower part of the high-pressure tank body and a furnace bottom temperature sensor. The temperature sensor is arranged at the center of the bottom of the heating furnace and contacts the bottom center of the high-pressure tank body.

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