Large-scale magnesium hydride production device and production process

Abstract

The invention aims to disclose a magnesium hydride large-scale production device and production process, and relates to the technical field of magnesium hydride preparation, the magnesium hydride large-scale production device comprises a magnesium powder buffer tank, a high-temperature and high-pressure hydrogenation reactor, a magnesium hydride buffer tank and a finished product tank; a feeding pipe is arranged between the magnesium powder buffer tank and the high-temperature and high-pressure hydrogenation reactor, and the feeding pipe is provided with a first valve; a double-helix stirring shaft is arranged in the high-temperature and high-pressure hydrogenation reactor, and a second valve is arranged on the discharging pipe; a spiral drill bit is arranged at the bottom of the double-spiral stirring shaft, extends into the discharging pipe and is close to the second valve; the high-temperature and high-pressure hydrogenation reactor is provided with a high-pressure hydrogen inlet, and a plurality of temperature sensors are arranged on the inner wall of the high-temperature and high-pressure hydrogenation reactor. The high-temperature and high-pressure hydrogenation reactor has the technical effects that high-pressure hydrogen is introduced under the condition that the first valve and the second valve are closed, and magnesium hydride is generated in the process that the double-helix stirring shaft rotates reversely to stir magnesium powder; and the second valve is opened, and the double-helix stirring shaft rotates forwards and drives the magnesium hydride powder to fall into the magnesium hydride buffer tank from the discharging pipe.

Description

Technical Field

[0001] The invention relates to the technical field of magnesium hydride preparation, and in particular to a large-scale production device and a production process of magnesium hydride. Background Art

[0002] The storage and transportation of hydrogen presents technical and cost challenges due to its high volatility and low density. Therefore, developing a safe and efficient solid-state storage and transportation technology for hydrogen is crucial to promoting the development of the hydrogen economy. Magnesium hydride, as a raw material with a wide range of sources and easy and safe storage and transportation, has become one of the main materials for solid-state storage of hydrogen. Conventional magnesium hydride synthesis equipment and methods are suitable for small-scale laboratory-level production, but are difficult to achieve industrial mass production.

[0003] In view of this, it is necessary to develop a large-scale production device and production process of magnesium hydride. Summary of the invention

[0004] In order to solve the above technical problems, the purpose of the present invention is to disclose a large-scale production device and production process of magnesium hydride.

[0005] The first object of the present invention is to provide a large-scale production device for magnesium hydride.

[0006] The second object of the present invention is to provide a large-scale production process of magnesium hydride.

[0007] To achieve the above first invention objective, the present invention provides a large-scale production device for magnesium hydride, comprising a magnesium powder buffer tank, a high-temperature and high-pressure hydrogenation reactor, a magnesium hydride buffer tank and a finished product tank, wherein the high-temperature and high-pressure hydrogenation reactor is placed vertically; A feed pipe is arranged between the magnesium powder buffer tank and the high-temperature and high-pressure hydrogenation reactor, and the feed pipe is provided with a first valve; A double-helix stirring shaft is arranged in the high-temperature and high-pressure hydrogenation reactor. When the double-helix stirring shaft rotates forward, the magnesium hydride powder is driven to enter the magnesium hydride buffer tank through the discharge pipe. When the double-helix stirring shaft rotates reversely, the magnesium powder and the magnesium hydride powder are driven to turn over and stir. The discharge pipe is provided with a second valve; A spiral drill bit is arranged at the bottom of the double-helix stirring shaft, and the spiral drill bit extends into the discharge pipe and approaches the second valve; and / or, the discharge pipe is in a bell-mouth shape, and a vibrator is arranged on the outer wall of the discharge pipe; The magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft and the forward thrust of the spiral drill bit, and falls from the discharge pipe into the magnesium hydride buffer tank; The high-temperature and high-pressure hydrogenation reactor is provided with a high-pressure hydrogen inlet, and the gas pressure in the high-temperature and high-pressure hydrogenation reactor is maintained at 2MPa-10MPa; A plurality of temperature sensors are arranged on the inner wall of the high-temperature and high-pressure hydrogenation reactor, and the plurality of temperature sensors are distributed at the upper part, the middle part and the bottom part of the inner wall of the high-temperature and high-pressure hydrogenation reactor.

[0008] Preferably, the magnesium powder buffer tank is provided with a first argon gas inlet and a first replacement exhaust port; The high-temperature and high-pressure hydrogenation reactor is provided with a second argon inlet and a second replacement exhaust port.

[0009] Preferably, when high-pressure hydrogen is introduced into the high-temperature and high-pressure hydrogenation reactor, the first valve and the second valve are closed.

[0010] Preferably, a safety valve and a filter with a filtration accuracy of less than 50 μm are arranged on the top of the high-temperature and high-pressure hydrogenation reactor.

[0011] Preferably, a first jacket is disposed on the outer wall of the high-temperature and high-pressure hydrogenation reactor, a spirally wound first heat transfer oil pipeline is disposed in the first jacket, and a first hot oil system or a first cold oil system introduces heat transfer oil into the first heat transfer oil pipeline; The heating rate and cooling rate of the heat transfer oil are both 50°C / h-150°C / h.

[0012] Preferably, a second jacket is provided on the outer wall of the magnesium hydride cache tank, a spirally wound second heat transfer oil pipeline is provided in the second jacket, and a second cooling oil system introduces heat transfer oil at 30°C-60°C into the second heat transfer oil pipeline.

[0013] Preferably, a magnetic drive is arranged on the top of the high-temperature and high-pressure hydrogenation reactor, and the magnetic drive drives the double-helix stirring shaft to rotate without contact, and the rotation speed of the double-helix stirring shaft is 5rpm-30rpm.

[0014] Preferably, when any of the temperature sensors issues an over-temperature warning, the introduction of hydrogen into the high-temperature and high-pressure hydrogenation reactor is stopped, the first cooling oil system is started and heat transfer oil is transported to the first heat transfer oil pipeline, and argon is introduced into the high-temperature and high-pressure hydrogenation reactor for cooling.

[0015] Preferably, the magnetic drive is provided with a current monitoring unit. If the working current of the magnetic drive monitored by the current monitoring unit reaches 80% of the threshold value, the introduction of hydrogen into the high-temperature and high-pressure hydrogenation reactor is stopped, the first cooling oil system is started and heat transfer oil is transported to the first heat transfer oil pipeline, and argon is introduced into the high-temperature and high-pressure hydrogenation reactor for cooling.

[0016] Based on the same inventive principle, in order to achieve the above second invention object, the present invention provides a large-scale production process of magnesium hydride, comprising the following steps: Adding magnesium powder into a magnesium powder buffer tank in an argon atmosphere; The gas in the high-temperature and high-pressure hydrogenation reactor is replaced with argon, magnesium powder is injected into the high-temperature and high-pressure hydrogenation reactor through a pressure difference, the first valve and the second valve are closed, the double-helix stirring shaft is reversed and high-pressure hydrogen is injected, so that the gas pressure in the high-temperature and high-pressure hydrogenation reactor is maintained at 2MPa-10MPa, and magnesium hydride is generated; When the second valve is opened, the magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft and the forward thrust of the spiral drill bit, and falls from the discharge pipe into the magnesium hydride buffer tank; Cool the magnesium hydride in the magnesium hydride buffer tank to 30°C-60°C; The magnesium hydride in the magnesium hydride buffer tank is transported to the finished product tank.

[0017] Compared with the prior art, the technical effects of the present invention are as follows: (1) A double-helix stirring shaft is arranged in a high-temperature and high-pressure hydrogenation reactor. High-pressure hydrogen is introduced when the first valve and the second valve are closed. Magnesium hydride is generated in the process of the double-helix stirring shaft rotating in a reverse direction to stir the magnesium powder. When the second valve is opened, the double-helix stirring shaft rotates forward and drives the magnesium hydride powder to fall from the discharge pipe into the magnesium hydride buffer tank. The forward and reverse rotation of the double-helix stirring shaft achieves stirring so that the magnesium powder is fully in contact with the hydrogen, and the discharge of the magnesium hydride is accelerated.

[0018] (2) A spiral drill bit is provided at the bottom of the double-helix stirring shaft. When the spiral drill bit rotates forward, it drives the magnesium hydride powder to fall from the discharge pipe into the magnesium hydride buffer tank. When the spiral drill bit rotates reversely, it loosens the magnesium hydride adhered to the inner wall of the discharge pipe to prevent the magnesium hydride from agglomerating. Alternatively, the discharge pipe is designed to be a trumpet-shaped with a small inlet and a large outlet, which can also prevent the magnesium hydride from agglomerating on the inner wall of the discharge pipe. In order to further prevent the residual magnesium hydride on the inner wall of the discharge pipe from affecting its discharge, a vibrator is provided on the outer wall of the discharge pipe, and the residual magnesium hydride on the inner wall of the discharge pipe is shaken off by the vibration of the vibrator.

[0019] (3) When magnesium hydride powder is discharged, it is affected by the pressure difference, gravity, the positive rotation driving force of the double-helix stirring shaft and the positive rotation driving force of the spiral drill bit, and the discharge speed is fast.

[0020] (4) A plurality of temperature sensors are arranged on the inner wall of the high-temperature and high-pressure hydrogenation reactor, and the plurality of temperature sensors are used to monitor the temperature of the upper, middle and bottom parts of the inner wall of the high-temperature and high-pressure hydrogenation reactor. When any temperature exceeds a threshold value, the hydrogenation reaction is stopped to avoid sintering of magnesium hydride due to excessively high temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0022] Figure 1 It is a schematic diagram of the working principle of the large-scale production device of magnesium hydride in Example 1 of the present invention.

[0023] Figure 2 It is a schematic diagram of the working principle of the large-scale production device of magnesium hydride in Example 2 of the present invention.

[0024] Figure 3 The present invention is a flow chart of the large-scale production process of magnesium hydride.

[0025] Among them, 1. magnesium powder buffer tank; 11. feed pipe; 12. first valve; 13. first argon inlet; 14. first displacement exhaust port; 2. high temperature and high pressure hydrogenation reactor; 21. double helical stirring shaft; 22. high pressure hydrogen inlet; 23. temperature sensor; 24. second argon inlet; 25. second displacement exhaust port; 26. first hot oil system; 27. first cold oil system; 28. magnetic drive; 29. ​​first jacket; 3. magnesium hydride buffer tank; 31. conical part; 32. second cold oil system; 33. second jacket; 34. third argon inlet; 35. third displacement exhaust port; 4. finished product tank; 5. discharge pipe; 51. second valve; 6. spiral drill bit; 7. safety valve; 71. filter. DETAILED DESCRIPTION

[0026] The present invention is described in detail below in conjunction with the various embodiments shown in the accompanying drawings, but it should be noted that these embodiments are not limitations of the present invention, and any equivalent transformations or substitutions in functions, methods, or structures made by ordinary technicians in the field based on these embodiments are all within the scope of protection of the present invention.

[0027] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0028] Embodiment 1, reference Figure 1 As shown, this embodiment discloses a specific implementation method of a large-scale production device for magnesium hydride (hereinafter referred to as "production device").

[0029] Magnesium hydride large-scale production equipment, see Figure 1 As shown, it includes a magnesium powder buffer tank 1, a high-temperature and high-pressure hydrogenation reactor 2, a magnesium hydride buffer tank 3 and a finished product tank 4, the high-temperature and high-pressure hydrogenation reactor 2 is placed vertically, and the temperature in the high-temperature and high-pressure hydrogenation reactor 2 is 180°C-400°C, preferably 280°C; a feed pipe 11 is arranged between the magnesium powder buffer tank 1 and the high-temperature and high-pressure hydrogenation reactor 2, and the feed pipe 11 is provided with a first valve 12; a double-helix stirring shaft 21 is arranged in the high-temperature and high-pressure hydrogenation reactor 2, and the double-helix stirring shaft 21 drives the magnesium hydride powder to pass through the outlet when the double-helix stirring shaft 21 rotates forward The material pipe 5 enters the magnesium hydride buffer tank 3, and the double-helix stirring shaft 21 drives the magnesium powder and the magnesium hydride powder to turn over and stir when it is reversed. The discharge pipe 5 is provided with a second valve 51. The bottom of the magnesium hydride buffer tank 3 and the finished product tank 4 are both tapered portions 31 with a cone angle of 30°-37°. The purpose of this design is to prevent the accumulation of magnesium hydride; a spiral drill bit 6 is provided at the bottom of the double-helix stirring shaft 2, and the spiral drill bit 6 extends into the discharge pipe 5 and approaches the second valve 51. When the spiral drill bit 6 rotates forward, it drives the magnesium hydride powder to fall from the discharge pipe 5 into the magnesium hydride buffer tank 3. The magnesium hydride buffer tank 3, the spiral drill bit 6 loosens the magnesium hydride adhered to the inner wall of the discharge pipe 5 when reversing to prevent the magnesium hydride from agglomerating. If necessary, a vibrator is set on the outer wall of the discharge pipe, and the magnesium hydride powder remaining on the inner wall of the discharge pipe 5 can be shaken off by the vibrator; the magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft 2 and the forward thrust of the spiral drill bit 6, and falls from the discharge pipe 5 into the magnesium hydride buffer tank 3; the high-temperature and high-pressure hydrogenation reactor 2 is provided with a high-pressure hydrogen inlet 22, and the gas in the high-temperature and high-pressure hydrogenation reactor 2 The pressure is maintained at 2MPa-10MPa, such as 3MPa, 5MPa, 7MPa, 9MPa, etc.; a plurality of temperature sensors 23 are arranged on the inner wall of the high-temperature and high-pressure hydrogenation reactor 2, and the plurality of temperature sensors 23 are distributed at the upper part, the middle part and the bottom part of the inner wall of the high-temperature and high-pressure hydrogenation reactor 2. The plurality of temperature sensors 23 are used to monitor the temperature of the upper part, the middle part and the bottom part of the inner wall of the high-temperature and high-pressure hydrogenation reactor 1. When any temperature exceeds the threshold value, the hydrogenation reaction is stopped to avoid sintering of magnesium hydride due to excessively high temperature.

[0030] Specifically, see Figure 1The magnesium powder buffer tank 1 is provided with a first argon inlet 13 and a first replacement exhaust port 14. Before magnesium powder is put into the magnesium powder buffer tank 1, argon is first injected through the first argon inlet 13, and air, water vapor, etc. are discharged through the first replacement exhaust port 14, so that the magnesium powder buffer tank 1 is filled with an inert environment of argon. The magnesium powder buffer tank 1 is provided with an online moisture monitor, an online oxygen monitor and an online hydrogen monitoring instrument. After magnesium powder is stored in the magnesium powder buffer tank 1, the moisture content is less than 5000ppm, the oxygen content is less than 5000ppm, and the hydrogen content is less than 5000ppm; the high-temperature and high-pressure hydrogenation reactor 2 is provided with a second argon inlet 24 and a second replacement exhaust port 25. Before magnesium powder is put into the high-temperature and high-pressure hydrogenation reactor 2, argon is first injected through the second argon inlet 24, and air, water vapor, etc. are discharged through the second replacement exhaust port 25, so that the high-temperature and high-pressure hydrogenation reactor 2 is filled with an inert environment of argon.

[0031] The warm and high pressure hydrogenation reactor 2 of the present embodiment is placed vertically, that is, placed vertically, so that the gravity of magnesium hydride can be fully utilized when the material is discharged. In addition, because the inner diameter of the discharge pipe 5 is only 50mm-100mm, when the magnesium powder and hydrogen are fully stirred and hydrogenated, it is difficult to discharge the material due to the stacking angle of the magnesium hydride powder at the moment when the second valve 51 is opened. For this reason, the present embodiment adopts the pressure difference, gravity, the forward thrust of the double-helix stirring shaft 2 and the forward thrust of the spiral drill bit 6 to synchronously promote the discharge of magnesium hydride; during the discharge process, if magnesium hydride is attached to the inner wall of the discharge pipe 5, sintering will occur in a high temperature environment, resulting in poor discharge, which will seriously affect the normal production. The material can be shaken by the vibrator on the outer wall of the discharge pipe 5, and the subsequent reversal of the spiral drill bit 6 can also play a role in loosening the magnesium hydride attached to the inner wall of the discharge pipe 5. Through this embodiment, the discharge of the thin-diameter discharge pipe 5 is guaranteed to be smoothly discharged and the magnesium hydride is effectively prevented from accumulating on the inner wall of the discharge pipe 5.

[0032] See also Figure 1A magnetic drive 28 is arranged on the top of the high-temperature and high-pressure hydrogenation reactor 2, and the magnetic drive 28 drives the double-helix stirring shaft 21 to rotate without contact. The rotation speed of the double-helix stirring shaft 21 is 5rpm-30rpm. There is no contact between the magnetic drive 28 and the double-helix stirring shaft 21, that is, there is no power transmission shaft, which reduces the risk of leakage of the power transmission shaft due to improper sealing; when high-pressure hydrogen is injected into the high-temperature and high-pressure hydrogenation reactor 2, in order to prevent hydrogen from entering the magnesium powder buffer tank 1 and the magnesium hydride buffer tank 3, the first valve 12 and the second valve 51 are closed. When the first valve 12 and the second valve 51 are closed, the double-helix stirring shaft 21 continues to reverse, and the magnesium powder and magnesium hydride particles are continuously fed The first heat transfer oil pipeline is provided in the first jacket 29, and the first hot oil system 26 or the first cold oil system 27 introduces heat transfer oil into the first heat transfer oil pipeline. The heat transfer oil enters from the bottom of the first heat transfer oil pipeline and flows back from the top. The spirally wound first heat transfer oil pipeline can ensure the reaction temperature in the high temperature and high pressure hydrogenation reactor 2. In case of emergency, cold heat transfer oil can also be introduced into the first heat transfer oil pipeline to cool the high temperature and high pressure hydrogenation reactor 2. The heating rate and cooling rate of the heat transfer oil are both 50℃ / h-150℃ / h, so that a faster heating or cooling speed can be achieved.

[0033] See also Figure 1 A safety valve 7 and a filter 71 with a filtration accuracy of less than 50 μm are arranged on the top of the high-temperature and high-pressure hydrogenation reactor 2. When the gas pressure in the high-temperature and high-pressure hydrogenation reactor 2 exceeds the threshold value, the safety valve 7 is opened and the gas is released to reduce the pressure. The gas released by the safety valve 7 contains magnesium powder or magnesium hydride powder. The filter 71 can intercept the magnesium powder or magnesium hydride powder to prevent the magnesium powder or magnesium hydride powder from escaping into the atmosphere.

[0034] During the reaction of magnesium powder and hydrogen, if the temperature of a certain part of the inner wall of the high-temperature and high-pressure hydrogenation reactor 2 is too high, the magnesium hydride will be sintered into a block, which will affect the normal synthesis of magnesium hydride. The high-temperature and high-pressure hydrogenation reactor 2 needs to be opened for processing. The high-temperature and high-pressure hydrogenation reactor 2 is full of hydrogen, magnesium powder and magnesium hydride. Opening the high-temperature and high-pressure hydrogenation reactor 2 is an extremely risky and costly action. Figure 1In order to prevent the generated magnesium hydride from being sintered into a block, when any of the temperature sensors 23 issues an over-temperature warning, the following measures are taken to cool down the temperature: stop introducing hydrogen into the high-temperature and high-pressure hydrogenation reactor 2, stop heating the heat transfer oil in the first hot oil system 26, start the first cold oil system 27 and transport the heat transfer oil to the first heat transfer oil pipeline, so that the heat transfer oil is cooled at a rate of 50°C / h-150°C / h. At the same time, argon is introduced into the high-temperature and high-pressure hydrogenation reactor 2 for cooling. The argon temperature can be -25°C-25°C. Through the above measures, the high-temperature and high-pressure hydrogenation reactor 2 can be cooled, thereby preventing the magnesium hydride from sintering into a block.

[0035] See also Figure 1 The magnetic drive 28 is provided with a current monitoring unit. If the working current of the magnetic drive 28 monitored by the current monitoring unit reaches 80% of the threshold value and lasts for more than 10s, it means that the stirring of the double-helix stirring shaft 21 is resisted. The source of the resistance may be that there is too much magnesium powder and the stirring cannot be performed, or that magnesium hydride has been sintered into a block in the high-temperature and high-pressure hydrogenation reactor 2, which increases the stirring resistance of the double-helix stirring shaft 21. If the working current of the magnetic drive 28 is too large, the following measures are taken to cool down: stop introducing hydrogen into the high-temperature and high-pressure hydrogenation reactor 2, stop heating the heat transfer oil in the first hot oil system 26, start the first cold oil system 27 and transport the heat transfer oil to the first heat transfer oil pipeline, so that the heat transfer oil is cooled at a rate of 50°C / h-150°C / h. At the same time, introduce argon gas into the high-temperature and high-pressure hydrogenation reactor 2 for cooling. The temperature of the argon gas may be -25°C-25°C. Through the above measures, the high-temperature and high-pressure hydrogenation reactor 2 can be cooled, thereby preventing magnesium hydride from sintering into a block.

[0036] See also Figure 1 A second jacket 33 is provided on the outer wall of the magnesium hydride cache tank 3, and a spirally coiled second heat transfer oil pipeline is provided in the second jacket 33. A second cold oil system 32 introduces 30°C-60°C heat transfer oil into the second heat transfer oil pipeline. The heat transfer oil enters from the bottom of the second heat transfer oil pipeline and flows back from the top. The spirally coiled second heat transfer oil pipeline can cool the magnesium hydride powder to 30°C-60°C; the magnesium hydride cache tank 3 is also provided with a third argon inlet 34 and a third replacement exhaust port 35. Before magnesium hydride is placed in the magnesium hydride cache tank 3, argon is first injected through the third argon inlet 34, and air, water vapor, etc. are discharged through the third replacement exhaust port 35, so that the magnesium hydride cache tank 3 is filled with an inert environment of argon.

[0037] See also Figure 1When the magnesium powder buffer tank 1 transports magnesium powder to the high-temperature and high-pressure hydrogenation reactor 2, in order to speed up the falling speed of the magnesium powder, high-pressure argon gas can be injected through the first argon gas inlet 13 to quickly transport the magnesium powder by pressure difference and gravity; when the high-temperature and high-pressure hydrogenation reactor 2 discharges material to the magnesium hydride buffer tank 3, in order to speed up the falling speed of the magnesium powder, high-pressure argon gas can be injected through the second argon gas inlet 24 to quickly transport the magnesium hydride powder by pressure difference and gravity.

[0038] Embodiment 2, reference Figure 2 As shown, this embodiment discloses a specific implementation method of a large-scale production device for magnesium hydride (hereinafter referred to as "production device").

[0039] Magnesium hydride large-scale production equipment, see Figure 2 As shown, the difference from Example 1 is that the discharge pipe 5 of Example 2 is a trumpet-shaped one with a small inlet and a large outlet, which can prevent magnesium hydride from agglomerating on the inner wall of the discharge pipe 5; in order to further prevent the residual magnesium hydride on the inner wall of the discharge pipe 5 from affecting its discharge, a vibrator is arranged on the outer wall of the discharge pipe 5, and the magnesium hydride remaining on the inner wall of the discharge pipe is shaken off by the vibration of the vibrator. On the basis that the discharge pipe 5 is a trumpet-shaped one with a small inlet and a large outlet, a spiral drill bit 6 is arranged at the bottom of the double-helix stirring shaft 2, and the spiral drill bit 6 extends into the discharge pipe 5 and approaches the second valve 51. When the spiral drill bit 6 is in forward rotation, it drives the magnesium hydride powder to fall from the discharge pipe 5 into the magnesium hydride buffer tank 3, and when the spiral drill bit 6 is in reverse rotation, it loosens the magnesium hydride adhering to the inner wall of the discharge pipe 5 to prevent the magnesium hydride from agglomerating.

[0040] The large-scale production device for magnesium hydride disclosed in Example 2 is similar to that in Example 1, and please refer to Example 1, which will not be described in detail here.

[0041] Embodiment 3, reference Figures 1 to 3 As shown, this embodiment discloses a specific implementation method of a large-scale production process of magnesium hydride.

[0042] For large-scale production process of magnesium hydride, see Figures 1 to 3 As shown, the following steps are included: Step S1: adding magnesium powder into the magnesium powder buffer tank 1 in an argon atmosphere; specifically, before putting the magnesium powder into the magnesium powder buffer tank 1, first inject argon gas through the first argon gas inlet 13, and discharge the air, water vapor, etc. through the first displacement exhaust port 14, so that the magnesium powder buffer tank 1 is filled with an inert environment of argon gas to prevent the magnesium powder from contacting oxygen and moisture; Step S2: replacing the gas in the high-temperature and high-pressure hydrogenation reactor 2 with argon, injecting magnesium powder into the high-temperature and high-pressure hydrogenation reactor 2 through a pressure difference, closing the first valve 12 and the second valve 51, reversing the double-helix stirring shaft 21 and injecting high-pressure hydrogen, so that the gas pressure in the high-temperature and high-pressure hydrogenation reactor 2 is maintained at 2MPa-10MPa, and magnesium hydride is generated; specifically, the first valve 12 is located at the inlet pipe 11 of the high-temperature and high-pressure hydrogenation reactor 2, and the second valve 51 is located at the outlet pipe 5 of the high-temperature and high-pressure hydrogenation reactor 2; the high-temperature and high-pressure hydrogenation reactor 2 is injected with magnesium powder of up to 50% of its volume, and the hydrogen and the magnesium powder are fully contacted during the reverse stirring of the double-helix stirring shaft 21 to generate magnesium hydride powder; Step S3: Open the second valve 51, and the magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft 21, and the forward thrust of the spiral drill bit 6, and falls from the discharge pipe into the magnesium hydride buffer tank; specifically, after the magnesium powder is fully hydrogenated, open the second valve 51, and inject high-pressure argon gas through the second argon gas inlet 24, so that the gas pressure in the high-temperature and high-pressure hydrogenation reactor 2 is temporarily increased to be at a positive pressure, and the double-helix stirring shaft 21 and the spiral drill bit 6 are changed to forward rotation, so that the magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft 21, and the forward thrust of the spiral drill bit 6, and is discharged quickly; Step S4: Cooling the magnesium hydride in the magnesium hydride cache tank to 30°C-60°C; specifically, a second jacket is provided on the outer wall of the magnesium hydride cache tank 3, a spirally wound second heat transfer oil pipeline is provided in the second jacket, and a second cold oil system introduces heat transfer oil at 30°C-60°C into the second heat transfer oil pipeline, and the heat transfer oil enters from the bottom of the second heat transfer oil pipeline and refluxes from the top. The spirally wound second heat transfer oil pipeline can cool the magnesium hydride powder to 30°C-60°C.

[0043] Step S5: The magnesium hydride in the magnesium hydride buffer tank is transported to the finished product tank.

[0044] The large-scale production process of magnesium hydride disclosed in Example 3 adopts the large-scale production device of magnesium hydride described in Example 1 or Example 2. For the same points as Example 1 or Example 2, please refer to Example 1 or Example 2, and no further details will be given here.

Claims

1. A large-scale production device for magnesium hydride, characterized in that: It includes a magnesium powder buffer tank, a high-temperature and high-pressure hydrogenation reactor, a magnesium hydride buffer tank and a finished product tank, wherein the high-temperature and high-pressure hydrogenation reactor is placed vertically; A feed pipe is arranged between the magnesium powder buffer tank and the high-temperature and high-pressure hydrogenation reactor, and the feed pipe is provided with a first valve; A double-helix stirring shaft is arranged in the high-temperature and high-pressure hydrogenation reactor. When the double-helix stirring shaft rotates forward, the magnesium hydride powder is driven to enter the magnesium hydride buffer tank through the discharge pipe. When the double-helix stirring shaft rotates reversely, the magnesium powder and the magnesium hydride powder are driven to turn over and stir. The discharge pipe is provided with a second valve; A spiral drill bit is arranged at the bottom of the double-helix stirring shaft, and the spiral drill bit extends into the discharge pipe and approaches the second valve; and / or, the discharge pipe is in a bell-mouth shape, and a vibrator is arranged on the outer wall of the discharge pipe; The magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft and the forward thrust of the spiral drill bit, and falls from the discharge pipe into the magnesium hydride buffer tank; The high-temperature and high-pressure hydrogenation reactor is provided with a high-pressure hydrogen inlet, and the gas pressure in the high-temperature and high-pressure hydrogenation reactor is maintained at 2MPa-10MPa; A plurality of temperature sensors are arranged on the inner wall of the high-temperature and high-pressure hydrogenation reactor, and the plurality of temperature sensors are distributed at the upper part, the middle part and the bottom part of the inner wall of the high-temperature and high-pressure hydrogenation reactor.

2. The magnesium hydride large-scale production device according to claim 1, characterized in that: The magnesium powder buffer tank is provided with a first argon gas inlet and a first replacement exhaust port; The high-temperature and high-pressure hydrogenation reactor is provided with a second argon inlet and a second replacement exhaust port.

3. The magnesium hydride large-scale production device according to claim 1, characterized in that: When high-pressure hydrogen is introduced into the high-temperature and high-pressure hydrogenation reactor, the first valve and the second valve are closed.

4. The large-scale production device for magnesium hydride according to claim 3, characterized in that: A safety valve and a filter with a filtration accuracy of less than 50 μm are arranged on the top of the high-temperature and high-pressure hydrogenation reactor.

5. The large-scale production device for magnesium hydride according to any one of claims 1 to 4, characterized in that: A first jacket is disposed on the outer wall of the high-temperature and high-pressure hydrogenation reactor, a first spirally wound heat transfer oil pipeline is disposed in the first jacket, and a first hot oil system or a first cold oil system introduces heat transfer oil into the first heat transfer oil pipeline; The heating rate and cooling rate of the heat transfer oil are both 50°C / h-150°C / h.

6. The large-scale production device for magnesium hydride according to claim 5, characterized in that: A second jacket is provided on the outer wall of the magnesium hydride buffer tank, a spirally wound second heat transfer oil pipeline is provided in the second jacket, and a second cold oil system introduces heat transfer oil at 30° C.-60° C. into the second heat transfer oil pipeline.

7. The large-scale production device for magnesium hydride according to claim 5, characterized in that: A magnetic drive is arranged on the top of the high-temperature and high-pressure hydrogenation reactor, and the magnetic drive drives the double-helix stirring shaft to rotate without contact, and the rotation speed of the double-helix stirring shaft is 5rpm-30rpm.

8. The large-scale production device for magnesium hydride according to claim 7, characterized in that: When any of the temperature sensors issues an over-temperature warning, the introduction of hydrogen into the high-temperature and high-pressure hydrogenation reactor is stopped, the first cooling oil system is started and heat transfer oil is transported to the first heat transfer oil pipeline, and argon is introduced into the high-temperature and high-pressure hydrogenation reactor for cooling.

9. The large-scale production device for magnesium hydride according to claim 7, characterized in that: The magnetic drive is provided with a current monitoring unit. If the working current of the magnetic drive monitored by the current monitoring unit reaches 80% of the threshold value, the introduction of hydrogen into the high-temperature and high-pressure hydrogenation reactor is stopped, the first cooling oil system is started and heat transfer oil is transported to the first heat transfer oil pipeline, and argon is introduced into the high-temperature and high-pressure hydrogenation reactor for cooling.

10. A large-scale production process of magnesium hydride, characterized in that: The following steps are involved: Adding magnesium powder into a magnesium powder buffer tank in an argon atmosphere; The gas in the high-temperature and high-pressure hydrogenation reactor is replaced with argon, magnesium powder is injected into the high-temperature and high-pressure hydrogenation reactor through a pressure difference, the first valve and the second valve are closed, the double-helix stirring shaft is reversed and high-pressure hydrogen is injected, so that the gas pressure in the high-temperature and high-pressure hydrogenation reactor is maintained at 2MPa-10MPa, and magnesium hydride is generated; When the second valve is opened, the magnesium hydride powder is simultaneously subjected to the pressure difference, gravity, the forward thrust of the double-helix stirring shaft and the forward thrust of the spiral drill bit, and falls from the discharge pipe into the magnesium hydride buffer tank; Cool the magnesium hydride in the magnesium hydride buffer tank to 30°C-60°C; The magnesium hydride in the magnesium hydride buffer tank is transported to the finished product tank.

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