Continuous production device and process of magnesium hydride

By designing continuous production equipment and processes of magnesium hydride, and using technical means such as argon gas replacement, heating and spiral thrusters, the problem of industrial mass production in the existing technology is solved, safe and efficient continuous production of magnesium hydride is achieved, and the hydrogen storage density reaches more than 7 wt%.

CN119499988BActive Publication Date: 2025-05-09YULIN ZHONGKE CLEAN ENERGY INNOVATION RES INST +1

Patent Information

Application Number
CN202510098023.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-22
Publication Date
2025-05-09
Estimated Expiration
2045-01-22

AI Technical Summary

Technical Problem

Existing magnesium hydride synthesis equipment and methods are difficult to achieve industrial mass production and cannot meet the needs of hydrogen energy economic development.

Method used

A continuous production device and process of magnesium hydride is designed, including sealed shell, heating inner liner, power assembly, feed assembly, discharge assembly, inert gas replacement assembly and hydrogenation inlet. Through argon replacement, heating, aspirator and steel ball/steel rod, continuous contact and reaction between magnesium powder and hydrogen are achieved to form magnesium hydride.

Benefits of technology

The continuous production of magnesium hydride is achieved, the production process is sealed, safe and reliable, and large-scale production can be achieved. The hydrogen storage density of magnesium hydride is no less than 7wt%.

✦ Generated by Eureka AI based on patent content.

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Abstract

The object of the present invention is to disclose a continuous production device and process of magnesium hydride, which relates to the technical field of magnesium hydride preparation, and comprises a sealed shell, a heating liner, a power assembly, a feed assembly, a discharge assembly, an inert gas replacement assembly and a hydrogenation inlet; the heating liner comprises a side wall, a feed end and a discharge end, a plurality of gas one-way valves are arranged on the side wall, a screw propeller, a plurality of steel balls and / or a plurality of steel rods are arranged in the heating liner, and a filter screen is arranged at the discharge end; a tapered portion and a recovery port are arranged at the bottom of the sealed shell; the feed assembly comprises a feed lock hopper and a feed pipe, and the feed pipe is connected to the feed end; the discharge assembly comprises a discharge pipe and a discharge lock hopper, and the discharge pipe is connected to the discharge end; technical effect: the particle size of the magnesium powder of the present invention is 10μm-300μm, and the particle size of the produced magnesium hydride is 50nm-800nm, which can realize continuous feeding, continuous reaction and continuous discharge, realize large-scale production of magnesium hydride, and the hydrogen storage density of magnesium hydride is not less than 7wt%.
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Description

Technical Field

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

[0002] Hydrogen energy has both energy and material attributes, and hydrogen energy has been incorporated into the national energy strategic deployment. The storage and transportation of hydrogen has technical and cost challenges due to its high volatility and low density. Therefore, the development of a safe and efficient solid-state storage and transportation technology for hydrogen is crucial to promoting the development of the hydrogen energy economy. Magnesium hydride, as a raw material with a wide range of sources and easy to store and transport safely, 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, and it is difficult to achieve industrial large-scale production.

[0003] In view of this, it is necessary to develop a continuous production device and process for 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 continuous production device and process of magnesium hydride.

[0005] The first object of the present invention is to develop a continuous production device for magnesium hydride.

[0006] The second invention object of the present invention is to develop a continuous production process of magnesium hydride.

[0007] To achieve the above first invention objective, the present invention provides a magnesium hydride continuous production device, comprising a sealed housing, a heating liner, a power assembly, a feed assembly, a discharge assembly, an inert gas replacement assembly and a hydrogenation inlet;

[0008] The heating inner container comprises a side wall, an inlet end and an outlet end, a plurality of gas one-way valves are arranged on the side wall, a screw propeller, a plurality of steel balls and / or a plurality of steel rods are arranged in the heating inner container, and a filter screen is arranged on the outlet end;

[0009] A conical portion and a recovery port are provided at the bottom of the sealing shell, and the recovery port is provided at the bottom of the conical portion;

[0010] The feed assembly comprises a feed lock bucket and a feed pipe, and the feed pipe is connected to the feed end;

[0011] The discharging assembly comprises a discharging pipe and a discharging lock bucket, and the discharging pipe is connected to the discharging end;

[0012] The inert gas replacement assembly includes a gas inlet and a gas outlet.

[0013] Preferably, the power assembly includes a motor, a magnetic drive, a power shaft, a driving gear and a passive gear;

[0014] The motor drives the driving gear through the magnetic drive, the driving gear meshes with the passive gear, and the passive gear drives the heating liner to rotate;

[0015] The motor rotates forward and reverse alternately.

[0016] Preferably, the rotation speed of the heating inner tank is 5r / min-25r / min.

[0017] Preferably, the heating temperature of the heating liner is 250°C-450°C.

[0018] Preferably, the diameter of the steel ball is 30 mm-100 mm, and the diameter of the steel rod is 30 mm-100 mm.

[0019] Preferably, the air pressure in the heating liner is 2MPa-4MPa.

[0020] Preferably, the sealed housing is provided with a moisture sensor, an oxygen sensor and an air pressure sensor;

[0021] A temperature sensor is arranged in the heating inner container.

[0022] Preferably, the feed pipe is provided with a first valve group and a second valve group respectively located before and after the feed lock bucket;

[0023] Open the first valve group and close the second valve group, and add magnesium powder into the feed lock hopper;

[0024] Open the second valve group and close the first valve group, and add magnesium powder into the heating inner container;

[0025] The discharge pipe is provided with a third valve group and a fourth valve group respectively located before and after the discharge lock bucket;

[0026] Open the third valve group and close the fourth valve group to allow magnesium hydride to flow from the heating inner tank into the discharge lock hopper;

[0027] The fourth valve group is opened and the third valve group is closed to collect magnesium hydride from the discharge lock hopper.

[0028] Based on the same inventive principle, in order to achieve the above second inventive object, the present invention provides a continuous production process of magnesium hydride, comprising the following steps:

[0029] Step S1: replacing the gas in the sealed outer shell and the heating inner container with argon gas, so that the oxygen content in the heating inner container is less than 4000 ppm and the water content is less than 4000 ppm;

[0030] Step S2: starting heating to make the temperature in the heating inner container reach 250° C.-450° C.;

[0031] Step S3: magnesium powder with a particle size of 10 μm-300 μm flows into the heating inner container from the feed lock hopper;

[0032] Step S4: start the motor and drive the heating inner container to rotate through the magnetic drive, and synchronously drive the screw propeller to rotate, the screw propeller drives the magnesium powder, a plurality of steel balls and / or a plurality of steel rods to rotate together, and hydrogen is injected into the heating inner container during the rotation, and the reaction is carried out for 2h-6h;

[0033] Step S5: Step S4 reacts to form magnesium hydride, wherein the particle size of the magnesium hydride is 50nm-800nm;

[0034] Step S6: The magnesium hydride in step S5 is discharged from the discharge lock hopper.

[0035] Preferably, in step S4, after the hydrogen is injected, the heating power of the heating inner container is reduced so that the temperature in the heating inner container is maintained at 250° C.-450° C.;

[0036] In step S4, the heating inner container rotates forward and reverse alternately;

[0037] In steps S3 and S4, if any data sensed by the moisture sensor and the oxygen sensor is abnormal, the injection of hydrogen and magnesium powder is stopped, the heating power of the heating liner is turned off, and argon is injected for replacement.

[0038] Compared with the prior art, the technical effects of the present invention are as follows:

[0039] (1) The heating liner is surrounded by a sealed outer shell. After the moisture and oxygen in the sealed outer shell and the heating liner are replaced by argon gas, magnesium powder is continuously added and hydrogen is injected. Through the rotation of the heating liner, the magnesium powder and hydrogen are continuously contacted and reacted to form magnesium hydride. The magnesium hydride passes through the filter and enters the discharge lock hopper, realizing the continuous production of magnesium hydride. The production process is sealed, safe and reliable.

[0040] (2) A screw propeller, a plurality of steel balls and / or a plurality of steel rods are arranged in the heating inner container. During the rotation of the heating inner container, the screw propeller can propel the magnesium powder or magnesium hydride forward and stir the magnesium powder or magnesium hydride. Under the combined action of rotational inertia and gravity, the plurality of steel balls and / or the plurality of steel rods continuously fall from the top of the heating inner container, hit the magnesium powder or magnesium hydride in the process of falling, and continuously crush the magnesium powder or magnesium hydride, so that the crushed magnesium powder is more exposed and contacts with hydrogen to react and generate more magnesium hydride.

[0041] (3) After the magnesium powder comes into contact with hydrogen, magnesium hydride is first formed on the outermost layer of the magnesium powder. Due to the coating effect of the magnesium hydride, if it is not crushed again, the coated magnesium powder cannot continue to react with hydrogen further. In order to make as much magnesium powder as possible react with hydrogen, under the action of a screw propeller, a plurality of steel balls and / or a plurality of steel rods, especially because the magnesium hydride coated on the surface of the magnesium powder is brittle, after being crushed by the plurality of steel balls and / or a plurality of steel rods, the magnesium hydride coating layer is destroyed, so that the exposed magnesium powder further reacts with hydrogen, and finally forms magnesium hydride with a hydrogen storage density of not less than 7wt%.

[0042] (4) The particle size of the magnesium powder of the present invention is 10 μm-300 μm, and the particle size of the produced magnesium hydride is 50 nm-800 nm, which can realize continuous feeding, continuous reaction and continuous discharging, and realize large-scale production of magnesium hydride. The hydrogen storage density of magnesium hydride is not less than 7wt%. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] 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.

[0044] Figure 1 It is a schematic diagram of the continuous production device of magnesium hydride of the present invention.

[0045] Figure 2 It is the XRD analysis diagram of magnesium hydride prepared by the present invention.

[0046] Figure 3 It is a test curve of hydrogen storage density of magnesium hydride prepared by the present invention.

[0047] Figure 4 The present invention is a continuous production process flow chart of magnesium hydride.

[0048] Among them, 1. sealed shell; 11. conical part; 12. recovery port; 13. moisture sensor; 14. oxygen sensor; 15. air pressure sensor; 2. heating liner; 21. side wall; 211. gas one-way valve; 22. feed end; 23. discharge end; 24. screw propeller; 25. several steel balls and / or several steel rods; 26. filter; 3. power assembly; 31. motor; 32. magnetic drive; 33. power shaft; 34. driving gear; 35. passive gear; 4. feed assembly; 41. feed lock hopper; 42. feed pipe; 421. first valve group; 422. second valve group; 5. discharge assembly; 51. discharge pipe; 511. third valve group; 512. fourth valve group; 52. discharge lock hopper; 6. inert gas replacement assembly; 61. air inlet; 62. air outlet; 7. hydrogenation inlet. DETAILED DESCRIPTION

[0049] 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.

[0050] 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.

[0051] Example 1

[0052] Ginseng Figure 1 As shown, this embodiment discloses a specific implementation of a continuous production device for magnesium hydride (hereinafter referred to as "production device").

[0053] Continuous production device for magnesium hydride, see Figure 1As shown, it includes a sealed shell 1, a heating liner 2, a power component 3, an inlet component 4, an outlet component 5, an inert gas replacement component 6 and a hydrogenation inlet 7; the heating liner 2 includes a side wall 21, an inlet end 22 and an outlet end 23, and a plurality of gas one-way valves 211 are arranged on the side wall 21, and the gas one-way valve 211 can ensure the entry of hydrogen and can avoid or greatly reduce the magnesium powder or magnesium hydride particles from being thrown out of the gas one-way valve 211, a screw propeller 24, a plurality of steel balls and / or a plurality of steel rods 25 are arranged in the heating liner 2, and a filter screen 2 is arranged on the outlet end 23. 6. The purpose of the filter 26 is to prevent a number of steel balls and / or a number of steel rods 25 from entering the discharge pipe 51 and the discharge lock hopper 52; a conical portion 11 and a recovery port 12 are provided at the bottom of the sealed housing 1, and the recovery port 12 is provided at the bottom of the conical portion 11; the feed assembly 4 includes a feed lock hopper 41 and a feed pipe 42, and the feed pipe 42 is connected to the feed end 22; the discharge assembly 5 includes a discharge pipe 51 and a discharge lock hopper 52, and the discharge pipe 51 is connected to the discharge end 23; the inert gas replacement assembly 6 includes an air inlet 61 and an air outlet 62.

[0054] Specifically, see Figure 1 , the sealed shell 1 is fixedly installed and isolates the heating liner 2 from the outside; before preparing magnesium hydride, the inert gas replacement component 6 is first started to replace and discharge the moisture, oxygen, etc. in the heating liner 2 and the sealed shell 1, so that the oxygen content in the heating liner 2 and the sealed shell 1 is less than 4000ppm, and the moisture content is less than 4000ppm; the inert gas replacement component 6 includes an air inlet 61 and an air outlet 62, and the air inlet 61 and the air outlet 62 are designed according to one of the following two schemes, First, the air inlet 61 is arranged at the feed lock hopper 41, and the air inlet pipeline enters the heating inner container 2 through the feed pipe 42 and the feed end 22, and the air outlet 62 is arranged at the discharge lock hopper 52, and the air outlet pipeline leads to the inert gas collection container through the discharge end 23, the discharge pipe 51 and the air outlet 62; second, the air inlet 61 is arranged at the sealed shell 1, and the inert gas enters the sealed shell 1 and then enters the heating inner container 2, and the air outlet 62 is also arranged at the sealed shell 1, and the air outlet 62 leads to the inert gas collection container. In this embodiment, the inert gas is preferably argon.

[0055] In order to ensure the sealing performance of the sealed shell 1, the following two aspects are used for guarantee. First, the power assembly 3 includes a motor 31, a magnetic drive 32, a power shaft 33, a driving gear 34 and a passive gear 35; the motor 31 drives the driving gear 34 through the magnetic drive 32, the driving gear 34 meshes with the passive gear 35, the passive gear 35 drives the heating liner 2 to rotate, the heating liner 2 is installed on the passive gear 35 through the rotating shaft, and the passive gear 35 drives the heating liner 2 to rotate through the rotating shaft; the motor 31 rotates forward and reverse alternately, and the magnetic drive 32 can realize contactless transmission of torque to prevent leakage from the power shaft 33 of the sealed shell 1; second, the feed pipe 42 is provided with a first valve group 421 and a second valve group 422 respectively located before and after the feed lock bucket 41, and the first valve group 421 and The second valve group 422 includes two valves to ensure airtightness. When the first valve group 421 is opened and the second valve group 422 is closed, magnesium powder is added to the feed lock hopper 41. When the second valve group 422 is opened and the first valve group 421 is closed, magnesium powder is added to the heating inner tank 2, thereby preventing external gas and magnesium powder from entering the heating inner tank 2 together. The discharge pipe 51 is provided with a third valve group 511 and a fourth valve group 512 respectively located before and after the discharge lock hopper 52. When the third valve group 511 is opened and the fourth valve group 512 is closed, magnesium hydride flows from the heating inner tank 2 into the discharge lock hopper 52. When the fourth valve group 512 is opened and the third valve group 511 is closed, magnesium hydride is collected from the discharge lock hopper 52. In the process of collecting magnesium hydride, the heating inner tank 2 is isolated from the outside world, thereby providing a guarantee for continuous production.

[0056] In order to realize the continuous production of magnesium hydride, the production device is also provided with a magnesium powder storage bin and a quantitative screw feeding assembly, wherein the magnesium powder storage bin stores magnesium powder and supplies magnesium powder to the feed lock hopper 41 through the first valve group 421, and the quantitative screw feeding assembly is arranged between the second valve group 422 and the feed end 22, so as to realize the quantitative supply of magnesium powder into the heating inner tank 2, which is conducive to accurately controlling the reaction ratio of magnesium powder and hydrogen.

[0057] The process and principle of continuous production of magnesium hydride are as follows: (1) The heating inner tank 2 is surrounded by the sealed outer shell 1. After the moisture and oxygen in the sealed outer shell 1 and the heating inner tank 2 are replaced by argon gas, magnesium powder is continuously added and hydrogen is injected. By rotating the heating inner tank 2, the magnesium powder and hydrogen are continuously contacted and reacted to form magnesium hydride. The magnesium hydride passes through the filter screen 26 and enters the discharge lock hopper 52, thereby realizing the continuous production of magnesium hydride. The production process is sealed, safe and reliable; (2) The particle size of the magnesium powder in this embodiment is 10μm-300μm. m, the particle size of the produced magnesium hydride is 50nm-800nm, which can realize continuous feeding, continuous reaction and continuous discharging, and realize large-scale production of magnesium hydride. The hydrogen storage density of magnesium hydride is not less than 7wt%; (3) a screw propeller 24, a plurality of steel balls and / or a plurality of steel rods 25 are arranged in the heating inner tank 2, the diameter of the steel balls is 30mm-100mm, the diameter of the steel rods is 30mm-100mm, each steel ball or steel rod has a considerable weight, and during the rotation of the heating inner tank 2, the screw propeller 24 In the process of pushing the magnesium powder or magnesium hydride forward and stirring the magnesium powder or magnesium hydride, the steel balls and / or steel rods 25 continuously fall from the top of the heating inner tank 2 under the combined action of rotational inertia and gravity, and hit the magnesium powder or magnesium hydride in the process of falling, and continuously crush or refine the magnesium powder or magnesium hydride particles, so that the crushed or refined magnesium powder particles are more exposed and contact with hydrogen to react to generate more magnesium hydride; during the reaction process, the heating temperature of the heating inner tank 2 is maintained at 250°C- 450°C. After hydrogen is introduced, since the reaction between magnesium powder and hydrogen is an exothermic reaction, in order to keep the heating temperature between 250°C and 450°C, the temperature of the heating inner tank 2 can be reduced to ensure that the heating temperature of the heating inner tank 2 is maintained between 250°C and 450°C. During the reaction, the rotation speed of the heating inner tank 2 is 5r / min-25r / min, and the air pressure in the heating inner tank 2 is 2MPa-4MPa. In the range of the rotation speed of 5r / min-25r / min, such as 10r / min , 15r / min, which can not only ensure the propulsion and stirring of magnesium powder or magnesium hydride, but also drive a plurality of steel balls and / or a plurality of steel rods 25 to rotate along the side wall 21. Under the joint action of rotational inertia and gravity, a plurality of steel balls and / or a plurality of steel rods 25 continuously fall from the top of the heating liner 2 and hit the magnesium powder or magnesium hydride to achieve the refinement of the magnesium powder or magnesium hydride. If the speed exceeds 25r / min, a plurality of steel balls and / or a plurality of steel rods 25 cannot fall due to excessive inertia, and the rotation speed is too low to drive a plurality of steel balls and / or a plurality of steel rods 25 to rotate with them.

[0058] The principle that the plurality of steel balls and / or steel rods 25 can effectively refine the magnesium hydride particles is as follows: after the magnesium powder contacts the hydrogen, the outermost layer of the magnesium powder first forms magnesium hydride. Due to the coating effect of the magnesium hydride, if it is no longer crushed, the coated magnesium powder cannot continue to react further with hydrogen. In order to make as much magnesium powder as possible react with hydrogen, under the action of the screw propeller 24, the plurality of steel balls and / or steel rods 25, especially because the magnesium hydride coated on the surface of the magnesium powder is brittle, after the plurality of steel balls and / or steel rods 25 are repeatedly smashed, the magnesium hydride coating layer is destroyed, so that the exposed magnesium powder further reacts with hydrogen. After repeated crushing or refining of the magnesium powder and magnesium hydride particles, nano-scale magnesium hydride particles are formed, and finally magnesium hydride with a hydrogen storage density of not less than 7wt% is formed. In order to ensure the reaction time and crushing efficiency of continuous production of magnesium hydride, the motor 31 rotates forward and reverse alternately to achieve the following effects: (1) the magnesium powder or magnesium hydride is fully stirred to increase the contact probability between the magnesium powder and hydrogen, and to increase the probability and time of the magnesium powder or magnesium hydride being crushed; (2) the magnesium powder or magnesium hydride stays in the heating inner tank 2 for 2h-6h. Even if the length of the heating inner tank 2 is short, the magnesium powder or magnesium hydride can still stay in the heating inner tank 2 for 2h-6h. By alternating forward and reverse rotation, the walking path of the magnesium hydride in the heating inner tank 2 can be effectively increased, which is beneficial to the crushing or refinement of the magnesium hydride particles; (3) Reversal can also cause a number of steel balls and / or a number of steel rods 25 to flow back, avoiding a number of steel balls and / or a number of steel rods 25 from accumulating near the filter 26, and effectively increasing the probability of a number of steel balls and / or a number of steel rods 25 crushing or refining the magnesium powder or magnesium hydride particles.

[0059] In order to ensure the safety of the magnesium hydride production process, the sealed shell 1 is provided with a moisture sensor 13, an oxygen sensor 14 and an air pressure sensor 15; the moisture sensor 13 is used to detect the moisture content of the sealed shell 1 and the heating liner 2, the oxygen sensor 14 is used to detect the oxygen content of the sealed shell 1 and the heating liner 2, the air pressure sensor 15 is used to detect the air pressure of the sealed shell 1 and the heating liner 2, and a temperature sensor is provided in the heating liner 2 to monitor the temperature in the heating liner 2 in real time. When the moisture sensor 13 senses that the moisture content exceeds 4000ppm, the hydrogen injection is stopped, the heating of the heating liner 2 is stopped, the feeding of magnesium powder is stopped, the inert gas replacement component 6 is started, and the argon replacement is started until the moisture content does not exceed 4000ppm, and production is resumed; when the oxygen sensor 14 senses that the oxygen content exceeds 4000ppm, the hydrogen injection is stopped, the heating of the heating liner 2 is stopped, the feeding of magnesium powder is stopped, the inert gas replacement component 6 is started, and the argon replacement is started until the oxygen content does not exceed 4000ppm, and production is resumed; when the air pressure sensor 15 senses that the air pressure exceeds 4MPa, the hydrogen injection is stopped; the temperature sensor is used to control and adjust the heating power of the heating liner 2 in real time to keep the temperature inside the heating liner 2 between 250℃ and 450℃.

[0060] See also Figure 2 , 50 mesh (particle size 300 μm) and 300 mesh (particle size 50 μm) magnesium powders were selected as raw materials, and magnesium hydride particles were prepared by the magnesium hydride continuous production device of this embodiment. After XRD analysis, characteristic peaks of magnesium hydride (110, 101, 200, 221) appeared in the X-ray diffraction diagram, proving that this embodiment can continuously synthesize magnesium hydride; see Figure 3 ,right Figure 2 The magnesium hydride particles obtained from the raw material 50 mesh magnesium powder are dehydrogenated. After exceeding 400°C, the magnesium hydride is cracked into magnesium and hydrogen. After measurement, Figure 2 The hydrogen content of the magnesium hydride particles obtained from the raw material 50 mesh magnesium powder can reach 7.2wt%, realizing the continuous preparation of magnesium hydride with a hydrogen storage density of not less than 7wt%.

[0061] Example 2

[0062] Ginseng Figure 4 As shown, this embodiment discloses a specific implementation method of a continuous production process of magnesium hydride.

[0063] The continuous production process of magnesium hydride, using the continuous production device of magnesium hydride described in Example 1, comprises the following steps:

[0064] Step S1: The gas in the sealed sealed shell and the heating inner tank is replaced by argon gas, so that the oxygen content in the heating inner tank is less than 4000ppm, and the moisture content is less than 4000ppm; specifically, the purpose of step S1 is to replace the oxygen and moisture in the sealed shell 1 and the heating inner tank 2 to prevent the magnesium powder from being oxidized or producing a violent reaction, thereby ensuring the safety of the magnesium hydride production process.

[0065] Step S2: start heating to make the temperature in the heating liner 2 reach 250°C-450°C;

[0066] Step S3: magnesium powder with a particle size of 10 μm-300 μm flows into the heating inner container from the feed lock hopper;

[0067] Step S4: Start the motor and drive the heating liner to rotate through the magnetic drive, and synchronously drive the spiral propeller to rotate, the spiral propeller drives the magnesium powder, a plurality of steel balls and / or a plurality of steel rods to rotate together, and injects hydrogen into the heating liner while rotating, and reacts for 2h-6h; Specifically, in step S4, on the one hand, after the hydrogen is injected, the heating power of the heating liner 2 is reduced to keep the temperature in the heating liner at 250°C-450°C; on the other hand, by adjusting the direction of the motor, the heating liner 2 rotates forward and reverse alternately, and the purpose of alternating is to (1) fully stir the magnesium powder or magnesium hydride to increase the contact probability between the magnesium powder and the hydrogen, The invention increases the probability and time of the crushing of magnesium powder or magnesium hydride; (2) the time that the magnesium powder or magnesium hydride stays in the heating inner tank 2 should last for 2h-6h. Even if the length of the heating inner tank 2 is short, the magnesium powder or magnesium hydride can still stay in the heating inner tank 2 for 2h-6h. By alternating forward and reverse rotation, the walking path of the magnesium hydride in the heating inner tank 2 can be effectively increased, which is beneficial to the crushing or refinement of the magnesium hydride particles; (3) Reversal can also make a number of steel balls and / or a number of steel rods 25 reflux, avoid a number of steel balls and / or a number of steel rods 25 from accumulating near the filter screen 26, and effectively increase the probability of a number of steel balls and / or a number of steel rods 25 crushing or refining the magnesium powder or magnesium hydride particles.

[0068] Step S5: Step S4 reacts to form magnesium hydride, wherein the particle size of the magnesium hydride is 50nm-800nm;

[0069] Step S6: The magnesium hydride in step S5 is discharged from the discharge lock hopper.

[0070] In steps S3 and S4, if any data sensed by the moisture sensor and the oxygen sensor is abnormal, the injection of hydrogen and magnesium powder is stopped, the heating power of the heating liner is turned off, and argon is injected for replacement; when the moisture sensor 13 senses that the moisture content exceeds 4000ppm, the hydrogen injection is stopped, the heating liner 2 stops heating, the magnesium powder stops feeding, the inert gas replacement component 6 is started, and the argon replacement is started until the moisture content does not exceed 4000ppm, and then production is resumed; when the oxygen sensor 14 senses that the oxygen content exceeds 4000ppm, the hydrogen injection is stopped, the heating liner 2 stops heating, the magnesium powder stops feeding, the inert gas replacement component 6 is started, and the argon replacement is started until the oxygen content does not exceed 4000ppm, and then production is resumed; when the air pressure sensor 15 senses that the air pressure exceeds 4MPa, the hydrogen injection is stopped; the temperature sensor is used to control and adjust the heating power of the heating liner 2 in real time to keep the temperature in the heating liner 2 between 250℃ and 450℃.

[0071] The continuous production process of magnesium hydride disclosed in this embodiment has the same technical solution as that in Example 1. Please refer to Example 1 and will not repeat it here.

Claims

1. A continuous production device for magnesium hydride, characterized in that: It includes a sealed shell, a heating liner, a power component, a feed component, a discharge component, an inert gas replacement component and a hydrogenation inlet; The heating inner container comprises a side wall, a feeding end and a discharging end, a plurality of gas one-way valves are arranged on the side wall, a screw propeller, a plurality of steel balls and / or a plurality of steel rods are arranged in the heating inner container, a filter screen is arranged on the discharging end, and the plurality of steel balls and / or a plurality of steel rods crush the magnesium powder and the magnesium hydride coated on the surface of the magnesium powder; A conical portion and a recovery port are provided at the bottom of the sealing shell, and the recovery port is provided at the bottom of the conical portion; The feed assembly comprises a feed lock bucket and a feed pipe, and the feed pipe is connected to the feed end; The discharging assembly comprises a discharging pipe and a discharging lock bucket, and the discharging pipe is connected to the discharging end; The inert gas replacement assembly includes a gas inlet and a gas outlet; The power assembly includes a motor, a magnetic drive, a power shaft, a driving gear and a passive gear; The motor drives the driving gear through the magnetic drive, the driving gear meshes with the passive gear, and the passive gear drives the heating liner to rotate; The motor rotates forward and reverse alternately.

2. The magnesium hydride continuous production device according to claim 1, characterized in that: The rotation speed of the heating inner tank is 5r / min-25r / min.

3. The magnesium hydride continuous production device according to claim 1, characterized in that: The heating temperature of the heating inner container is 250°C-450°C.

4. The magnesium hydride continuous production device according to claim 1, characterized in that: The diameter of the steel ball is 30mm-100mm, and the diameter of the steel rod is 30mm-100mm.

5. The magnesium hydride continuous production device according to claim 1, characterized in that: The air pressure in the heating liner is 2MPa-4MPa.

6. The magnesium hydride continuous production device according to claim 1, characterized in that: The sealed housing is provided with a moisture sensor, an oxygen sensor and an air pressure sensor; A temperature sensor is arranged in the heating inner container.

7. The continuous production device for magnesium hydride according to claim 1, characterized in that: The feed pipe is provided with a first valve group and a second valve group respectively located before and after the feed lock bucket; Open the first valve group and close the second valve group, and add magnesium powder into the feed lock hopper; Open the second valve group and close the first valve group, and add magnesium powder into the heating inner container; The discharge pipe is provided with a third valve group and a fourth valve group respectively located before and after the discharge lock bucket; Open the third valve group and close the fourth valve group to allow magnesium hydride to flow from the heating inner tank into the discharge lock hopper; The fourth valve group is opened and the third valve group is closed to collect magnesium hydride from the discharge lock hopper.

8. A continuous production process for magnesium hydride, characterized in that: The magnesium hydride continuous production device according to any one of claims 1 to 7 comprises the following steps: Step S1: replacing the gas in the sealed outer shell and the heating inner container with argon gas, so that the oxygen content in the heating inner container is less than 4000 ppm and the water content is less than 4000 ppm; Step S2: starting heating to make the temperature in the heating inner container reach 250° C.-450° C.; Step S3: magnesium powder with a particle size of 10 μm-300 μm flows into the heating inner container from the feed lock hopper; Step S4: starting the motor and driving the heating liner to rotate through the magnetic drive, and synchronously driving the screw propeller to rotate, the screw propeller drives the magnesium powder, a plurality of steel balls and / or a plurality of steel rods to rotate together, and injecting hydrogen into the heating liner while rotating, reacting for 2h-6h, the plurality of steel balls and / or a plurality of steel rods crushing the magnesium powder and the magnesium hydride coated on the surface of the magnesium powder; Step S5: Step S4 reacts to form magnesium hydride, wherein the particle size of the magnesium hydride is 50nm-800nm; Step S6: The magnesium hydride in step S5 is discharged from the discharge lock hopper.

9. The continuous production process of magnesium hydride according to claim 8, characterized in that: In step S4, after the hydrogen is injected, the heating power of the heating inner tank is reduced so that the temperature in the heating inner tank is maintained at 250° C.-450° C.; In step S4, the heating inner container rotates forward and reverse alternately; In steps S3 and S4, if any data sensed by the moisture sensor and the oxygen sensor is abnormal, the injection of hydrogen and magnesium powder is stopped, the heating power of the heating liner is turned off, and argon is injected for replacement.

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