Continuous preparation method and preparation device of nano magnesium hydride

Abstract

The invention discloses a continuous preparation method and a preparation device of nano magnesium hydride, and the continuous preparation method of nano magnesium hydride comprises the following steps: a, preparing realization materials including magnesium chloride, lithium hydride and ultra-dry tetrahydrofuran, b, respectively adding magnesium chloride and lithium hydride into tetrahydrofuran in an argon gas atmosphere, and continuously stirring to obtain the nano magnesium hydride. The molar ratio of the magnesium chloride to the lithium hydride is 1: 2, c, in an argon atmosphere, stirring and mixing the tetrahydrofuran solution of the magnesium chloride and the tetrahydrofuran turbid liquid of the lithium hydride in which the tetrahydrofuran turbid liquid of the magnesium chloride is uniformly dispersed to obtain a tetrahydrofuran solution of the magnesium chloride and a tetrahydrofuran turbid liquid of the lithium hydride, and drying the tetrahydrofuran solution of the magnesium chloride and the tetrahydrofuran turbid liquid of the lithium hydride; according to the continuous preparation method and the preparation device of the nano magnesium hydride, the preparation efficiency is high, and the collected target product has relatively high purity and relatively good hydrogen absorption and desorption performance.

Description

Technical Field

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

[0002] MgH2 has the advantages of abundant resources, low price and high hydrogen storage capacity, and is considered to be the most promising low-pressure solid-state hydrogen storage material. However, due to its high thermodynamic stability and large kinetic energy barrier, its high hydrogen absorption / desorption temperature, slow reaction rate, and poor cycle performance have greatly restricted the commercial application of magnesium-based hydrogen storage materials.

[0003] Because the Mg-H chemical bond has strong ionic bond characteristics, the dehydrogenation temperature of MgH2 is relatively high. In order to improve the hydrogen absorption / desorption performance of MgH2, researchers at home and abroad have carried out a lot of work, mainly including alloying, catalyst doping and nano-sizing.

[0004] Among them, alloying is one of the effective methods to improve the hydrogen absorption / desorption performance of MgH2. Commonly used alloying metal elements are mainly transition metal elements and rare earth metal elements, such as Ni, Co, Cu, La, Ce, etc. Although the thermodynamic properties can be improved by alloying transition metals with Mg, the alloying elements are heavy. The presence of a large amount of alloying elements will reduce the hydrogen storage capacity of the hydrogen storage material, and the kinetic performance is also not ideal.

[0005] The use of a small amount of catalyst to modify the hydrogen storage performance of MgH2 is a current research hotspot. Studies have shown that transition metals and their oxides, halides, intermetallic compounds, etc. have a good catalytic effect on MgH2. By introducing catalytic components, the active sites of the reaction system are increased, the energy barrier of hydrogen absorption and desorption reactions is significantly reduced, the ability of H atoms to diffuse into the interior of the lattice is increased, and the kinetic properties are improved. However, the thermodynamics of MgH2 is relatively stable, and the initial hydrogen desorption temperature is still relatively high.

[0006] Compared with alloying and catalyst doping, nano-sizing is expected to improve both the kinetic and thermodynamic properties of MgH2. For magnesium-based hydrogen storage materials, when the size is reduced to nano-size, the diffusion path will be shortened, the diffusion of hydrogen atoms will be accelerated, and the time of hydrogen absorption and desorption reactions will be shortened. Moreover, nano-sizing can reduce the nucleation energy barrier and make the reaction easier, thus helping to improve the kinetic performance. At the same time, the nano-sizing of particles will increase the instability of the hydrogen storage system and affect the enthalpy change of hydrogen absorption and desorption reactions. However, the existing MgH2 nano-sizing is mainly achieved by uniformly loading the material with high specific surface area graphene, MOF, etc., thereby reducing the hydrogen storage capacity of the material.

[0007] Therefore, it is of great practical significance to prepare nano-MgH2 with high hydrogen storage capacity and excellent hydrogen absorption and desorption performance. Summary of the invention

[0008] The present invention provides a continuous preparation method and a preparation device for nano magnesium hydride, which are used to solve the problems of low production efficiency and poor hydrogen storage capacity in the prior art when preparing nano magnesium hydride.

[0009] The technical solution of the present invention is as follows: A continuous preparation method of nano magnesium hydride comprises the following steps:

[0010] a. Prepare realization materials, wherein the realization materials include magnesium chloride, lithium hydride and ultra-dry tetrahydrofuran;

[0011] b. In an argon gas atmosphere, magnesium chloride and lithium hydride are added to tetrahydrofuran respectively, and stirred to obtain a tetrahydrofuran solution in which magnesium chloride is completely dissolved and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, respectively, and the molar ratio of magnesium chloride to lithium hydride is 1:2;

[0012] c. In an argon gas atmosphere, stirring and mixing a tetrahydrofuran solution of magnesium chloride and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, to obtain an organic suspension in which magnesium chloride and lithium hydride are uniformly mixed;

[0013] d. In an argon gas atmosphere, subjecting the organic suspension uniformly mixed with magnesium chloride and lithium hydride to constant temperature ultrasonic treatment;

[0014] e. After the reaction is completed, the reaction product is in situ passivated, and then centrifuged and dried to obtain nano magnesium hydride particles;

[0015] f. The supernatant after centrifugation is transferred to a solvent purification system, and the treated tetrahydrofuran is transferred to a preparation device for recycling and continuous preparation of the next batch.

[0016] As the preferred technical solution of this application;

[0017] In step a, the magnesium chloride is anhydrous magnesium chloride;

[0018] In step b, before adding magnesium chloride and lithium hydride to tetrahydrofuran, magnesium chloride and lithium hydride need to be ground respectively to obtain magnesium chloride and lithium hydride powders. After adding magnesium chloride powder to tetrahydrofuran, the stirring time is set to 6 to 12 hours, and after adding lithium hydride powder to tetrahydrofuran, the stirring time is set to 0.5 to 1 hour;

[0019] In step c, the stirring time of the organic suspension is set to 1 to 2 hours;

[0020] In step d, the organic suspension is ultrasonically treated with an ultrasonic rod, the single ultrasonic time is 3 to 5 seconds, the interval time is 3 to 5 seconds, the cumulative ultrasonic time is 1 to 4 hours, and the ultrasonic constant temperature is 5 to 10°C.

[0021] A continuous preparation device for nano magnesium hydride, used to implement steps a to d, comprising a preparation support, a raw material insulation cylinder, a main mixing cylinder, an ultrasonic vibration rod, a main mixing mechanism and an auxiliary mixing mechanism with a crushing function;

[0022] The raw material insulation cylinder is arranged on the preparation support, and the two sides of the raw material insulation cylinder are respectively connected with a liquid inlet insulation pipe and a liquid outlet insulation pipe;

[0023] The main mixing cylinder is arranged in the raw material insulation cylinder, and a sealed insulation cavity is formed between the main mixing cylinder and the raw material insulation cylinder. The bottom of the main mixing cylinder is connected with a main discharge pipe, which penetrates and seals the raw material insulation cylinder and the preparation bracket, and a main discharge valve is installed on the main discharge pipe;

[0024] There are multiple ultrasonic vibration rods, which penetrate the raw material insulation cylinder and the main mixing cylinder at equal angles and are sealed;

[0025] The main mixing mechanism is arranged on the preparation support, and the main mixing mechanism penetrates and is sealed and rotatably arranged in the raw material heat preservation cylinder;

[0026] There are multiple auxiliary mixing mechanisms, which are arranged on the preparation support, sealed and connected with the raw material insulation cylinder, and meshed with the main mixing mechanism.

[0027] On the basis of the above scheme, the main mixing mechanism includes a main mixing rod, a mixing motor, a spiral mixing blade, a mixing evenly distributed baffle, a mixing reciprocating screw rod and a bevel gear;

[0028] The main mixing rod penetrates and is rotatably and sealingly arranged on the main mixing cylinder;

[0029] The mixing motor is installed on the preparation bracket, and the output end of the mixing motor is connected to the main mixing rod;

[0030] The spiral mixing blade is arranged on the main mixing rod, and the spiral mixing blade is located in the main mixing barrel;

[0031] The mixing evenly distributing baffle is arranged on the main mixing rod, and the mixing evenly distributing baffle is located above the spiral mixing blade in the main mixing barrel;

[0032] The mixing reciprocating screw rod is arranged on the main mixing rod, a mixing ball nut group is threadedly connected to the mixing reciprocating screw rod, and the auxiliary mixing mechanism is connected to the mixing reciprocating screw rod;

[0033] The bevel gear 1 is arranged on the main mixing rod, and the auxiliary mixing mechanism is meshed with the bevel gear 1.

[0034] On the basis of the above scheme, the auxiliary mixing mechanism includes an auxiliary mixing cylinder, a feeding pipe, an auxiliary mixing component with segmented material discharging and storage functions, and a crushing component;

[0035] The auxiliary mixing cylinder is arranged on the preparation support;

[0036] The feeding pipe is arranged between the auxiliary mixing cylinder and the main mixing cylinder in an inclined sealed manner, and a feeding valve is installed on the feeding pipe;

[0037] The auxiliary mixing component is disposed on the auxiliary mixing barrel, and the auxiliary mixing component is connected to the mixing ball nut assembly;

[0038] The crushing component is arranged on the preparation support, the crushing component is connected to the auxiliary mixing box, and the crushing component is meshed with the bevel gear one.

[0039] Further on the basis of the above scheme, the auxiliary mixing assembly includes an auxiliary mixing tube, an auxiliary separation plate, a one-way control plate and a control plate steering portion with a self-locking function;

[0040] The auxiliary mixing tube penetrates and is longitudinally sealed and slidably arranged on the auxiliary mixing cylinder, and the auxiliary mixing tube is connected to the mixing ball nut assembly through a connecting frame;

[0041] The auxiliary separation disk is sealed and slidably disposed in the auxiliary mixing tube, and the auxiliary separation disk is connected to the auxiliary mixing tube;

[0042] A one-way regulating groove is formed at one end of the auxiliary separation plate away from the auxiliary mixing tube, the one-way regulating plate is sealed and rotatably arranged in the one-way regulating groove, a plurality of one-to-one corresponding mixing through holes are formed on the one-way regulating plate and the auxiliary separation plate, and a mixing rack is arranged in each mixing through hole;

[0043] The steering portion of the regulating plate is sealed and rotatably arranged in the auxiliary mixing tube, and the steering portion of the regulating plate is connected to the one-way regulating plate.

[0044] On the basis of the above scheme, the steering part of the control plate includes a steering rod, a hexagonal steering rod, a steering handle, a steering limit column and a steering limit plate;

[0045] The steering rod penetrates and is sealed and rotatably arranged in the auxiliary mixing tube, one end of the steering rod is connected to the one-way regulating plate, and the other end of the steering rod is provided with a hexagonal limit regulating groove;

[0046] The hexagonal steering rod penetrates and is slidably arranged in the hexagonal limit adjustment groove, and a limit spring is arranged between the hexagonal steering rod and the hexagonal limit adjustment groove;

[0047] The steering handle is arranged at one end of the hexagonal steering rod away from the steering lever;

[0048] The steering limit column is arranged on the steering handle;

[0049] The steering limit plate is arranged on the auxiliary mixing tube, a plurality of limit through holes are provided at equal angles on the steering limit plate, and the steering limit posts are located in the corresponding limit through holes.

[0050] Further on the basis of the above scheme, the crushing assembly includes a conical crushing box, a crushing tube, a grinding rotating rod 1, a conical grinding head, a grinding rotating rod 2, a bevel gear 2, a bevel gear 3, a bevel gear 4 and a feed hopper;

[0051] The conical crushing box is arranged on the preparation support;

[0052] The crushed material delivery pipe is arranged between the conical crushed material box and the auxiliary mixing cylinder, and an upper delivery valve and a lower delivery valve are installed on the crushed material delivery pipe, and a material storage cavity is formed between the upper delivery valve and the lower delivery valve;

[0053] The grinding rotating rod is penetrated and sealed and rotatably arranged on the conical crushing box;

[0054] The conical grinding head is arranged on the first grinding rotating rod, and the conical grinding head is located in the conical crushing box, and a grinding cavity is formed between the conical grinding head and the conical crushing box;

[0055] The grinding rotating rod 2 is rotatably disposed on the preparation bracket;

[0056] The second bevel gear is arranged on the second grinding rotating rod, and the second bevel gear is meshed with the first bevel gear;

[0057] The bevel gear 3 is arranged on the grinding rotating rod 2;

[0058] The bevel gear 4 is arranged on the grinding rotating rod 1, and the bevel gear 4 is meshed with the bevel gear in three phases;

[0059] The feed hopper is arranged on the preparation support through the feed hopper, and the feed hopper is communicated with the conical crushing box.

[0060] Further on the basis of the above scheme, each of the auxiliary mixing cylinders is connected to a liquid inlet pipe, the liquid inlet pipe passes through the preparation bracket, and a liquid inlet valve is installed on the liquid inlet pipe.

[0061] Further on the basis of the above solution, the main mixing cylinder and each of the auxiliary mixing cylinders are connected with an air supply pipe, and the air supply pipe is installed with an air supply valve.

[0062] The preparation principle and beneficial effects of the present invention are:

[0063] 1. In the present invention, before the preparation stage, the gas transmission pipe is connected to the argon gas storage tank, the liquid inlet pipe is connected to the ultra-dry tetrahydrofuran solution storage tank, the liquid inlet insulation pipe and the liquid outlet insulation pipe are respectively connected to the liquid inlet end and the liquid outlet end of the insulation mold temperature controller, the feed hopper is connected to the glove box, and finally the main discharge pipe is connected to the in-situ passivation equipment;

[0064] 2. In the present invention, when preparing nano magnesium hydride, magnesium chloride particles and lithium hydride particles are added into a conical crushing box through a corresponding glove box and a feed hopper, and then the upper delivery valve is opened, the lower delivery valve is closed, and the mixing motor is started. The rotation of the mixing motor drives the main mixing rod to rotate, and the rotation of the main mixing rod drives the bevel gear 1 to rotate, and the rotation of the bevel gear 1 drives the bevel gear 2 to rotate, and the rotation of the bevel gear 2 drives the grinding rotating rod 2 to rotate, and the rotation of the grinding rotating rod 2 drives the bevel gear 3 to rotate, and the rotation of the bevel gear 3 drives the bevel gear 4 to rotate, and the rotation of the bevel gear 4 drives the grinding rotating rod 1 to rotate, and the rotation of the grinding rotating rod 1 drives the conical grinding head to rotate, and the magnesium chloride particles and lithium hydride particles in the conical crushing box are crushed by the rotation of the conical grinding head, so that the crushed pieces fall into the material storage cavity, and then the upper delivery valve is closed to store the crushed raw materials;

[0065] 3. In the present invention, after the magnesium chloride particles and the lithium hydride particles are ground and prepared, the main mixing rod is rotated to drive the mixing reciprocating screw rod to rotate, the rotation of the mixing reciprocating screw rod drives the mixing ball nut group to perform linear reciprocating motion, the movement of the mixing ball nut group drives the connecting frame to move, the connecting frame drives the auxiliary mixing pipe to move, and the auxiliary separation plate is driven to move in the auxiliary mixing cylinder through the auxiliary mixing pipe. When the auxiliary separation plate moves to one side of the crushed material delivery pipe, the mixing motor stops starting, and then the steering handle is pulled upward, and the hexagonal turn is deformed through the limit spring. The steering rod slides in the hexagonal limit adjustment groove, and at the same time separates the steering limit column from the steering limit plate, and then the steering handle is turned. The rotation of the steering handle drives the hexagonal steering rod to rotate, and the rotation of the hexagonal steering rod drives the steering rotating rod to rotate. The rotation of the steering rotating rod drives the one-way control plate to rotate, so that the mixing through holes in the one-way control plate and the auxiliary separation plate are in a staggered state. At this time, the one-way control plate and the auxiliary separation plate will form a sealing plate, and then the steering handle is loosened to insert the steering limit column into the corresponding limit through hole to fix the position of the one-way control plate;

[0066] 4. In the present invention, after the position of the one-way control plate is fixed, the mixing motor is started again, and the auxiliary partition plate is moved toward one side of the feeding pipe through the mixing ball nut group. When the auxiliary partition plate moves toward one side of the feeding pipe, a vacuum area is formed between the auxiliary partition plate and the crushed material delivery pipe in the auxiliary mixing barrel. Under the action of air pressure, the gas and liquid in the argon gas storage tank and the ultra-dry tetrahydrofuran solution storage tank are respectively delivered to the auxiliary mixing barrel through the gas delivery pipe and the liquid inlet pipe. In this process, by starting the lower delivery valve, a certain amount of magnesium chloride particles or lithium hydride particles after crushing can be added to the auxiliary mixing barrel at the same time, completing the scheme described in step 2;

[0067] 5. In the present invention, when the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are stirred and mixed, the mixing motor is first stopped and started, and the one-way control plate and the mixing through hole in the auxiliary partition plate are made to coincide with each other by rotating the steering handle, and the mixing motor is started again, so that the auxiliary partition plate moves back and forth in a straight line in the auxiliary mixing cylinder, and the solution in the auxiliary mixing box passes through the mixing through hole, and the solution is stirred by the mixing rack in the mixing through hole, so that the solution is mixed;

[0068] 6. According to the present invention, after the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are mixed and stirred, the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are discharged into the main mixing barrel for reaction preparation, and after the auxiliary partition plate is moved to the side of the crushed material delivery pipe again, the one-way control plate and the auxiliary partition plate are turned to form a sealing plate, and then the feeding valve is opened, and then the mixing motor is started to move the auxiliary partition plate toward the feeding pipe, and the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride in the auxiliary mixing barrel are squeezed into the main mixing barrel through the corresponding feeding pipes, and at the same time, the next batch of tetrahydrofuran solution of magnesium chloride and tetrahydrofuran suspension of lithium hydride can be synchronously added to the auxiliary mixing barrel through the gas transmission pipe, the liquid inlet pipe and the crushed material delivery pipe to carry out continuous processing of nano magnesium hydride;

[0069] 7. In the present invention, when the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride in the auxiliary mixing barrel are respectively discharged into the main mixing barrel through corresponding feeding pipes, the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are preferentially converged and collided on the mixing and spreading baffle plate to perform preliminary fusion. Then, after the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride enter the main mixing barrel, the rotation of the main mixing rod will also drive the spiral mixing blade to rotate. The mixed liquid in the main mixing barrel is stirred and mixed by the rotation of the spiral mixing blade. In the mixing process, the ultrasonic vibration rod is intermittently started to provide energy by the cavitation effect generated by ultrasonic waves in the liquid to promote the occurrence of chemical reaction between magnesium chloride and lithium hydride. By using an ultrasonic rod type ultrasonic instrument for ultrasonic reaction, compared with ordinary ultrasonic cleaning machines, the ultrasonic energy provided by the ultrasonic vibration rod is more concentrated, the reaction rate is faster, and the production efficiency is higher. At the same time, the crushing effect of ultrasonic waves can effectively control the particle size of the product and avoid particle agglomeration, thereby obtaining nano-scale magnesium hydride.

[0070] 8. In the present invention, the reaction degree of the reactants gradually increases with the accumulation of ultrasonic time during the ultrasonic process by the ultrasonic vibrating rod, and the amount of nano magnesium hydride generated increases accordingly. However, with the accumulation of energy in the organic medium, the temperature of the reaction system tends to increase, which will promote the growth of nano particles, and the hydrogen absorption and desorption kinetics of the obtained product will be attenuated. Similar to the extension of ultrasonic time, excessive power will also cause excess energy, resulting in an increase in system temperature and an increase in product particles. Therefore, by starting the heat preservation mold temperature machine, constant temperature water enters the sealed heat preservation cavity through the liquid inlet heat preservation pipe, and then is discharged through the liquid outlet heat preservation pipe, and the solution inside the main mixing cylinder is subjected to constant temperature treatment through heat exchange;

[0071] 9. The present invention, after the chemical reaction between magnesium chloride and lithium hydride is completed in the main mixing barrel, the main discharge valve is opened, argon gas is introduced into the main mixing barrel through the gas pipe, the reacted solution is squeezed into the in-situ passivation equipment, and 1‰ O2-Ar mixed gas is introduced into the mixed solution after the reaction to perform in-situ passivation. After a passivation time of 15-20 minutes, the nano magnesium hydride particles can be obtained by centrifugation and drying, and the supernatant after centrifugation is transferred to a solvent purification system, and the treated tetrahydrofuran is transferred to an ultra-dry tetrahydrofuran solution storage tank for recycling.

[0072] 10. The present invention, the continuous preparation method, uses the cavitation effect generated by ultrasound in the liquid to provide energy to promote the chemical reaction between magnesium chloride and lithium hydride. The ultrasonic energy provided by the ultrasonic vibration rod is more concentrated and the reaction rate is faster. Therefore, compared with the experimental schemes of other energy sources of the same type, the preparation method of the present invention has simple process, short experimental cycle and high production efficiency. At the same time, the preparation process is controllable and can be industrially produced. The reactants magnesium chloride and lithium hydride react chemically under the drive of ultrasonic energy to generate magnesium hydride and lithium chloride (the reaction chemical equation is: [MgCl2+2LiH→MgH2+2LiCl]), wherein magnesium chloride and lithium chloride are easily soluble in tetrahydrofuran, and lithium hydride has a lower density and is usually suspended in an organic medium. Therefore, the target product collected after the reaction has a higher purity and a larger hydrogen storage capacity. BRIEF DESCRIPTION OF THE DRAWINGS

[0073] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0074] Figure 1 It is a schematic structural diagram of a partial cross-section of a continuous preparation device of nano magnesium hydride of the present invention;

[0075] Figure 2 For the present invention Figure 1 A schematic diagram of the local enlarged structure at point A in the middle;

[0076] Figure 3 For the present invention Figure 1 A schematic diagram of the local enlarged structure at B in the middle;

[0077] Figure 4 For the present invention Figure 1 A schematic diagram of the local enlarged structure at C in the middle;

[0078] Figure 5 For the present invention Figure 1 A schematic diagram of the local enlarged structure at D in the middle;

[0079] Figure 6 For the present invention Figure 1 A schematic diagram of the local enlarged structure at E in the middle;

[0080] Figure 7 It is a structural schematic diagram of a partial cross-section of the matching parts of a raw material insulation cylinder, a liquid inlet insulation pipe, a liquid outlet insulation pipe, a main mixing cylinder, a main discharge pipe, a main discharge valve and an ultrasonic vibration rod in a continuous preparation device for nano magnesium hydride of the present invention;

[0081] Figure 8 It is a structural schematic diagram of a main mixing mechanism in a continuous preparation device for nano-magnesium hydride of the present invention;

[0082] Fig. 9 It is a structural schematic diagram of a partial cross-section of an auxiliary mixing tube and a steering part of a control plate in a continuous preparation device for nano-magnesium hydride of the present invention;

[0083] Fig.10 It is a schematic diagram of the overall structure of a continuous preparation device for nano-magnesium hydride of the present invention;

[0084] Fig.11 This is a transmission electron microscope image of nano magnesium hydride prepared by the present invention;

[0085] Fig.12 The X-ray diffraction pattern of the nano magnesium hydride prepared by the present invention;

[0086] Fig.13 The mass spectrum of hydrogen signal of temperature-dependent dehydrogenation of nano magnesium hydride prepared by the present invention is shown.

[0087] In the figure: 001, main mixing mechanism; 002, auxiliary mixing mechanism;

[0088] 1. Preparation bracket; 2. Raw material insulation cylinder; 3. Liquid inlet insulation pipe; 4. Liquid outlet insulation pipe; 5. Main mixing cylinder; 6. Main discharge pipe; 7. Main discharge valve; 8. Ultrasonic vibration rod; 9. Main mixing rod; 10. Mixing motor; 11. Spiral mixing blade; 12. Mixing evenly distributed baffle; 13. Mixing reciprocating screw rod; 14. Mixing ball nut group; 15. Bevel gear 1; 16. Auxiliary mixing cylinder; 17. Feeding pipe; 18. Feeding valve; 19. Auxiliary mixing pipe; 20. Auxiliary partition plate; 21. One-way control plate ; 22. Mixing rack; 23. Steering lever; 24. Hexagonal steering lever; 25. Limit spring; 26. Steering handle; 27. Steering limit column; 28. Steering limit plate; 29. ​​Conical crushing box; 30. Crushing material delivery pipe; 31. Upper delivery valve; 32. Grinding lever one; 33. Conical grinding head; 34. Grinding lever two; 35. Bevel gear two; 36. Bevel gear three; 37. Bevel gear four; 38. Feed hopper; 39. Liquid inlet pipe; 40. Liquid inlet valve; 41. Gas pipe; 42. Gas valve. DETAILED DESCRIPTION

[0089] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0090] Embodiment 1

[0091] like Figures 1 to 13 As shown, this embodiment proposes a continuous preparation method of nano magnesium hydride, comprising the following steps:

[0092] a. Prepare realization materials, which include magnesium chloride, lithium hydride and ultra-dry tetrahydrofuran;

[0093] b. In an argon gas atmosphere, magnesium chloride and lithium hydride are added to tetrahydrofuran respectively, and stirred to obtain a tetrahydrofuran solution in which magnesium chloride is completely dissolved and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, respectively, and the molar ratio of magnesium chloride to lithium hydride is 1:2;

[0094] c. In an argon gas atmosphere, stirring and mixing a tetrahydrofuran solution of magnesium chloride and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, to obtain an organic suspension in which magnesium chloride and lithium hydride are uniformly mixed;

[0095] d. In an argon gas atmosphere, subjecting the organic suspension uniformly mixed with magnesium chloride and lithium hydride to constant temperature ultrasonic treatment;

[0096] e. After the reaction is completed, the reaction product is in situ passivated, and then centrifuged and dried to obtain nano magnesium hydride particles;

[0097] f. The supernatant after centrifugation is transferred to a solvent purification system, and the treated tetrahydrofuran is transferred to a preparation device for recycling and continuous preparation of the next batch.

[0098] In step a, the magnesium chloride is anhydrous magnesium chloride.

[0099] In step b, before adding magnesium chloride and lithium hydride to tetrahydrofuran, magnesium chloride and lithium hydride need to be ground respectively to obtain magnesium chloride and lithium hydride powders. After the magnesium chloride powder is added to tetrahydrofuran, the stirring time is set to 6 hours, and after the lithium hydride powder is added to tetrahydrofuran, the stirring time is set to 1 hour.

[0100] In step c, the stirring time of the organic suspension is set to 2 h.

[0101] In step d, the organic suspension is ultrasonically treated with an ultrasonic rod, the single ultrasonic time is 5 s, the interval time is 3 s, the cumulative ultrasonic time is 2 h, and the ultrasonic constant temperature is 10°C.

[0102] Embodiment 2

[0103] Embodiment 2 of the present application, based on Embodiment 1, proposes a continuous preparation device for nano-magnesium hydride, which is used to implement steps a to d, including a preparation bracket 1, a raw material insulation cylinder 2, a main mixing cylinder 5, an ultrasonic vibration rod 8, a main mixing mechanism 001 and an auxiliary mixing mechanism 002 with a crushing function.

[0104] Among them, the raw material insulation cylinder 2 is arranged on the preparation bracket 1, and the two sides of the raw material insulation cylinder 2 are respectively connected with the liquid inlet insulation pipe 3 and the liquid outlet insulation pipe 4, the main mixing cylinder 5 is arranged in the raw material insulation cylinder 2, and a sealed insulation cavity is formed between the main mixing cylinder 5 and the raw material insulation cylinder 2, and the bottom of the main mixing cylinder 5 is connected with a main discharge pipe 6, the main discharge pipe 6 passes through and is sealed with the raw material insulation cylinder 2 and the preparation bracket 1, and the main discharge pipe 6 is installed with a main discharge valve 7.

[0105] Specifically, the liquid inlet insulation pipe 3 and the liquid outlet insulation pipe 4 are respectively connected to the liquid inlet end and the liquid outlet end of the insulation mold temperature controller in the prior art. By starting the insulation mold temperature controller, the constant temperature solution circulates through the liquid inlet insulation pipe 3, the sealed insulation cavity and the liquid outlet insulation pipe 4, and the main mixing barrel 5 is subjected to constant temperature treatment.

[0106] As mentioned above, there are multiple ultrasonic vibration rods 8, and the multiple ultrasonic vibration rods 8 are evenly angled and sealed on the raw material insulation cylinder 2 and the main mixing cylinder 5. The ultrasonic vibration rods 8 are started intermittently to provide energy with the cavitation effect generated by ultrasound in the liquid to promote the chemical reaction between magnesium chloride and lithium hydride. By using an ultrasonic rod-type ultrasonic instrument for ultrasonic reaction, compared with ordinary ultrasonic cleaning machines, the ultrasonic energy provided by the ultrasonic vibration rods 8 is more concentrated, the reaction rate is faster, and the production efficiency is higher. At the same time, the crushing effect of ultrasound can effectively control the particle size of the product and avoid particle agglomeration, thereby obtaining nano-scale magnesium hydride.

[0107] As mentioned above, the main mixing mechanism 001 is arranged on the preparation support 1, and the main mixing mechanism 001 penetrates and is sealed and rotatably arranged in the raw material insulation cylinder 2. The main mixing mechanism 001 includes a main mixing rod 9, a mixing motor 10, a spiral mixing blade 11, a mixing evenly spreading baffle 12, a mixing reciprocating screw rod 13 and a bevel gear 15. The main mixing rod 9 penetrates and is sealed and rotatably arranged on the main mixing cylinder 5. The mixing motor 10 is installed on the preparation support 1, and the output end of the mixing motor 10 is connected to the main mixing rod 9. The spiral mixing blade 11 is connected to the main mixing rod 9. It is arranged on the main mixing rod 9, the spiral mixing blade 11 is located in the main mixing barrel 5, the mixing evenly distributing baffle 12 is arranged on the main mixing rod 9, the mixing evenly distributing baffle 12 is located above the spiral mixing blade 11 in the main mixing barrel 5, the mixing reciprocating screw rod 13 is arranged on the main mixing rod 9, and the mixing reciprocating screw rod 13 is threadedly connected with a mixing ball nut group 14, the auxiliary mixing mechanism 002 is connected to the mixing reciprocating screw rod 13, and the bevel gear 15 is arranged on the main mixing rod 9, and the auxiliary mixing mechanism 002 is meshed with the bevel gear 15.

[0108] As mentioned above, there are multiple auxiliary mixing mechanisms 002, which are arranged on the preparation bracket 1, the auxiliary mixing mechanism 002 is sealed and connected with the raw material insulation barrel 2, and the auxiliary mixing mechanism 002 is meshed with the main mixing mechanism 001, the auxiliary mixing mechanism 002 includes an auxiliary mixing barrel 16, a feeding pipe 17, an auxiliary mixing component with a segmented discharge and storage function, and a crushing component, the auxiliary mixing barrel 16 is arranged on the preparation bracket 1, the feeding pipe 17 is inclined and sealed and connected between the auxiliary mixing barrel 16 and the main mixing barrel 5, a feeding valve 18 is installed on the feeding pipe 17, the auxiliary mixing component is arranged on the auxiliary mixing barrel 16, and the auxiliary mixing component is connected to the mixing ball nut group 14, the crushing component is arranged on the preparation bracket 1, the crushing component is connected to the auxiliary mixing box, and the crushing component is meshed with the bevel gear 15.

[0109] The auxiliary mixing component includes an auxiliary mixing tube 19, an auxiliary separation disk 20, a one-way control plate 21 and a control plate steering portion with a self-locking function. The auxiliary mixing tube 19 penetrates and is longitudinally sealed and slidably arranged on the auxiliary mixing barrel 16. The auxiliary mixing tube 19 is connected to the mixing ball nut group 14 through a connecting frame. The auxiliary separation disk 20 is sealed and slidably arranged in the auxiliary mixing barrel 16, and the auxiliary separation disk 20 is connected to the auxiliary mixing tube 19. A one-way control groove is provided at one end of the auxiliary separation disk 20 away from the auxiliary mixing tube 19. The one-way control plate 21 is sealed and rotatably arranged in the one-way control groove. A plurality of one-to-one corresponding mixing through holes are provided on the one-way control plate 21 and the auxiliary separation disk 20, and a mixing frame 22 is provided in each mixing through hole. The control plate steering portion is sealed and rotatably arranged in the auxiliary mixing tube 19, and the control plate steering portion is The steering part of the control plate includes a steering rod 23, a hexagonal steering rod 24, a steering handle 26, a steering limit column 27 and a steering limit disk 28. The steering rod 23 passes through and is sealed and rotatably arranged in the auxiliary mixing tube 19. One end of the steering rod 23 is connected to the one-way control plate 21. The other end of the steering rod 23 is provided with a hexagonal limit adjustment groove. The hexagonal steering rod 24 passes through and is slidably arranged in the hexagonal limit adjustment groove. A limit spring 25 is arranged between the hexagonal steering rod 24 and the hexagonal limit adjustment groove. The steering handle 26 is arranged at one end of the hexagonal steering rod 24 away from the steering rod 23. The steering limit column 27 is arranged on the steering handle 26. The steering limit disk 28 is arranged on the auxiliary mixing tube 19. A plurality of limit through holes are opened at equal angles on the steering limit disk 28, and the steering limit column 27 is located in the corresponding limit through holes.

[0110] The crushing assembly includes a conical crushing box 29, a crushing delivery pipe 30, a grinding rotating rod 1 32, a conical grinding head 33, a grinding rotating rod 2 34, a bevel gear 2 35, a bevel gear 3 36, a bevel gear 4 37 and a feed hopper 38. The conical crushing box 29 is arranged on the preparation bracket 1. The crushing delivery pipe 30 is connected and arranged between the conical crushing box 29 and the auxiliary mixing barrel 16. The crushing delivery pipe 30 is equipped with an upper delivery valve 31 and a lower delivery valve. A material storage cavity is formed between the upper delivery valve 31 and the lower delivery valve. The grinding rotating rod 1 32 penetrates and is sealed and rotatably arranged on the conical crushing box 29. The conical grinding The head 33 is set on the grinding rotating rod 1 32, the conical grinding head 33 is located in the conical crushing box 29, and a grinding cavity is formed between the conical grinding head 33 and the conical crushing box 29. The grinding rotating rod 2 34 is rotatably set on the preparation bracket 1, the bevel gear 2 35 is set on the grinding rotating rod 2 34, and the bevel gear 2 35 is meshed with the bevel gear 1 15. The bevel gear 36 is set on the grinding rotating rod 2 34, and the bevel gear 4 37 is set on the grinding rotating rod 1 32. The bevel gear 4 37 is meshed with the bevel gear 36. The feed hopper 38 is set on the preparation bracket 1, and the feed hopper 38 is connected to the conical crushing box 29.

[0111] Among them, each auxiliary mixing cylinder 16 is connected to a liquid inlet pipe 39, the liquid inlet pipe 39 passes through the preparation bracket 1, and a liquid inlet valve 40 is installed on the liquid inlet pipe 39, and the main mixing cylinder 5 and each auxiliary mixing cylinder 16 are connected to an air supply pipe 41, and an air supply valve 42 is installed on the air supply pipe 41.

[0112] Specifically, before the preparation stage, the gas delivery pipe 41 is connected to the argon gas storage tank, the liquid inlet pipe 39 is connected to the ultra-dry tetrahydrofuran solution storage tank, the feed hopper 38 is connected to the glove box, and finally the main discharge pipe 6 is connected to the in-situ passivation equipment, wherein the glove box, the argon gas storage tank, the ultra-dry tetrahydrofuran solution storage tank and the in-situ passivation equipment are all existing equipment for preparing magnesium hydride in the prior art, and are well known to those skilled in the art. The specific structure is not the main innovation point of the present application, and no excessive elaboration is given here.

[0113] When preparing nano magnesium hydride, magnesium chloride particles and lithium hydride particles are respectively added into the conical crushing box 29 through the corresponding glove box and the feed hopper 38, then the upper delivery valve 31 is opened, the lower delivery valve is closed, and the mixing motor 10 is started. The rotation of the mixing motor 10 drives the main mixing rod 9 to rotate, and the rotation of the main mixing rod 9 drives the bevel gear 15 to rotate, and the rotation of the bevel gear 15 drives the bevel gear 2 35 to rotate, and the rotation of the bevel gear 2 35 drives the grinding rotating rod 2 34 to rotate, and the rotation of the grinding rotating rod 2 34 drives the bevel gear 3 36 to rotate, and the rotation of the bevel gear 3 36 drives the bevel gear 4 37 to rotate, and the rotation of the bevel gear 4 37 drives the grinding rotating rod 1 32 to rotate, and the rotation of the grinding rotating rod 1 32 drives the conical grinding head 33 to rotate, and the magnesium chloride particles and lithium hydride particles in the conical crushing box 29 are crushed by the rotation of the conical grinding head 33, so that the crushed fragments fall into the material storage cavity, and then the upper delivery valve 31 is closed to store the crushed raw materials.

[0114] After the magnesium chloride particles and the lithium hydride particles are ground and prepared, the main mixing rod 9 is rotated to drive the mixing reciprocating screw rod 13 to rotate, and the rotation of the mixing reciprocating screw rod 13 drives the mixing ball nut group 14 to perform linear reciprocating motion, and the movement of the mixing ball nut group 14 drives the connecting frame to move, and the connecting frame drives the auxiliary mixing tube 19 to move, and the auxiliary mixing tube 19 drives the auxiliary partition plate 20 to move in the auxiliary mixing barrel 16. When the auxiliary partition plate 20 moves to one side of the crushed material delivery tube 30, the mixing motor 10 stops starting, and then the steering handle 26 is pulled upwards, and the hexagonal steering rod 24 is deformed in the hexagonal direction through the deformation of the limit spring 25. The steering handle 26 is then turned, and the rotation of the steering handle 26 drives the hexagonal steering rod 24 to rotate. The rotation of the hexagonal steering rod 24 drives the steering turn bar 23 to rotate, and the rotation of the steering turn bar 23 drives the one-way control plate 21 to rotate, so that the mixing through holes in the one-way control plate 21 and the auxiliary separation plate 20 are in a staggered state. At this time, the one-way control plate 21 and the auxiliary separation plate 20 will form a sealing plate, and then the steering handle 26 is released to insert the steering limit column 27 into the corresponding limit through hole to fix the position of the one-way control plate 21.

[0115] After fixing the position of the one-way control plate 21, start the mixing motor 10 again, and move the auxiliary partition plate 20 toward one side of the feed pipe 17 through the mixing ball nut group 14. When the auxiliary partition plate moves toward one side of the feed pipe 17, a vacuum area will be formed between the auxiliary partition plate 20 and the crushed material delivery pipe 30 in the auxiliary mixing barrel 16. Under the action of air pressure, the gas and liquid in the argon gas storage tank and the ultra-dry tetrahydrofuran solution storage tank will be transported to the auxiliary mixing barrel 16 through the gas pipe 41 and the liquid inlet pipe 39 respectively. In this process, by starting the lower delivery valve, a certain amount of crushed magnesium chloride particles or lithium hydride particles can be added to the auxiliary mixing barrel 16 at the same time, completing the scheme described in step 2.

[0116] When the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are stirred and mixed, first stop and start the mixing motor 10, and by turning the steering handle 26, make the one-way control plate 21 and the mixing through hole in the auxiliary partition plate 20 overlap, and start the mixing motor 10 again, so that the auxiliary partition plate 20 can reciprocate linearly in the auxiliary mixing barrel 16. During this process, the solution in the auxiliary mixing box passes through the mixing through hole, and the solution is stirred by the mixing rack 22 in the mixing through hole to mix the solution.

[0117] After the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are mixed and stirred, the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are discharged into the main mixing barrel 5 for reaction preparation, and the auxiliary partition plate 20 is moved to the side of the crushed material delivery pipe 30 again, and the steering handle 26 is turned to form a sealing plate between the one-way control plate 21 and the auxiliary partition plate 20, and then the feeding valve 18 is opened, and then the mixing motor 10 is started to make the crushed material delivery pipe 30 and the crushed material delivery pipe 30 be discharged. The auxiliary partition plate 20 moves toward the direction of the feeding pipe 17, and squeezes the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride in the auxiliary mixing barrel 16 into the main mixing barrel 5 through the corresponding feeding pipes 17. At the same time, the next batch of tetrahydrofuran solution of magnesium chloride and tetrahydrofuran suspension of lithium hydride can be added to the auxiliary mixing barrel 16 through the gas pipe 41, the liquid inlet pipe 39 and the crushed material delivery pipe 30 to carry out continuous processing of nano magnesium hydride.

[0118] It should be noted that, since the stirring time after magnesium chloride powder is added to tetrahydrofuran is set to 6 to 12 hours, the stirring time after lithium hydride powder is added to tetrahydrofuran is set to 0.5 to 1 hour, and the stirring time of the organic suspension is set to 1 to 2 hours, the auxiliary mixing mechanism 002 is set to eight groups as the best choice, six of which are used to stir magnesium chloride powder and tetrahydrofuran solution, one group is used to stir lithium hydride powder and tetrahydrofuran solution, and the other group is used for standby, so that uninterrupted continuous preparation of nano magnesium hydride can be achieved.

[0119] When the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride in the auxiliary mixing barrel 16 are respectively discharged into the main mixing barrel 5 through the corresponding feeding pipes 17, the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride are preferentially converged and collided on the mixing and evenly spreading baffle 12 for preliminary fusion. Then, after the tetrahydrofuran solution of magnesium chloride and the tetrahydrofuran suspension of lithium hydride enter the main mixing barrel 5, the rotation of the main mixing rod 9 will also drive the spiral mixing blade 11 to rotate, and the mixed liquid in the main mixing barrel 5 is stirred and mixed by the rotation of the spiral mixing blade 11. In the mixing process, the ultrasonic vibration rod 8 is intermittently started to provide energy by the cavitation effect generated by ultrasonic waves in the liquid, so as to promote the occurrence of the chemical reaction between magnesium chloride and lithium hydride.

[0120] During the ultrasonic process, as the ultrasonic time accumulates, the reaction degree of the reactants gradually increases, and the amount of nano magnesium hydride generated increases accordingly. However, as the energy in the organic medium accumulates, the temperature of the reaction system tends to increase, which will promote the growth of nanoparticles. The hydrogen absorption and desorption kinetics of the resulting product are attenuated. Similar to extending the ultrasonic time, excessive power will also cause excess energy, resulting in an increase in the system temperature and an increase in the product particles. Therefore, by starting the insulation mold temperature machine, constant temperature water enters the sealed insulation cavity through the liquid inlet insulation pipe 3 and is then discharged through the liquid outlet insulation pipe 4. The solution inside the main mixing barrel 5 is subjected to constant temperature treatment through heat exchange.

[0121] After the chemical reaction between magnesium chloride and lithium hydride is completed in the main mixing barrel 5, the main discharge valve 7 is opened, and argon gas is introduced into the main mixing barrel 5 through the gas pipe 41, and the reacted solution is squeezed into the in-situ passivation equipment, and 1‰ O2-Ar mixed gas is introduced into the mixed solution after the reaction to perform in-situ passivation. After a passivation time of 15-20 minutes, the nano magnesium hydride particles can be obtained by centrifugation and drying, and the supernatant after centrifugation is transferred to a solvent purification system, and the treated tetrahydrofuran is transferred to an ultra-dry tetrahydrofuran solution storage tank for recycling.

[0122] The above-mentioned operations of in-situ passivation and centrifugal drying of the solution after the reaction are common technical methods for preparing nano-magnesium hydride in the art. The specific preparation equipment and method are not the main innovation points of this application and will not be described in detail here.

[0123] It is further explained that the transmission electron microscope image, X-ray diffraction image, and temperature-dependent dehydrogenation mass spectrum of the nano-magnesium hydride prepared in this embodiment are as follows: Fig.11 , Fig.12 , Fig.13 As shown in the figure, it can be seen that nano magnesium hydride is relatively pure, with a particle size of about 10nm, an initial hydrogen desorption temperature of 50°C, a hydrogen desorption peak temperature of about 100°C, and has good hydrogen desorption kinetics.

[0124] Embodiments 3 to 5

[0125] The following Examples 3 to 5 prepare different nano magnesium hydride respectively, and the preparation process and preparation device are the same as those of Examples 1 and 2, and the only difference is that the parameters in the preparation process are different, as shown in the following table:

[0126]

[0127]

[0128] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A continuous preparation method of nano magnesium hydride, characterized in that: The following steps are involved: (a) preparing an implementation material, wherein the implementation material comprises magnesium chloride, lithium hydride and ultra-dry tetrahydrofuran; (b) in an argon gas atmosphere, respectively adding magnesium chloride and lithium hydride to tetrahydrofuran, and stirring to obtain a tetrahydrofuran solution in which magnesium chloride is completely dissolved and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, respectively, wherein the molar ratio of magnesium chloride to lithium hydride is 1:2; (c) in an argon gas atmosphere, stirring and mixing a tetrahydrofuran solution of magnesium chloride and a tetrahydrofuran suspension in which lithium hydride is uniformly dispersed, to obtain an organic suspension in which magnesium chloride and lithium hydride are uniformly mixed; (d) subjecting the organic suspension uniformly mixed with magnesium chloride and lithium hydride to constant temperature ultrasonic treatment in an argon gas atmosphere; (e) after the reaction is completed, the reaction product is in situ passivated, and then centrifuged and dried to obtain nano magnesium hydride particles; (f) The supernatant after centrifugation is transferred to a solvent purification system, and the treated tetrahydrofuran is transferred to a preparation device for recycling and continuous preparation of the next batch.

2. The continuous preparation method of nano magnesium hydride according to claim 1, characterized in that: In step (a), the magnesium chloride is anhydrous magnesium chloride; In step (b), before adding magnesium chloride and lithium hydride to tetrahydrofuran, magnesium chloride and lithium hydride need to be ground respectively to obtain magnesium chloride and lithium hydride powders. After adding magnesium chloride powder to tetrahydrofuran, the stirring time is set to 6 to 12 hours, and after adding lithium hydride powder to tetrahydrofuran, the stirring time is set to 0.5 to 1 hour; In step (c), the stirring time of the organic suspension is set to 1 to 2 hours; In step (d), the organic suspension is ultrasonically treated with an ultrasonic rod, the single ultrasonic time is 3 to 5 seconds, the interval time is 3 to 5 seconds, the cumulative ultrasonic time is 1 to 4 hours, and the ultrasonic constant temperature is 5 to 10°C.

3. A continuous preparation device for nano magnesium hydride, which refers to the continuous preparation method for nano magnesium hydride described in claim 2, and is used to implement steps (a) to (d), characterized in that: include: preparing a scaffold (1); A raw material insulation cylinder (2), wherein the raw material insulation cylinder (2) is arranged on the preparation support (1), and the two sides of the raw material insulation cylinder (2) are respectively connected with a liquid inlet insulation pipe (3) and a liquid outlet insulation pipe (4); A main mixing cylinder (5), the main mixing cylinder (5) being arranged in the raw material heat preservation cylinder (2), a sealed heat preservation cavity being formed between the main mixing cylinder (5) and the raw material heat preservation cylinder (2), a main discharge pipe (6) being connected at the bottom of the main mixing cylinder (5), the main discharge pipe (6) penetrating and sealingly arranged the raw material heat preservation cylinder (2) and the preparation support (1), and a main discharge valve (7) being installed on the main discharge pipe (6); An ultrasonic vibration rod (8), wherein a plurality of the ultrasonic vibration rods (8) are provided, and the plurality of ultrasonic vibration rods (8) are uniformly penetrated and sealed on the raw material insulation cylinder (2) and the main mixing cylinder (5); A main mixing mechanism (001), the main mixing mechanism (001) being arranged on the preparation support (1), and the main mixing mechanism (001) being penetrated and rotatably sealed inside the raw material heat preservation cylinder (2); An auxiliary mixing mechanism (002) having a crushing function, wherein a plurality of the auxiliary mixing mechanisms (002) are provided, the auxiliary mixing mechanism (002) is arranged on the preparation support (1), the auxiliary mixing mechanism (002) is sealed and connected to the raw material insulation cylinder (2), and the auxiliary mixing mechanism (002) is meshed with the main mixing mechanism (001).

4. A continuous preparation device for nano magnesium hydride according to claim 3, characterized in that: The main mixing mechanism (001) comprises: A main mixing rod (9), the main mixing rod (9) penetrates through and is rotatably arranged on the main mixing barrel (5); A mixing motor (10), the mixing motor (10) being mounted on the preparation support (1), the output end of the mixing motor (10) being connected to the main mixing rod (9); A spiral mixing blade (11), wherein the spiral mixing blade (11) is arranged on the main mixing rod (9), and the spiral mixing blade (11) is located in the main mixing barrel (5); a mixing evenly distributing baffle (12), wherein the mixing evenly distributing baffle (12) is arranged on the main mixing rod (9), and the mixing evenly distributing baffle (12) is located above the spiral mixing blade (11) in the main mixing barrel (5); A mixing reciprocating screw rod (13), the mixing reciprocating screw rod (13) being arranged on the main mixing rod (9), a mixing ball nut group (14) being threadedly connected to the mixing reciprocating screw rod (13), and the auxiliary mixing mechanism (002) being connected to the mixing reciprocating screw rod (13); Bevel gear one (15), the bevel gear one (15) is arranged on the main mixing rod (9), and the auxiliary mixing mechanism (002) is meshed with the bevel gear one (15).

5. A continuous preparation device for nano magnesium hydride according to claim 4, characterized in that: The auxiliary mixing mechanism (002) comprises: An auxiliary mixing cylinder (16), wherein the auxiliary mixing cylinder (16) is arranged on the preparation support (1); A feeding pipe (17), the feeding pipe (17) is arranged between the auxiliary mixing cylinder (16) and the main mixing cylinder (5) in an inclined sealed manner, and a feeding valve (18) is installed on the feeding pipe (17); An auxiliary mixing component with a segmented material discharging and storing function, the auxiliary mixing component is arranged through the auxiliary mixing barrel (16), and the auxiliary mixing component is connected to the mixing ball nut assembly (14); A crushing component, wherein the crushing component is arranged on the preparation support (1), the crushing component is connected to the auxiliary mixing box, and the crushing component is meshed with the bevel gear 1 (15).

6. A continuous preparation device for nano magnesium hydride according to claim 5, characterized in that: The auxiliary mixing component comprises: An auxiliary mixing tube (19), the auxiliary mixing tube (19) penetrates and is longitudinally sealed and slidably arranged on the auxiliary mixing cylinder (16), and the auxiliary mixing tube (19) is connected to the mixing ball nut assembly (14) via a connecting frame; an auxiliary separation plate (20), the auxiliary separation plate (20) being sealed and slidably disposed in the auxiliary mixing barrel (16), and the auxiliary separation plate (20) being connected to the auxiliary mixing tube (19); a one-way regulating plate (21), wherein one end of the auxiliary separation plate (20) away from the auxiliary mixing tube (19) is provided with a one-way regulating groove, wherein the one-way regulating plate (21) is sealed and rotatably disposed in the one-way regulating groove, wherein the one-way regulating plate (21) and the auxiliary separation plate (20) are both provided with a plurality of one-to-one corresponding mixing through holes, and a mixing rack (22) is disposed in each of the mixing through holes; A control plate steering portion having a self-locking function, the control plate steering portion is sealed and rotatably arranged in the auxiliary mixing tube (19), and the control plate steering portion is connected to the one-way control plate (21).

7. A continuous preparation device for nano magnesium hydride according to claim 6, characterized in that: The steering part of the control plate comprises: A steering rod (23), the steering rod (23) penetrates through and is sealed and rotatably arranged in the auxiliary mixing tube (19), one end of the steering rod (23) is connected to the one-way regulating plate (21), and the other end of the steering rod (23) is provided with a hexagonal limit regulating groove; A hexagonal steering rod (24), the hexagonal steering rod (24) penetrates and is slidably disposed in the hexagonal limit adjustment groove, and a limit spring (25) is disposed between the hexagonal steering rod (24) and the hexagonal limit adjustment groove; A steering handle (26), the steering handle (26) being arranged at one end of the hexagonal steering rod (24) away from the steering lever (23); A steering limit column (27), wherein the steering limit column (27) is arranged on the steering handle (26); A steering limit plate (28), wherein the steering limit plate (28) is arranged on the auxiliary mixing tube (19), a plurality of limit through holes are provided on the steering limit plate (28) at equal angles, and the steering limit column (27) is located in the corresponding limit through hole.

8. The continuous preparation device of nano magnesium hydride according to claim 7, characterized in that: The crushing component comprises: A conical crushing box (29), wherein the conical crushing box (29) is arranged on the preparation support (1); a crushed material delivery pipe (30), the crushed material delivery pipe (30) being arranged in communication between the conical crushed material box (29) and the auxiliary mixing cylinder (16), an upper delivery valve (31) and a lower delivery valve being installed on the crushed material delivery pipe (30), a material storage cavity being formed between the upper delivery valve (31) and the lower delivery valve; A grinding rotating rod (32), the grinding rotating rod (32) penetrates through and is rotatably disposed on the conical crushing box (29); A conical grinding head (33), wherein the conical grinding head (33) is arranged on the grinding rotating rod (32), the conical grinding head (33) is located in the conical crushing box (29), and a grinding cavity is formed between the conical grinding head (33) and the conical crushing box (29); A second grinding rotating rod (34), the second grinding rotating rod (34) being rotatably disposed on the preparation support (1); Bevel gear 2 (35), the bevel gear 2 (35) is arranged on the grinding rotating rod 2 (34), and the bevel gear 2 (35) is meshed with the bevel gear 1 (15); Bevel gear three (36), the bevel gear three (36) is arranged on the grinding rotating rod two (34); Bevel gear four (37), the bevel gear four (37) is arranged on the grinding rotating rod one (32), and the bevel gear four (37) is meshed with the bevel gear three (36); A feed hopper (38), wherein the feed hopper (38) is disposed on the preparation support (1) and is communicated with the conical crushing box (29).

9. A continuous preparation device for nano magnesium hydride according to claim 8, characterized in that: Each of the auxiliary mixing cylinders (16) is connected to a liquid inlet pipe (39), the liquid inlet pipe (39) passes through the preparation support (1), and a liquid inlet valve (40) is installed on the liquid inlet pipe (39).

10. The continuous preparation device of nano magnesium hydride according to claim 9, characterized in that: The main mixing cylinder (5) and each of the auxiliary mixing cylinders (16) are connected to an air supply pipe (41), and an air supply valve (42) is installed on the air supply pipe (41).

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