Method and device for preparing lithium hydride

Abstract

The invention discloses a method and device for preparing lithium hydride, and the device comprises a feeding table which is used for feeding raw materials; the discharging table is used for taking out the prepared lithium hydride; the hydrogenation reactor is used for synthesizing lithium hydride; a push rod is arranged on the feeding table, automatic operation of feeding and discharging is achieved through control of the push rod, then manual intervention is reduced, and production efficiency and safety are improved. The device is suitable for large-scale production of lithium hydride, and the prepared lithium hydride is high in quality.

Description

Technical Field

[0001] The invention belongs to the technical field of new energy materials and relates to a method and a device for preparing lithium hydride. Background Art

[0002] With the transformation of the global energy structure and the growing demand for clean energy, hydrogen energy, as an efficient and environmentally friendly energy form, has received widespread attention. In the storage and transportation of hydrogen energy, solid-state hydrogen storage material lithium hydride (LiH) has become a research hotspot due to its high hydrogen storage density, low hydrogen release temperature and good stability.

[0003] At present, the preparation methods of lithium hydride mainly include solution synthesis method, vapor deposition method and solid phase reaction method. The solution synthesis method is to dissolve metallic lithium in an organic solvent and then introduce hydrogen for reaction. This method reduces the reaction temperature and pressure to a certain extent, but the use of organic solvents brings environmental pollution and safety hazards. The vapor deposition method deposits lithium hydride on a substrate through a vapor phase reaction. This method can obtain high-purity lithium hydride, but the equipment is complex, the production efficiency is low, and it is difficult to achieve large-scale production. The solid phase reaction method mixes metallic lithium with a hydride (such as sodium hydride, potassium hydride, etc.) and generates lithium hydride by heating. The reaction conditions of this method are relatively mild, but the product particle size is difficult to control, and the cost of the hydride raw material is high.

[0004] In summary, the existing lithium hydride preparation method has certain limitations in large-scale production.

[0005] In order to meet market demand, reduce production costs, and improve the output and quality of lithium hydride, it is necessary to provide an efficient, environmentally friendly, and low-cost method for large-scale preparation of lithium hydride to promote the widespread application of hydrogen energy. Summary of the invention

[0006] In order to overcome the above problems, the inventors propose a method and device for preparing lithium hydride, the device comprising: a feed station for feeding raw materials; a discharge station for taking out the prepared lithium hydride; a hydrogenation reactor for synthesizing lithium hydride; a push rod is provided on the feed station, and the automatic operation of feeding and discharging is realized by controlling the push rod, thereby reducing manual intervention and improving production efficiency and safety. The device is suitable for large-scale production of lithium hydride, and the prepared product is of high quality, thereby completing the present invention.

[0007] Specifically, the purpose of the present invention is to provide the following aspects: In one aspect, a device for preparing lithium hydride is provided, the device comprising: A feeding table, which is used for feeding raw materials; A discharging platform, which is used to take out the prepared lithium hydride; A hydrogenation reactor for synthesizing lithium hydride; The feeding platform is provided with a push rod, and the automatic operation of feeding and discharging is realized by controlling the push rod at one end of the feeding platform.

[0008] Wherein, the hydrogenation reactor comprises: A first heating unit, which is used to provide heat for the lithium hydride reaction; A second heating unit, which is used to cooperate with the first heating unit to provide heat for the lithium hydride reaction; Wherein, the hydrogenation reactor further comprises a hydraulic cylinder, which is used to drive the opening and closing of the first heating unit.

[0009] Wherein, the hydraulic cylinder is connected between the first heating unit and the second heating unit.

[0010] Wherein, the hydrogenation reactor further comprises an exterior panel, which is arranged outside the second heating unit and is used for heat preservation and external heat insulation.

[0011] Wherein, the hydrogenation reactor further includes a translation unit, which is used to drive the translation of the first heating unit and the second heating unit.

[0012] Wherein, the hydrogenation reactor further comprises: A gas inlet, which is used to provide a desired reaction atmosphere; An air outlet is used for exhausting air.

[0013] Wherein, a material rack with rollers is arranged inside the second heating unit.

[0014] In a second aspect, a method for preparing lithium hydride using the device according to the first aspect is provided, wherein the method comprises: Step 1, placing a metal lithium ingot in a hydrogenation reactor using a feed station; Step 2, providing heat for the lithium hydride reaction through the first heating unit and the second heating unit of the hydrogenation reactor, and obtaining the lithium hydride through a hydrogenation synthesis reaction; Step 3, taking out the lithium hydride using a discharging platform.

[0015] In step 2, hydrogen is introduced into the hydrogenation reactor before the hydrogenation synthesis reaction.

[0016] The beneficial effects of the present invention include: (1) The device for preparing lithium hydride provided by the present invention adopts a material loading and unloading platform and a push rod, and the automated operation realizes fast and accurate material loading and unloading operation, reduces manual intervention, and improves production efficiency.

[0017] (2) The device for preparing lithium hydride provided by the present invention opens the first heating unit by back-pulling of a hydraulic cylinder, and uses an electric lead screw and a translation unit to quickly move the first heating unit and the second heating unit out of the heating area, so that the hydrogenation reactor can be cooled more quickly, thereby shortening the single batch production time.

[0018] (3) The device for preparing lithium hydride provided by the present invention is a normal pressure device, and the operating surface is completely separated from the operator, which improves the safety of operation and reduces the operation risk.

[0019] (4) The method for preparing lithium hydride provided by the present invention is suitable for large-scale production, and the product obtained is of high quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] By reading the detailed description of the preferred specific embodiments below, various other advantages and benefits of the present invention will become clear to those of ordinary skill in the art. The drawings in the specification are only used for the purpose of illustrating the preferred embodiments and are not considered to be limitations of the present invention. Obviously, the drawings described below are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative work.

[0021] In the attached picture: Figure 1 A schematic diagram showing the structure of the lithium hydride device of the present invention is shown; Figure 2 A side view of the structure of the hydrogenation reactor of the present invention is shown; Figure 3 The X-ray diffraction pattern of lithium hydride prepared in Example 1 is shown; Figure 4 The X-ray diffraction pattern of lithium hydride prepared in Example 2 is shown; Description of Reference Numerals 1-Feeding table; 2-Discharging table; 3-Hydrogenation reactor; 31-first heating unit; 32- second heating unit; 321-Material cavity; 33-Hydraulic cylinder; 331-Robotic arm; 332-piston rod; 34-exterior panel; 35- translation unit; 351- bottom plate; 352-support platform; 353-Supporting member; 354-first stopper; 355-second limiter; 36-circulating cooling water inlet; 37-circulating cooling water outlet; 38-air inlet; 39-air outlet; 30-Electric screw; 301- telescopic bracket; 302-Substrate; 303-driving rod; 304-roller; 305-connector; 306-supporting part; 311-feeding port; 312-discharging port; 313-semicircular inner top surface; 4-Putter. DETAILED DESCRIPTION

[0022] The following will refer to the attached Figures 1 to 4 Specific embodiments of the present invention are described in more detail. Although specific embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to enable a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art.

[0023] It should be noted that certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that technicians may use different nouns to refer to the same component. This specification and claims do not use the difference in nouns as a way to distinguish components, but use the difference in the functions of the components as the criterion for distinction. As mentioned throughout the specification and claims, "including" or "comprising" is an open term, so it should be interpreted as "including but not limited to". The subsequent description of the specification is a preferred embodiment of the present invention, but the description is based on the general principles of the specification and is not intended to limit the scope of the present invention. The scope of protection of the present invention shall be determined by the attached claims.

[0024] In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", etc. indicate positions or positional relationships based on the working state of the present invention, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", "third", and "fourth" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0025] To facilitate understanding of the embodiments of the present invention, further explanation will be given below by taking specific embodiments as examples in conjunction with the accompanying drawings, and each of the accompanying drawings does not constitute a limitation on the embodiments of the present invention.

[0026] On the one hand, according to a device for preparing lithium hydride provided by the present invention, Figure 1 As shown, the device comprises: A feeding platform 1, which is used for feeding raw materials; A discharging station 2, which is used to take out the prepared lithium hydride; A hydrogenation reactor 3, which is used to synthesize lithium hydride; In the present invention, a push rod 4 is provided on the feed table 1, and the automatic operation of feeding and discharging is realized through the control of the push rod 4, thereby reducing manual intervention and improving production efficiency and safety.

[0027] In the present invention, the feed station 1 and the discharge station 2 are arranged at both ends of the hydrogenation reactor 3 for rapid feeding and discharging of materials, and the arrangement of the push rod 4 is the key to solving the large-scale feeding and discharging of materials. When in use, the feed station 1 with the push rod 4 is connected to the hydrogenation reactor 3, the material boat with the lithium ingot is placed in the reserved pushing position of the feed station 1, the push rod 4 of the feed station 1 is turned on, and the push rod 4 works to push the material boat into the hydrogenation reactor 3. For safety and manpower saving, the push rod 4 is preferably electric.

[0028] In the present invention, if Figure 2 As shown, the hydrogenation reactor 3 comprises: A first heating unit 31, which is used to provide heat for the lithium hydride reaction; A second heating unit 32, which is used to cooperate with the first heating unit 31 to provide heat for the lithium hydride reaction; The material chamber 321 is used for lithium hydride reaction; A hydraulic cylinder 33, which is used to drive the first heating unit 31 to open and close; An outer decorative plate 34 is disposed outside the first heating unit 31 and the second heating unit 32 and is used for heat preservation and external heat insulation; An electric lead screw 30, which is used to drive the first heating unit 31 and the second heating unit 32 to rise and fall; A translation unit 35, which is used to drive the first heating unit 31 and the second heating unit 32 to move in a horizontal direction; A circulating cooling water inlet 36, which is used to provide a cooling water source; A circulating cooling water outlet 37, which is used to discharge circulating cooling water; An air inlet 38 for providing a desired reaction atmosphere; An air outlet 39 for exhausting air; A feed port 311, which is used for feeding; The material discharging port 312 is used for discharging materials.

[0029] In the present invention, if Figure 2 As shown, the first heating unit 31 is provided with a semicircular inner top surface 313, and the semicircular inner top surface 313 can be buckled to the upper surface of the material cavity 321; the second heating unit 32 is also provided with a semicircular curved surface for buckling to the lower surface of the material cavity 321. When the lithium hydride reaction is carried out, the material cavity 321 is clamped between the first heating unit 31 and the second heating unit 32. At this time, the first heating unit 31 and the second heating unit 32 are closely connected to provide uniform heat for the reaction materials in the material cavity 321.

[0030] In the present invention, a material rack with rollers is provided in the material cavity 321 , and the rollers have a rotation function to facilitate the entry and exit of the material boat in the material cavity 321 .

[0031] Furthermore, the material cavity 321 can be any one of a column, a prism, and a cube, preferably a column that is easy to process and industrially operate. In this case, the columnar material cavity 321 fits more closely with the first heating unit 31 and the second heating unit 32, that is, the heating effect is better.

[0032] In the present invention, the first heating unit 31 is movably arranged on the second heating unit 32, and preferably the first heating unit 31 and the second heating unit 32 are connected by a hinge to facilitate the opening and closing of the first heating unit 31. During operation, the two are closely connected in the heating area; after the reaction is completed, the first heating unit 31 is opened, and the first heating unit 31 and the second heating unit 32 are moved out from the periphery of the material cavity 321, that is, the material cavity 321 is away from the heat source to achieve rapid cooling.

[0033] In the present invention, the hydraulic cylinder 33 is connected between the first heating unit 31 and the second heating unit 32, and is specifically arranged on the hinge connection side of the first heating unit 31 and the second heating unit 32. The hydraulic cylinder 33 includes a mechanical arm 331 and a piston rod 332, and the first heating unit 31 is connected to the lower end of the second heating unit 32 through the mechanical arm 331 and the piston rod 332 in turn, and the mechanical arm 331 and the piston rod 332 are hingedly connected. When the first heating unit 31 is closed above the second heating unit 32, the piston rod 332 is parallel to the hinge axis. When working, the piston rod 332 of the hydraulic cylinder 33 is extended and retracted, pushing or pulling the first heating unit 31 to rotate around the hinge axis, thereby controlling the opening and closing of the first heating unit 31 above the second heating unit 32. The hydraulic cylinder 33 also realizes the close docking of the first heating unit 31 and the second heating unit 32 during the reaction process, providing uniform heat distribution.

[0034] In the present invention, an electric screw 30 is provided at the bottom of the second heating unit 32. The electric screw 30 includes a telescopic bracket 301 and a base plate 302. The telescopic bracket 301 is composed of at least two telescopic rods, and the telescopic rods can be telescoped in the vertical direction. By adjusting the telescopic bracket 301, the height adjustment between the first heating unit 31 and the second heating unit 32 is achieved to meet the use requirements under different working conditions. A connecting piece 305 is provided at the top of the telescopic bracket 301 for fixed connection with the bottom of the second heating unit 32; a supporting part 306 is provided at the bottom of the telescopic bracket 301 for fixed connection with the base plate 302.

[0035] Furthermore, the telescopic brackets 301 are preferably 4 in number, with 2 telescopic brackets 301 as a group, that is, the 2 groups of telescopic brackets 301 are symmetrically distributed at the bottom of the second heating unit 32, and a driving rod 303 is provided at the lower position between each group of telescopic brackets 301, and the driving rod 303 is connected to the driver, and the telescopic bracket 301 is driven by the driving rod 303, thereby driving the first heating unit 31 and the second heating unit 32 to rise and fall smoothly.

[0036] Further, the substrate 302 is arranged below the bracket 301, and the substrate 302 is used to provide support for the bracket 301. Preferably, a roller 304 is provided at the bottom of the substrate 302, and the roller 304 enables the substrate 302 to translate on the translation unit 35, thereby realizing the overall translation of the electric lead screw 30 and the first heating unit 31 and the second heating unit 32 thereon.

[0037] In the present invention, the translation unit 35 is arranged at the bottom of the electric lead screw 30, and the translation unit 35 includes a bottom plate 351 and a support platform 352, and the bottom plate 351 is located below the support platform 352 and close to one end of the electric lead screw 30. The length of the support platform 352 is about 2 to 3 times the length of the bottom plate 351, and the bottom plate 351 is used to provide support for part of the support platform 352 and the electric lead screw 30, the first heating unit 31, and the second heating unit 32 above the support platform 352. A plurality of support members 353 are arranged below the portion not supported by the bottom plate 351, for example, two support members 353 are arranged, and the specific number of the support members 353 is flexibly set according to the length of the support platform 352.

[0038] Furthermore, the translation unit 35 further includes a first stopper 354 and a second stopper 355, wherein the first stopper 354 is located at the end of the roller 304 of the electric lead screw 30 above the support platform 352, and the second stopper 355 is located at the end above the support platform 352 away from the electric lead screw 30. The first stopper 354 and the second stopper 355 prevent the electric lead screw 30 from exceeding a predetermined movement range.

[0039] In the present invention, during the reaction, the first heating unit 31 and the second heating unit 32 are closely connected to provide the heat required for the reaction. After the reaction is completed, the hydraulic cylinder 33 opens the first heating unit 31 in a back-pulling manner, and the first heating unit 31 and the second heating unit 32 are moved out of the heating area by using the translation unit 35 and the electric screw 30, so that the hydrogenation reactor 3 is quickly cooled down.

[0040] In the present invention, the exterior panel 34 is arranged outside the first heating unit 31 and the second heating unit 32, the bottom of the inner wall of the exterior panel 34 abuts against the first limiter 354, and a certain gap is reserved between the exterior panel 34 and the first heating unit 31 and the second heating unit 32.

[0041] In the present invention, one end of the material cavity 321 is closely connected to the feed port 311, and the other end is closely connected to the discharge port 312, and the inner diameters of the feed port 311 and the discharge port 312 are consistent with the inner diameter of the material cavity 321. Further, the feed port 311 and the push rod 4 of the feed platform 1 are located at the same horizontal position, which facilitates the push rod 4 to transport the material to the material rack of the hydrogenation reactor 3 through the feed port 311; the discharge port 312 and the discharge platform 2 are located at the same horizontal position, which facilitates the material to be removed from the material rack of the hydrogenation reactor 3 through the discharge port 312.

[0042] In the present invention, the circulating cooling water inlet 36 and the circulating cooling water outlet 37 include two groups, one group of circulating cooling water inlet 36 and circulating cooling water outlet 37 is arranged at the sealing flange of the feed port 311, and the other group of circulating cooling water inlet 36 and circulating cooling water outlet 37 is arranged at the sealing flange of the discharge port 312. The circulating cooling water is rapidly cooled through the circulating cooling pipe between the circulating cooling water inlet 36 and the circulating cooling water outlet 37.

[0043] In the present invention, the air inlet 38 is arranged on one side of the feed port 311, and the air outlet 39 is arranged on one side of the discharge port 312. The air inlet 38 and the air outlet 39 as well as the circulating cooling water inlet 36 and the circulating cooling water outlet 37 respectively have independent operation systems.

[0044] Before the reaction, the feed station 1 and the discharge station 2 are docked and fixed to the two ends of the hydrogenation reactor 3, and the lithium ingot is placed on the material boat, which is placed at the push position of the push rod 4 of the feed station 1. The push rod 4 of the feed station 1 delivers the lithium ingot to the material cavity 321, and the empty material boat is moved out to the discharge station 2 through the discharge port 312. Then, the feed station 1 and the discharge station 2 are moved out of the docking position, and the feed port 311 and the discharge port 312 are closed. Since the telescopic bracket 301 on the electric screw 30 can be telescoped in the vertical direction, the material cavity 321 is evenly heated between the first heating unit 31 and the second heating unit 32.

[0045] During the reaction, the feed port 311 and the discharge port 312 are closed, and the first heating unit 31 and the second heating unit 32 are closely connected to provide uniform heat for the reaction.

[0046] After the reaction is finished, the hydraulic cylinder 33 opens the first heating unit 31 by back-pulling, and uses the translation unit 35 and the electric lead screw 30 to move the first heating unit 31 and the second heating unit 32 out of the heating area to the part not supported by the bottom plate 351. When the material chamber 321 drops to room temperature, the feed table 1 and the discharge table 2 are docked and fixed to the two ends of the material chamber 321 respectively, and the push rod 4 of the feed table 1 is used to move the product lithium hydride to the discharge table 2, and then the feed table 1 and the discharge table 2 are moved out of the docking position, and the feed port 311 and the discharge port 312 are closed.

[0047] On the other hand, according to the present invention, a method for preparing lithium hydride using the device according to the first aspect is provided, the method comprising: Step 1, placing a metal lithium ingot in a hydrogenation reactor 3 using a feed station 1; Step 2, providing heat for the lithium hydride reaction through the first heating unit 31 and the second heating unit 32 of the hydrogenation reactor 3, and obtaining the lithium hydride through a hydrogenation synthesis reaction; Step 3, using the discharging platform 2 to take out the lithium hydride.

[0048] The above method is described in detail below.

[0049] Step 1: placing a metal lithium ingot into a hydrogenation reactor 3 using a feed station 1.

[0050] In step 1, the feed platform 1 and the discharging platform 2 are respectively docked and fixed to the two ends of the hydrogenation reactor 3, and the lithium ingot is placed on the material boat, which is placed on the pushing position of the push rod 4 of the feed platform 1. The push rod 4 of the feed platform 1 delivers the metallic lithium to the material rack of the material chamber 321 through the feed port 311. With the help of the rotation function of the roller equipped on the material rack, the empty material boat is moved out to the discharging platform 2 through the discharging port 312, and then the feed platform 1 and the discharging platform 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0051] Step 2, providing heat for the lithium hydride reaction through the first heating unit 31 and the second heating unit 32 of the hydrogenation reactor 3, and obtaining the lithium hydride through a hydrogenation synthesis reaction.

[0052] In step 2, before the hydrogenation synthesis reaction, the air is exhausted through the gas outlet 39 of the hydrogenation reactor 3; and the inert gas such as argon is replaced through the gas inlet 38, and the air is evacuated again to -0.008~-0.1Mpa, such as -0.098Mpa; then hydrogen is introduced through the gas inlet 38 to make the pressure slightly positive.

[0053] In step 2, the hydrogenation synthesis reaction is achieved in stages, including: The first stage: heating from room temperature to 300~400℃ at a heating rate of 5~15℃ / min, and keeping warm for 20~40min; The second stage: heating from the first stage holding temperature to 700-800°C at a heating rate of 5-15°C / min, and keeping the temperature for 10-40 minutes; The third stage: the temperature is naturally lowered to 250-350°C, the first heating unit 31 is turned on, and the temperature is further lowered to room temperature.

[0054] Among them, the appropriate heating rate is selected according to the melting speed of lithium. The purpose of insulation is to ensure that the metallic lithium is fully melted under high temperature conditions to prevent the unsynthesized lithium hydride from wrapping the unmelted metallic lithium, thereby affecting the product quality. Heating the temperature in stages can improve the quality of the produced lithium hydride.

[0055] In the present invention, in the third stage, water flows in the circulating cooling water inlet 36 and the circulating cooling water outlet 37 and naturally cools down to 250-350°C, and then the first heating unit 31 is opened by back-traction by the hydraulic cylinder 33, and the first heating unit 31 and the second heating unit 32 are moved out of the heating area by the translation unit 35 and the electric screw 30.

[0056] In a further preferred embodiment, the hydrogenation synthesis reaction comprises: The first stage: heating from room temperature to 340~360℃ at a heating rate of 7~12℃ / min, and keeping warm for 30~35min; The second stage: heating from the first stage holding temperature to 740-760°C at a heating rate of 7-12°C / min, and keeping the temperature for 20-30 minutes; The third stage: the temperature is naturally lowered to 280-310°C, the first heating unit 31 is turned on, and the temperature is further lowered to room temperature.

[0057] In a further preferred embodiment, the hydrogenation synthesis reaction comprises: The first stage: heating from room temperature to 350°C at a heating rate of 10°C / min and keeping the temperature for 30 minutes; The second stage: the temperature was raised from the first stage holding temperature to 750°C at a heating rate of 10°C / min and kept at this temperature for 20 minutes; The third stage: the temperature is naturally lowered to 300° C., the first heating unit 31 is turned on, and the temperature is further lowered to room temperature.

[0058] In the present invention, hydrogen is continuously introduced into the material chamber 321 during the hydrogenation synthesis reaction (the first stage and the second stage), and the gas replenishment rate is 5-108.5m 3 / h, preferably 8~98.5m3 / h, for example 8.5m 3 / h.

[0059] In the present invention, since there may be unreacted hydrogen in the material chamber 321 after the reaction is completed, for safety reasons, before opening the first heating unit 31, it is preferred to replace the hydrogen in the material chamber 321 with an inert gas such as argon, so that the hydrogen content in the material chamber 321 is reduced to less than 0.4%. More specifically, before opening the first heating unit 31, an inert gas such as argon is added in advance through the air inlet 38 to balance the pressure in the material chamber 321 or to form a slightly positive pressure; then the air outlet 39 is opened and argon is continuously introduced to replace the hydrogen in the material chamber 321, so that the hydrogen content in the material chamber 321 is reduced to less than 0.4%.

[0060] Step 3, using the discharging platform 2 to take out the lithium hydride.

[0061] In step 3, the feed table 1 and the discharging table 2 are respectively docked and fixed to the two ends of the material chamber 321, and the push rod 4 of the feed table 1 is used to send the empty material boat to the material rack of the material chamber 321 through the feed port 311. With the help of the rotation function of the roller equipped with the material rack, the product lithium hydride and the material boat are moved out to the discharging table 2 through the discharging port 312. Then, the feed table 1 and the discharging table 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0062] The present invention is further described below through specific examples, but these examples are merely exemplary and do not constitute any limitation to the scope of protection of the present invention.

[0063] Example 1 The feed platform 1 and the discharging platform 2 are respectively docked and fixed to the two ends of the hydrogenation reactor 3, and a 4.35 kg metal lithium ingot is placed on the material boat, which is placed on the pushing position of the push rod 4 of the feed platform 1. The push rod 4 of the feed platform 1 delivers the metal lithium to the material rack of the material cavity 321 through the feed port 311. With the help of the rotation function of the roller equipped on the material rack, the empty material boat is moved out to the discharging platform 2 through the discharging port 312. Then, the feed platform 1 and the discharging platform 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0064] The gas outlet 39 of the hydrogenation reactor 3 is evacuated to exhaust the air, and argon is introduced through the gas inlet 38, and the vacuum is again evacuated to -0.098Mpa, and hydrogen is introduced through the gas inlet 38 to make the pressure slightly positive. The sintering procedure of the first heating unit 31 and the second heating unit 32 of the hydrogenation reactor 3 is set as follows: The first stage: heating from 25°C to 350°C at a heating rate of 10°C / min, and keeping warm for 30 minutes; The second stage: heating from 350°C to 750°C at a heating rate of 10°C / min and keeping the temperature for 20 minutes; The third stage: water flows in the circulating cooling water inlet 36 and the circulating cooling water outlet 37, and the temperature naturally drops to 300°C. At this time, the first heating unit 31 is opened at 45° by the back-pulling method of the hydraulic cylinder 33, and the first heating unit 31 and the second heating unit 32 are moved out of the heating area by the translation unit 35 and the electric screw 30, and the temperature continues to drop to normal temperature.

[0065] In the first and second stages, the hydrogenation synthesis reaction continued by introducing hydrogen into the feed chamber 321 through the gas inlet 38 at a gas supply rate of 8.5 m / s. 3 / h; before opening the first heating unit 31, argon gas is first added through the air inlet 38 to make the pressure in the material chamber 321 slightly positive; then the air outlet 39 is opened and argon gas is continuously introduced through the air inlet 38 to replace the hydrogen in the material chamber 321, so that the hydrogen content in the material chamber 321 is reduced to less than 0.4%.

[0066] When the temperature drops to room temperature, the feed table 1 and the discharging table 2 are respectively docked and fixed to the two ends of the material chamber 321, and the push rod 4 of the feed table 1 is used to send the empty material boat to the material rack of the material chamber 321 through the feed port 311. With the help of the rotation function of the roller equipped with the material rack, the product lithium hydride and the material boat are moved out to the discharging table 2 through the discharging port 312. Then, the feed table 1 and the discharging table 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0067] The shape of the product taken out basically maintains the shape of the metal lithium ingot when the material was added, and some lithium hydride is melted and condensed into blocks. According to the product scale, it is crushed, ground and screened by mechanical means, and finally packaged into finished products. The obtained lithium hydride X-ray diffraction pattern is as follows Figure 3 As shown, it can be seen that it completely corresponds to the standard PDF74-1153 card of LiH, indicating that lithium hydride has been successfully prepared in batches; and no characteristic diffraction peak of metallic Li is found in the X-ray diffraction spectrum, indicating that complete hydrogenation of metallic lithium has been achieved.

[0068] Example 2 Lithium hydride was prepared in a similar manner to Example 1, except that 43.5 kg of lithium metal ingot was used. Specifically: The feed platform 1 and the discharging platform 2 are respectively docked and fixed to the two ends of the hydrogenation reactor 3, and a 43.5 kg metal lithium ingot is placed on the material boat, which is placed on the pushing position of the push rod 4 of the feed platform 1. The push rod 4 of the feed platform 1 delivers the metal lithium to the material rack of the material cavity 321 through the feed port 311. With the help of the rotation function of the roller equipped on the material rack, the empty material boat is moved out to the discharging platform 2 through the discharging port 312. Then, the feed platform 1 and the discharging platform 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0069] The gas outlet 39 of the hydrogenation reactor 3 is evacuated to exhaust the air, and argon is introduced through the gas inlet 38, and the vacuum is again evacuated to -0.098Mpa, and hydrogen is introduced through the gas inlet 38 to make the pressure slightly positive. The sintering procedure of the first heating unit 31 and the second heating unit 32 of the hydrogenation reactor 3 is set as follows: The first stage: heating from 25°C to 350°C at a heating rate of 10°C / min, and keeping warm for 30 minutes; The second stage: heating from 350°C to 750°C at a heating rate of 10°C / min and keeping the temperature for 20 minutes; The third stage: water flows in the circulating cooling water inlet 36 and the circulating cooling water outlet 37, and the temperature naturally drops to 300°C. The first heating unit 31 is opened at 45° by the back-pulling method of the hydraulic cylinder 33, and the first heating unit 31 and the second heating unit 32 are moved out of the heating area by the translation unit 35 and the electric screw 30, and the temperature continues to drop to normal temperature.

[0070] In the first and second stages, the hydrogenation synthesis reaction continued by introducing hydrogen into the feed chamber 321 through the gas inlet 38 at a gas supply rate of 8.5 m / s. 3 / h; before opening the first heating unit 31, argon gas is first added through the air inlet 38 to make the pressure in the material chamber 321 slightly positive; then the air outlet 39 is opened and argon gas is continuously introduced through the air inlet 38 to replace the hydrogen in the material chamber 321, so that the hydrogen content in the material chamber 321 is reduced to less than 0.4%.

[0071] When the temperature drops to room temperature, the feed platform 1 and the discharging platform 2 are respectively docked and fixed to the two ends of the hydrogenation reactor 3, and the push rod 4 of the feed platform 1 is used to send the empty boat to the material rack of the material chamber 321 through the feed port 311. With the help of the rotation function of the roller equipped with the material rack, the product lithium hydride and the boat are moved out to the discharging platform 2 through the discharging port 312. Then, the feed platform 1 and the discharging platform 2 are moved out of the docking position, and the feed port 311 and the discharging port 312 are closed.

[0072] The shape of the product taken out basically maintains the shape of the metal lithium ingot when the material was added, and some lithium hydride is melted and condensed into blocks. According to the product scale, it is crushed, ground and screened by mechanical means, and finally packaged into finished products. The obtained lithium hydride X-ray diffraction pattern is as follows Figure 4 As shown, it can be seen that it completely corresponds to the standard PDF74-1153 card of LiH, indicating that lithium hydride has been successfully prepared in batches; and no characteristic diffraction peak of metallic Li is found in the X-ray diffraction spectrum, indicating that complete hydrogenation of metallic lithium has been achieved.

[0073] The present invention is described in detail above in combination with preferred embodiments and exemplary examples. However, it should be noted that these specific embodiments are only illustrative explanations of the present invention and do not constitute any limitation on the protection scope of the present invention. Without exceeding the spirit and protection scope of the present invention, various improvements, equivalent substitutions or modifications may be made to the technical content of the present invention and its embodiments, which all fall within the protection scope of the present invention. The protection scope of the present invention shall be subject to the attached claims.

Claims

1. A device for preparing lithium hydride, characterized in that: The device comprises: A feeding platform (1) for feeding raw materials; A discharging platform (2) for taking out the prepared lithium hydride; A hydrogenation reactor (3) for synthesizing lithium hydride; The feed table (1) is provided with a push rod (4), and automatic operation of feeding and discharging is achieved through the control of the push rod (4) at one end of the feed table (1).

2. The device according to claim 1, characterized in that Preferably, the hydrogenation reactor (3) comprises: A first heating unit (31), which is used to provide heat for the lithium hydride reaction; The second heating unit (32) is used to cooperate with the first heating unit (31) to provide heat for the lithium hydride reaction.

3. The device according to claim 1, characterized in that The hydrogenation reactor (3) further comprises a hydraulic cylinder (33) which is used to drive the opening and closing of the first heating unit (31).

4. The device according to claim 1, characterized in that The hydraulic cylinder (33) is connected between the first heating unit (31) and the second heating unit (32).

5. The device according to claim 1, characterized in that The hydrogenation reactor (3) further comprises an exterior panel (34), which is arranged outside the first heating unit (31) and the second heating unit (32) and is used for heat preservation and external heat insulation.

6. The device according to claim 1, characterized in that The hydrogenation reactor (3) further comprises a translation unit (35) for driving the translation of the first heating unit (31) and the second heating unit (32).

7. The device according to claim 1, characterized in that The hydrogenation reactor (3) further comprises: An air inlet (38) for providing a desired reaction atmosphere; An air outlet (39) is used for exhausting air.

8. The device according to claim 1, characterized in that A material rack with rollers is arranged inside the second heating unit (32).

9. The method for preparing lithium hydride according to any one of claims 1 to 7, characterized in that: The method comprises: Step 1, placing a metal lithium ingot in a hydrogenation reactor (3) using a feed station (1); Step 2, providing heat for the lithium hydride reaction through the first heating unit (31) and the second heating unit (32) of the hydrogenation reactor (3), and obtaining the lithium hydride through a hydrogenation synthesis reaction; Step 3, using the discharging platform (2) to take out the lithium hydride.

10. The method according to claim 8, characterized in that In step 2, hydrogen is introduced into the hydrogenation reactor (3) before the hydrogenation synthesis reaction.

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