Solid metal hydride preparation device and method

Abstract

The invention discloses a solid metal hydride preparation device and method.In the solid metal hydride preparation device, a premixing tank comprises a feeding port used for inputting solid metal powder, a solvent and a catalyst, a stirrer used for stirring the solid metal powder, the solvent and the catalyst and a discharging port used for guiding out a mixture; the reaction kettle is communicated with the premixing tank, the filtering vacuum drying system is connected with the reaction kettle, the jacket at least partially wraps the vacuum shell so as to heat the vacuum shell to a preset temperature, and the stirrer is vertically and rotatably connected into the vacuum shell and comprises a helical ribbon and a scraper; the filter screen is arranged in the shell and surrounds the stirrer to separate the solid metal hydride from the reactant, and the solvent and the catalyst return to the premixing tank from the filtrate outlet.

Description

Technical Field

[0001] The present invention relates to the technical field of new energy solid-state hydrogen storage materials, and in particular to a device and method for preparing solid metal hydrides. Background Art

[0002] Metal hydrides, as solid-state hydrogen storage materials used in the new energy sector, have attracted considerable attention for their preparation processes. Sodium aluminum hydride and lithium aluminum hydride are common examples of these metal hydrides. With the continuous advancement of research, these two materials have evolved from traditional organic reducing agents to become the newest and most researched hydrogen storage materials.

[0003] Sodium aluminum hydride is a complex metal hydride with the molecular formula NaAlH4. Shen Banwen and Che Yunxia of Nankai University detailed a synthesis method for sodium aluminum hydride in China ZL89108190. The reaction can be divided into two steps: the first step is the hydrogenation of metallic sodium, as shown in the following reaction equation:

[0004] 2Na(s)+H2(g)→2NaH(s),

[0005] In the reaction formula, s represents a solid and g represents a gas. The reaction conditions for the first step are normal temperature and pressure. The catalysts used are naphthalene and titanium tetrachloride, and the reaction is carried out in tetrahydrofuran. The second step is the reaction of sodium hydride and aluminum trichloride. The reaction equation is as follows:

[0006] 4NaH+AlCl3→NaAlH4+3NaCl,

[0007] The reaction conditions of the second step reaction are room temperature and the reaction is carried out in tetrahydrofuran. Some processing steps are required between the first and second steps.

[0008] The above method for preparing sodium aluminum hydride is suitable for synthesizing sodium aluminum hydride in the laboratory, and needs to be carried out step by step, the steps are complicated, and it is not suitable for large-scale production in a factory.

[0009] Lithium aluminum hydride is a complex metal hydride with the molecular formula LiAlH4. Lithium aluminum hydride is a white solid, but industrial products are usually gray powders due to impurities. In 1947, HISchlesinger, A.C. Bond, and A.E. Finholt first prepared lithium aluminum hydride by reacting lithium hydride with anhydrous aluminum chloride in diethyl ether:

[0010] 4LiH+AlCl3-Et2O→LiAlH4+3LiCl

[0011] This reaction, commonly known as the Schlesinger reaction, has a yield of 86% based on aluminum chloride. A small amount of lithium aluminum hydride must be added as an initiator at the start of the reaction; otherwise, the reaction requires an induction period before it can occur. Once initiated, the reaction proceeds at a rapid rate, making accidents more likely. However, this method is relatively simple and remains the primary method for producing lithium aluminum hydride.

[0012] The above method for preparing lithium aluminum hydride is suitable for synthesizing lithium aluminum hydride in the laboratory. However, due to the large amount of heat of formation released, it is only suitable for small-batch production and not suitable for large-scale production in factories. The conversion rate of lithium in the lithium aluminum hydride conversion product, lithium aluminum hydride, is only 25%, which is a low conversion rate.

[0013] The above information disclosed in this Background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known to a person of ordinary skill in the art. Summary of the Invention

[0014] In view of the problems existing in the prior art, the present invention proposes a solid metal hydride preparation device and method, which is suitable for producing a variety of solid metal hydrides and industrial mass production using a one-step process.

[0015] The purpose of the present invention is achieved through the following technical solutions: a solid metal hydride preparation device comprising:

[0016] A premixing tank comprising an inlet for inputting solid metal powder, solvent and catalyst, an agitator for stirring the solid metal powder, solvent and catalyst, and an outlet for discharging the mixture;

[0017] A reactor connected to the premixing tank, the reactor comprising:

[0018] The kettle body includes a first inlet connected to the discharge port, a second inlet for introducing metal liquid, a third inlet for introducing hydrogen, and an outlet for discharging reactants generated by the reaction in the kettle body, wherein the reactants include solid metal hydride, solvent, and catalyst.

[0019] a stirring device for stirring the mixture from the first inlet and the metal liquid,

[0020] A first temperature regulating device is connected to the kettle body to adjust to a first reaction temperature,

[0021] A pressure regulating device, which regulates the reaction pressure in the kettle;

[0022] A filtration vacuum drying system is connected to the reactor, and the filtration vacuum drying system includes:

[0023] A filter vacuum dryer comprising,

[0024] The vacuum housing includes an inlet connected to the discharge port for introducing reactants, an exhaust port for discharging solvent vapor, and a filtrate outlet connected to the feed port.

[0025] a jacket at least partially surrounding the vacuum housing to heat the vacuum housing to a predetermined temperature,

[0026] A stirrer is vertically rotatably connected to the vacuum housing, and the stirrer includes a spiral ribbon and a scraper.

[0027] A filter is arranged in the shell and surrounds the stirrer to separate the solid metal hydride from the reactants. The solvent and the catalyst are returned to the premixing tank from the filtrate outlet.

[0028] In the solid metal hydride preparation device, the filtration vacuum drying system further comprises:

[0029] A primary condenser connected to the exhaust port to condense the solvent vapor to obtain solvent liquid,

[0030] A gas-liquid separation tank connected to the primary condenser to separate the solvent liquid from the solvent vapor,

[0031] Vacuum pump, which is connected to the gas-liquid separation tank to reduce the system pressure before the pump,

[0032] The secondary condenser is connected to a vacuum pump to introduce solvent vapor.

[0033] An activated carbon adsorption tank is connected to the secondary condenser to adsorb the uncondensed solvent vapor.

[0034] The solid metal hydride preparation device further includes:

[0035] A reaction tank connected to the outlet for introducing reactants, the reaction tank comprising:

[0036] The separation part separates the solid metal hydride from the reactants by static gravity.

[0037] The reaction part includes an input port for inputting materials and a stirring unit, wherein the input materials and the solid metal hydride generate a second solid metal hydride solution in the reaction part.

[0038] a second temperature regulating device connected to the reaction part to regulate the reaction temperature to a second reaction temperature;

[0039] A flat filter is connected to the reaction tank and the inlet to filter and obtain a second solid metal hydride solution, which is then fed into a filter vacuum dryer as a reactant.

[0040] In the solid metal hydride preparation device, the premixing tank, the reaction kettle and the filtering vacuum drying system are all provided with nitrogen purge pipelines.

[0041] In the solid metal hydride preparation device, the filter screen comprises a metal sintered filter screen, and the pore size of the filter screen is 5-20 μm.

[0042] In the solid metal hydride preparation device, the first temperature regulating device includes a heater, the second temperature regulating device includes a cooler, and the first temperature regulating device and the second temperature regulating device are controlled by PID.

[0043] In the solid metal hydride preparation device, the pressure regulating device includes an electric regulating valve.

[0044] The preparation method of the solid metal hydride preparation device comprises the following steps:

[0045] Aluminum powder, solvent, and catalyst are weighed and placed in a premix tank and stirred evenly. Then, they are transferred to a reactor, the stirring device is turned on, and the temperature is raised to above 100°C.

[0046] The sodium solution is sent to the reactor, and hydrogen is introduced into the reactor when the temperature reaches 150°C. The synthesis reaction is carried out at 130-170°C and a pressure of 13-25 MPa. The reaction lasts for 4-8 hours. After the reaction, the reactant containing sodium aluminum hydride is cooled, depressurized, and sent to a filtered vacuum dryer;

[0047] The filter vacuum dryer is first filtered, and the filtrate containing the catalyst solvent is recovered to the premixing tank. The remaining sodium aluminum hydride slurry in the filter vacuum dryer is added with solvent, and filtered again and the catalyst-containing solvent is recovered to the premixing tank. The remaining solvent is recovered by evaporation and condensation through the filter vacuum dryer system. The heating temperature of the filter vacuum dryer is 50-70°C, the vacuum degree is -0.095Mpa, and the drying time is 1-3 hours. After the drying is completed, the sodium aluminum hydride solid particle product is discharged and sealed and packaged for storage.

[0048] In the preparation method, a reactant containing sodium aluminum hydride is obtained after the reaction, cooled and depressurized, and then sent to a reaction tank. The sodium aluminum hydride is separated by static gravity in the reaction tank, an upper layer of catalyst-containing solvent clear liquid is extracted and recovered, a solvent is added to the lower solid phase, and the mixture is uniformly stirred. Anhydrous lithium chloride is quantitatively added in batches to the reaction tank, and the mixture reacts with the sodium aluminum hydride at room temperature and pressure. After the reaction is complete, the lithium aluminum hydride is dissolved in an ether solution, and sodium chloride is precipitated. The sodium chloride and the lithium aluminum hydride ether solution are separated by a flat filter, and the filtrate is sent to a filter vacuum dryer. The filter vacuum dryer is heated with thermal oil at a heating temperature of 50-90°C and a vacuum degree of -0.030Mpa to -0.075Mpa. The drying time is 1-3 hours. After the drying is completed, the lithium aluminum hydride solid particle product is discharged, sealed, and stored.

[0049] In the preparation method, before preparation, the premixing tank, the reaction kettle and the filter vacuum dryer are all purged with nitrogen.

[0050] Compared with the prior art, the present invention has the following advantages: the solid metal hydride preparation device described in the present invention adopts a one-step method to produce sodium aluminum hydride solid products on a large scale. It is suitable for the large-scale production of solid products such as sodium aluminum hydride and lithium aluminum hydride. The device of the present invention has one production line and can produce different metal hydride products. Compared with one production line producing one product, the investment is small. The filtration vacuum drying system adopts vacuum drying of the filtered slurry to achieve energy saving and consumption reduction. After passing through a two-stage condenser, the solvent in the slurry is recovered, and the remaining small amount of non-condensable gas is adsorbed by an activated carbon adsorption tank. The sodium aluminum hydride synthesis reactor adopts PID control, which can stably control the pressure and temperature in the reactor. The reactor can realize the recycling of catalysts and solvents and the cleaning of metal hydride slurry. The reaction yield of lithium aluminum hydride prepared by the reaction of sodium aluminum hydride and lithium chloride is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0051] Various other advantages and benefits of the present invention will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiments below. The accompanying drawings are intended only to illustrate preferred embodiments and are not to be construed as limiting the present invention. It should be understood that the drawings described below are merely examples of the present invention, and that those skilled in the art will be able to derive other drawings from these drawings without inventive effort. Throughout the drawings, identical reference numerals are used to denote identical components.

[0052] In the attached figure:

[0053] Figure 1 This is a schematic diagram of a process flow for industrially synthesizing a solid sodium aluminum hydride product using a solid metal hydride preparation device according to one embodiment of the invention;

[0054] Figure 2 This is a schematic diagram of a process flow for industrially synthesizing lithium aluminum hydride solid products using a solid metal hydride preparation device according to one embodiment of the invention;

[0055] Figure 3 It is a structural schematic diagram of a filtering vacuum drying system of a solid metal hydride preparation device according to an embodiment of the invention.

[0056] The present invention will be further explained below with reference to the accompanying drawings and embodiments. DETAILED DESCRIPTION

[0057] The following will refer to the attached Figures 1 to 3Specific embodiments of the present invention will now be described in greater detail. Although specific embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention may be implemented in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided to facilitate a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art.

[0058] 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 invention. The scope of protection of the present invention shall be as defined in the attached claims.

[0059] To facilitate understanding of the embodiments of the present invention, further explanation will be given below using specific embodiments as examples in conjunction with the accompanying drawings, and the accompanying drawings do not constitute a limitation on the embodiments of the present invention.

[0060] For better understanding, Figures 1 to 3 As shown, the solid metal hydride preparation device includes:

[0061] The premixing tank 1 includes an inlet for inputting solid metal powder, solvent and catalyst, an agitator for stirring the solid metal powder, solvent and catalyst, and an outlet for discharging the mixture;

[0062] A reactor is connected to the premixing tank 1, and the reactor comprises:

[0063] The kettle body includes a first inlet connected to the discharge port, a second inlet for introducing metal liquid, a third inlet for introducing hydrogen, and an outlet for discharging reactants generated by the reaction in the kettle body, wherein the reactants include solid metal hydride, solvent, and catalyst.

[0064] a stirring device for stirring the mixture from the first inlet and the metal liquid,

[0065] A first temperature regulating device is connected to the kettle body to adjust to a first reaction temperature,

[0066] A pressure regulating device, which regulates the reaction pressure in the kettle;

[0067] A filtration vacuum drying system 3 is connected to the reactor, and the filtration vacuum drying system 3 includes:

[0068] A filter vacuum dryer 301 comprising:

[0069] The housing includes an inlet connected to the outlet for introducing reactants, an exhaust port for discharging solvent vapor, and a filtrate outlet 3017,

[0070] a jacket 3016 at least partially surrounding the shell to heat the shell to a predetermined temperature,

[0071] A stirrer 3012 is vertically rotatably connected to the vacuum housing. The stirrer 3012 includes a spiral ribbon, a scraper 3013, and a crusher 3014.

[0072] The filter 3011 is disposed in the shell and surrounds the agitator 3012 to separate the solid metal hydride from the reactants. The solvent and the catalyst return to the premixing tank 1 through the filtrate outlet 3017 .

[0073] In a preferred embodiment of the solid metal hydride preparation device, the filtration vacuum drying system 3 further includes:

[0074] The primary condenser 302 is connected to the exhaust port to condense the solvent vapor to obtain solvent liquid.

[0075] The gas-liquid separation tank 303 is connected to the primary condenser 302 to separate the solvent liquid from the solvent vapor.

[0076] The vacuum pump 304 is connected to the gas-liquid separation tank 303 to reduce the system pressure before the pump.

[0077] The secondary condenser 305 is connected to the vacuum pump 304 to introduce the solvent vapor.

[0078] The activated carbon adsorption tank 306 is connected to the secondary condenser 305 to adsorb the uncondensed solvent vapor.

[0079] In a preferred embodiment of the solid metal hydride preparation device, the device further comprises:

[0080] A reaction tank 4 is connected to the outlet to introduce reactants, and the reaction tank 4 includes:

[0081] The separation part separates the solid metal hydride from the reactants by static gravity.

[0082] The reaction part includes an input port for inputting materials and a stirring unit, wherein the input materials and the solid metal hydride generate a second solid metal hydride solution in the reaction part.

[0083] a second temperature regulating device connected to the reaction part to regulate the reaction temperature to a second reaction temperature;

[0084] The flat plate filter 5 is connected to the reaction tank 4 and the inlet to filter and obtain the second solid metal hydride solution and send the second solid metal hydride solution into the filtration vacuum dryer 301 .

[0085] In a preferred embodiment of the solid metal hydride preparation device, the premixing tank 1, the reaction kettle and the filtering vacuum drying system 3 are all provided with nitrogen purge pipelines.

[0086] In a preferred embodiment of the solid metal hydride preparation device, the filter screen 3011 comprises a metal sintered filter screen, and the pore size of the filter screen 3011 is 5-20 μm.

[0087] In a preferred embodiment of the solid metal hydride preparation device, the first temperature regulating device includes a heater, the second temperature regulating device includes a cooler, and the first temperature regulating device and the second temperature regulating device are controlled by PID.

[0088] In a preferred embodiment of the solid metal hydride preparation device, the pressure regulating device includes an electric regulating valve.

[0089] In one embodiment, agitator 3012 is supported in filter vacuum dryer 301 via fixed agitation support 3015 .

[0090] In one embodiment, the filter vacuum dryer 301 system Figure 3 As shown, the apparatus comprises a filter vacuum dryer 301, a primary condenser 302, a gas-liquid separation tank 303, a vacuum pump 304, a secondary condenser 305, and an activated carbon adsorption tank 306. The filter vacuum dryer 301 has a filter screen 3011 with a pore size of 5-20 μm, which separates the sodium aluminum hydride particles from the solvent solution. Its cylinder wall is jacketed with a heat-conducting oil heating jacket 3016, which allows for separation of the sodium aluminum hydride material from the solvent solution by heating it from room temperature to 70°C. It also has an agitator 3012 with a spiral ribbon, a scraper 3013, and a crusher 3014 to prevent the sodium aluminum hydride dry material from clumping and allowing for crushing and unloading. The filter dryer 301 is connected to a vacuum pump 304, which maintains an internal pressure of -0.095 MPa. Under heating conditions, the solvent evaporates at a temperature of 50-90°C, drying the sodium aluminum hydride material.

[0091] In one embodiment, the reaction tank 4 serves both as a separator and a reactor, and is equipped with a cooling device that uses PID to regulate the amount of circulating cooling water to precisely control the reaction temperature within the tank. During the production of lithium aluminum hydride, the reaction tank 4 serves as both a sedimentation separator and a reactor.

[0092] In one embodiment, the filtration vacuum dryer 301 performs filtering, heating, and vacuum drying functions. Filtration reduces solvent evaporation, significantly reducing energy consumption. Vacuum drying allows the metal hydride slurry to be dried at low temperatures, preventing product decomposition and allowing for solvent recovery. Furthermore, the filtration vacuum dryer 301 includes a stirring ribbon, scraper 3013, and crusher 3014 to prevent sticking and facilitate unloading.

[0093] In one embodiment, the filter vacuum dryer 301 has heating, filtering, and vacuum drying functions. Its filter screen is a metal sintered screen with a pore size of 5-20 μm. It is connected to a vacuum pump 304, which can achieve an internal pressure range of 0 to -0.095 MPa, maintaining an evaporation temperature range of 30 to 90°C for the metal hydride slurry, ensuring that the metal hydride is dried below its decomposition temperature. The stirring device includes a spiral ribbon, scraper 3013, and crusher 3014 to prevent sticking and to facilitate crushing and unloading.

[0094] In one embodiment, the method uses aluminum powder, liquid sodium, and hydrogen to directly synthesize sodium aluminum hydride in a high-pressure reaction vessel at a certain temperature (130-170° C.) and a certain pressure (13-25 MPa).

[0095] Na(l)+Al(s)+2H2(g)→NaAlH4(s)

[0096] The reaction is carried out in toluene, ether, or methylcyclohexane solvents. Since sodium aluminum hydride is insoluble in toluene, ether, or methylcyclohexane, the prepared sodium aluminum hydride solid particles can be separated by sedimentation and dried to obtain a sodium aluminum hydride solid product.

[0097] Industrially synthesized sodium aluminum hydride is then subjected to a double decomposition reaction with lithium chloride in an ether solution, and after filtration and drying, a solid particle product of lithium aluminum hydride can be obtained. This preparation method can achieve a high yield of lithium aluminum hydride:

[0098] NaAlH4+LiCl→LiAlH4+NaCl.

[0099] The preparation method of the solid metal hydride preparation device comprises the following steps:

[0100] Aluminum powder, solvent, and catalyst are weighed and placed in premix tank 1 and stirred evenly. Then, they are transferred to the reactor, the stirring device is turned on, and the temperature is raised to above 100°C.

[0101] The sodium solution is sent to the reactor, and when the temperature reaches 150° C., hydrogen is introduced into the reactor to carry out a synthesis reaction at 130-170° C. and a pressure of 13-25 MPa. The reaction lasts for 4-8 hours. After the reaction, the reactant containing sodium aluminum hydride is cooled, depressurized, and sent to a filtration vacuum dryer 301;

[0102] The filter vacuum dryer 301 is first filtered, and the filtrate containing the catalyst solvent is recovered to the premixing tank 1. The remaining sodium aluminum hydride slurry in the filter vacuum dryer 301 is added with solvent, and filtered again and the catalyst-containing solvent is recovered to the premixing tank 1. The remaining solvent vapor is condensed and recovered by the filter vacuum dryer 301 system. The filter vacuum dryer 301 is heated at a temperature of 50-70°C, a vacuum degree of -0.095Mpa, and a drying time of 1-3 hours. After drying is completed, the sodium aluminum hydride solid particle product is discharged and sealed and packaged for storage.

[0103] In a preferred embodiment of the preparation method, the reactant containing sodium aluminum hydride obtained after the reaction is cooled and depressurized and then sent to a reaction tank 4. The sodium aluminum hydride is subjected to static gravity separation in the reaction tank 4, the upper layer of catalyst-containing solvent clear liquid is extracted and recovered, the lower layer of solid phase is added with solvent, and stirred evenly. Anhydrous lithium chloride is added to the reaction tank 4 in batches and quantitatively, and reacts with the sodium aluminum hydride at room temperature and pressure. After the reaction is complete, the lithium aluminum hydride is dissolved in the ether solution and sodium chloride is precipitated. The sodium chloride and the lithium aluminum hydride ether solution are separated by a flat filter 5, and the filtrate is sent to a filter vacuum dryer 301. The filter vacuum dryer 301 is heated with thermal oil at a heating temperature of 50-90°C, a vacuum degree of -0.030Mpa to -0.075Mpa, and a drying time of 1 to 3 hours. After drying is completed, the lithium aluminum hydride solid particle product is discharged and sealed and packaged for storage.

[0104] In a preferred embodiment of the preparation method, before preparation, the premixing tank 1, the SAH reactor 2, the reaction tank 4 and the filter vacuum dryer 301 are all purged with nitrogen.

[0105] In one embodiment, a solid sodium aluminum hydride product is synthesized industrially, and all equipment is nitrogen-purged before feeding. Aluminum powder, solvent, and catalyst are weighed and placed in a premixing tank 1 where they are stirred evenly. The solvent can be a hydrocarbon insoluble in sodium aluminum hydride, such as toluene, and the catalyst is triethylaluminum. The mixture is transferred to a high-pressure SAH reactor 2, where the agitator is turned on and the temperature is raised to above 100°C. The sodium solution is then transferred to the high-pressure SAH reactor 2. When the temperature reaches 150°C, hydrogen is introduced to slowly raise the pressure in the reactor to 25 MPa. The synthesis reaction proceeds with the hydrogen. As the temperature rises during the reaction, cooling oil is turned on to remove the reaction heat. The reaction lasts for 4-8 hours. The product after the reaction is cooled and depressurized, and then the material is transferred to a filter vacuum dryer 301. Filtering is performed first, and the filtrate containing the catalyst solvent is recovered to the premixing tank 1. New solvent is added to the remaining sodium aluminum hydride slurry in the filter vacuum dryer 301, and the filtrate containing the catalyst solvent is filtered again and recovered to the premixing tank 1. The remaining small amount of solvent is condensed and recovered in the filter vacuum dryer 301 system. The filter vacuum dryer 301 is heated with thermal oil at a temperature of 50-70°C and a vacuum degree of -0.095 MPa. Each drying time is 1-3 hours. After drying is completed, the sodium aluminum hydride solid particle product is discharged and sealed and stored.

[0106] In one embodiment, lithium aluminum hydride solid product is synthesized industrially, and all equipment is nitrogen-substituted before feeding. Aluminum powder, solvent, and catalyst are weighed and put into premix tank 1 and stirred evenly. The solvent can be ether, and the catalyst can be sodium diethyl aluminum dihydride. Transfer to high-pressure SAH reactor 2, turn on the agitator and heat to above 100°C, then send the sodium solution to high-pressure SAH reactor 2, and when the temperature reaches 150°C, introduce hydrogen to slowly raise the pressure in the reactor to 25Mpa, and carry out synthesis reaction with hydrogen. When the temperature rises during the reaction, the cooling oil can be turned on to remove the reaction heat. The product after the reaction is cooled and depressurized, and the material is sent to reactor 4. Reactor 4 is equipped with a stirring device, a jacket, etc. Taking advantage of the fact that sodium aluminum hydride is insoluble in ether, sodium aluminum hydride is separated by static gravity, the upper layer containing the catalyst solvent clear liquid is extracted and recovered, and the lower solid phase is added with new solvent and stirred evenly. Anhydrous lithium chloride is added to reaction tank 4 in batches and quantitatively, and reacts with sodium aluminum hydride at room temperature and pressure. Cooling water is passed through the jacket to remove the reaction heat. After the reaction is complete, the lithium aluminum hydride will dissolve in the ether solution, and the sodium chloride will precipitate. The sodium chloride and the lithium aluminum hydride ether solution are separated by a flat plate filter 5. The filtrate is sent to the filter vacuum dryer 301. The filter vacuum dryer 301 is heated with thermal oil at a temperature of 50-90°C, a vacuum degree of -0.030 MPa to -0.075 MPa, and each drying time is 1 to 3 hours. After drying is complete, the lithium aluminum hydride solid particle product is discharged, sealed and packaged for storage.

[0107] Example 1

[0108] A sodium aluminum hydride production unit with a batch capacity of 1kg per batch was used. All equipment was nitrogen-purged before feeding. 0.495kg of aluminum powder, 1.62kg of toluene, and 0.212kg of the catalyst sodium diethylaluminum dihydride were placed in premix tank 1 and stirred evenly. The mixture was transferred to high-pressure SAH reactor 2. The agitator 3012 was activated and the temperature was raised to above 100°C. 0.42kg of sodium solution was then added to the high-pressure SAH reactor 2. When the temperature reached 150°C, hydrogen was introduced to slowly raise the pressure in the reactor to 25 MPa. The synthesis reaction proceeded with the hydrogen. As the temperature rose during the reaction, cooling oil was activated to remove the reaction heat. The reaction lasted for 6 hours. The product was cooled and depressurized before being transferred to a filter vacuum dryer 301. Filtering was performed using a 20μm pore size filter. 1.4kg of the catalyst-containing solvent filtrate was recovered and transferred to premix tank 1. The remaining solvent was condensed and recovered in the filter vacuum dryer 301. The filter vacuum dryer 301 was heated with thermal oil at 70°C, a vacuum degree of -0.095 MPa, and a drying time of 1 hour. After drying, 0.987 kg of sodium aluminum hydride solid particle product was discharged and sealed and stored.

[0109] Example 2:

[0110] A sodium aluminum hydride production unit with a daily output of 100kg is used. All equipment is nitrogen-purged before feeding. 18.15kg of aluminum powder, 60kg of toluene, and 28kg of triethylaluminum catalyst are weighed and placed in premix tank 1, where they are stirred evenly. The mixture is transferred to a 100L high-pressure SAH reactor 2. The agitator 3012 is turned on and the temperature is raised to 100°C. 15.5kg of sodium solution is then added to the high-pressure SAH reactor 2. When the temperature reaches 150°C, hydrogen is introduced to slowly raise the pressure in the reactor to 25 MPa. A synthesis reaction is then carried out with the hydrogen. As the temperature rises during the reaction, cooling oil can be turned on to remove the reaction heat. The reaction lasts for 6 hours. The product is cooled and depressurized before being transferred to a filtered vacuum dryer 301. First, filter the slurry using a 20μm pore size filter. 50kg of the catalyst-solvent filtrate is filtered out and returned to premix tank 1. 10kg of new toluene solvent is added to the remaining sodium aluminum hydride slurry in the filter vacuum dryer 301. The slurry is filtered again, and 10kg of the catalyst and solvent are recovered and returned to premix tank 1. The remaining small amount of solvent is condensed and recovered in the filter vacuum dryer 301 system. The remaining sodium aluminum hydride slurry is heated in the filter vacuum dryer 301 with thermal oil at 70°C, a vacuum of -0.095 MPa, and a drying time of 3 hours. After drying, 31.44kg of solid sodium aluminum hydride particles are discharged, sealed, and stored.

[0111] Example 3:

[0112] A lithium aluminum hydride production unit with a batch capacity of 1kg was used. All equipment was nitrogen-purged before feeding. 0.76kg of aluminum powder, 1.4kg of ether, and 0.38kg of the catalyst sodium diethylaluminum dihydride were weighed and placed in premix tank 1, where they were stirred evenly. The mixture was then transferred to high-pressure SAH reactor 2. The agitator 3012 was activated and the temperature was raised to 100°C. 0.63kg of sodium solution was then added to the reactor. When the temperature reached 150°C, hydrogen was introduced to slowly raise the pressure in the reactor to 25 MPa. The synthesis reaction proceeded with the hydrogen. As the temperature rose during the reaction, a cooling oil was activated to remove the heat of reaction. The reaction lasted for 6 hours. The product was cooled, depressurized, and transferred to reactor tank 4. Taking advantage of the insolubility of sodium aluminum hydride in ether, the sodium aluminum hydride was separated by gravity in reactor tank 4. 1.1kg of the supernatant containing the catalyst solvent was withdrawn from the upper layer, and 1.1kg of new solvent was added to the lower solid phase, which was stirred evenly. A total of 1.12 kg of anhydrous lithium chloride was added to the reaction tank 4 in batches and reacted with sodium aluminum hydride at room temperature and pressure. Cooling water was passed through the jacket to remove the reaction heat. After the reaction is complete, the lithium aluminum hydride will dissolve in the ether solution and the sodium chloride will precipitate. The sodium chloride is separated from the lithium aluminum hydride ether solution through the flat filter 5, and 1.5 kg of sodium chloride is isolated. The filtrate containing lithium aluminum hydride is sent to the filter vacuum dryer 301. The filter vacuum dryer 301 is heated with thermal oil at a heating temperature of 50°C, a vacuum degree of -0.075 MPa, and a drying time of 1 hour. After drying, 0.99 kg of lithium aluminum hydride solid particle product is discharged and sealed and stored.

[0113] Embodiment 4:

[0114] A 100kg / day lithium aluminum hydride production unit was used. All equipment was nitrogen-purged before feeding. 23kg of aluminum powder, 42kg of ether, and 11.4kg of the catalyst sodium diethylaluminum dihydride were weighed and placed in premix tank 1, where they were stirred evenly. The mixture was then transferred to a 100L high-pressure SAH reactor 2. The agitator 3012 was activated and the temperature was raised to 100°C. 19kg of sodium solution was then added to the 100L high-pressure SAH reactor 2. When the temperature reached 150°C, hydrogen was introduced to slowly raise the pressure in the reactor to 25 MPa. The synthesis reaction proceeded with the hydrogen. As the temperature rose during the reaction, cooling oil was activated to remove the heat. The reaction lasted for 6 hours. The product was cooled, depressurized, and transferred to reactor tank 4. Taking advantage of the insolubility of sodium aluminum hydride in ether, the sodium aluminum hydride was gravity-separated in reactor 4. 35kg of the upper catalyst-containing solvent layer was withdrawn for recovery, and 30kg of fresh solvent was added to the lower solid phase, which was then stirred evenly. A total of 34 kg of anhydrous lithium chloride was added to reaction tank 4 in batches and reacted with sodium aluminum hydride at room temperature and pressure. Cooling water was passed through the jacket to remove the reaction heat. After the reaction was complete, the lithium aluminum hydride dissolved in the ether solution and sodium chloride precipitated. The sodium chloride was separated from the lithium aluminum hydride ether solution through a flat filter 5, and 45 kg of sodium chloride was isolated. The filtrate containing lithium aluminum hydride was sent to the filter vacuum dryer 301. The filter vacuum dryer 301 was heated with thermal oil at a heating temperature of 50°C, a vacuum degree of -0.075 MPa, and a drying time of 3 hours. After drying, 30 kg of lithium aluminum hydride solid particle product was discharged and sealed and stored.

[0115] Although the embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above-mentioned specific embodiments and application fields. The above-mentioned specific embodiments are merely illustrative and instructive, and are not restrictive. A person skilled in the art, guided by this specification and without departing from the scope of protection of the claims of the present invention, may also devise various forms, all of which fall within the scope of protection of the present invention.

Claims

1. A solid metal hydride preparation device, characterized in that: It includes, A premixing tank comprising an inlet for inputting solid metal powder, solvent and catalyst, an agitator for stirring the solid metal powder, solvent and catalyst, and an outlet for discharging the mixture; A reactor connected to the premixing tank, the reactor comprising: The kettle body includes a first inlet connected to the discharge port, a second inlet for introducing metal liquid, a third inlet for introducing hydrogen, and an outlet for discharging reactants generated by the reaction in the kettle body, wherein the reactants include solid metal hydride, solvent, and catalyst. a stirring device for stirring the mixture from the first inlet and the metal liquid, A first temperature regulating device is connected to the kettle body to adjust to a first reaction temperature, A pressure regulating device, which regulates the reaction pressure in the kettle; A filtration vacuum drying system is connected to the reactor, and the filtration vacuum drying system includes: A filter vacuum dryer comprising, The vacuum housing includes an inlet connected to the discharge port for introducing reactants, an exhaust port for discharging solvent vapor, and a filtrate outlet connected to the feed port. a jacket at least partially surrounding the vacuum housing to heat the vacuum housing to a predetermined temperature, A stirrer is vertically rotatably connected to the vacuum housing, and the stirrer includes a spiral ribbon and a scraper. A filter is arranged in the shell and surrounds the stirrer to separate the solid metal hydride from the reactants. The solvent and the catalyst are returned to the premixing tank from the filtrate outlet.

2. The solid metal hydride preparation device according to claim 1, characterized in that: Preferably, the filtration vacuum drying system further comprises: A primary condenser connected to the exhaust port to condense the solvent vapor to obtain solvent liquid, A gas-liquid separation tank connected to the primary condenser to separate the solvent liquid from the solvent vapor, Vacuum pump, which is connected to the gas-liquid separation tank to reduce the system pressure before the pump, The secondary condenser is connected to a vacuum pump to introduce solvent vapor. An activated carbon adsorption tank is connected to the secondary condenser to adsorb the remaining solvent vapor.

3. The solid metal hydride preparation device according to claim 1, characterized in that: Also includes, A reaction tank connected to the outlet for introducing reactants, the reaction tank comprising: The separation part separates the solid metal hydride from the reactants by static gravity. The reaction part includes an input port for inputting materials and a stirring unit, wherein the input materials and the solid metal hydride generate a second solid metal hydride solution in the reaction part. a second temperature regulating device connected to the reaction part to regulate the reaction temperature to a second reaction temperature; A flat plate filter is connected to the reaction tank and the inlet to filter and obtain a second solid metal hydride solution, and then the solution is sent to a filter vacuum dryer for drying to obtain a second solid metal hydride.

4. The solid metal hydride preparation device according to claim 1, characterized in that: The premixing tank, the reaction kettle and the filtering vacuum drying system are all provided with nitrogen purge pipelines.

5. The solid metal hydride preparation device according to claim 1, characterized in that: The filter screen comprises a metal sintered filter screen, and the pore size of the filter screen is 5-20 μm.

6. The solid metal hydride preparation device according to claim 1, characterized in that: The first temperature regulating device includes a heater, the second temperature regulating device includes a cooler, and the first temperature regulating device and the second temperature regulating device are connected to a PID controller.

7. The solid metal hydride preparation device according to claim 1, characterized in that: The pressure regulating device includes an electric regulating valve.

8. A method for preparing the device according to any one of claims 1 to 7, characterized in that: After the reaction, a reactant containing sodium aluminum hydride is obtained, which is cooled, depressurized, and then sent to a reaction tank. The sodium aluminum hydride is subjected to static gravity separation in the reaction tank, an upper layer of catalyst-containing solvent clear liquid is extracted and recovered, a solvent is added to the lower solid phase, and the mixture is uniformly stirred. Anhydrous lithium chloride is quantitatively added in batches to the reaction tank, and the mixture reacts with the sodium aluminum hydride at room temperature and pressure. After the reaction is complete, the lithium aluminum hydride is dissolved in an ether solution, and sodium chloride is precipitated. The sodium chloride and the lithium aluminum hydride ether solution are separated by a flat filter, and the filtrate is sent to a filter vacuum dryer. The filter vacuum dryer is heated with heat-conducting oil at a heating temperature of 50-90°C and a vacuum degree of -0.030Mpa to -0.075Mpa. The drying time is 1-3 hours. After the drying is completed, the lithium aluminum hydride solid particle product is discharged and sealed and packaged for storage.

9. A method for preparing the device according to any one of claims 1 to 7, characterized in that: Before preparation, the premixing tank, reactor and filter vacuum dryer were all purged with nitrogen.

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