System and method for preparing metal hydride powder

Abstract

A system for preparing metal hydride powder, comprising: a rapid gas heating device (1), an atomization hydrogenation powder making device (2), and a gas circulation pressurization device (4). The rapid gas heating device (1) comprises a gas inlet end and a gas outlet end; the gas inlet end is in communication with a gas generation device; the gas generation device is configured to supply, to the rapid gas heating device (1), gas for preparing a hydrogenation mixed gas; the gas outlet end is in communication with the atomization hydrogenation powder making device (2); the atomization hydrogenation powder making device (2) comprises a gas atomization structure in communication with molten metal; the gas atomization structure is in communication with the gas outlet end, and can convert the molten metal into hydrogenated metal powder by using the gas introduced from the gas outlet end; the gas circulation pressurization device (4) is arranged between the atomization hydrogenation powder making device (2) and the gas generation device, and can introduce, by means of the gas generation device, the gas discharged from the atomization hydrogenation powder making device (2) into the rapid gas heating device (1) for recycling. The method improves the production efficiency, production capacity, and product consistency of metal hydrides, reduces costs, and enhances the controllability and safety of large-scale production. The present invention further relates to a method for preparing magnesium-based metal hydride powder.

Description

A system and method for preparing metal hydride powder Technical Field

[0001] This solution relates to the field of hydrogen storage materials technology, specifically to a metal hydride powder preparation system and method. Background Technology

[0002] Hydrogen energy, with its high energy density, environmental friendliness, and renewability, is considered a green energy source with immense development potential. Hydrogen energy storage is a crucial link in the development of the hydrogen economy, and driven by dual-carbon goals, solid-state hydrogen storage materials with high hydrogen storage density and low storage pressure have attracted significant attention. Solid-state hydrogen storage combines hydrogen with solid materials through physical or chemical means, storing hydrogen in the material in atomic, molecular, or ionic form. This technology is considered highly promising and is expected to meet future demands for high-density, low-pressure, and highly safe hydrogen storage.

[0003] Metal hydrides are the mainstream solid-state hydrogen storage materials. Hydrogen can form hydrides with certain metals (such as magnesium, titanium, lithium, and sodium), and these hydrides can release hydrogen under certain conditions. Common metal hydrides include magnesium hydride (MgH₂), titanium hydride (TiH₂), and lithium hydride (LiH). Currently, both domestic and international hydrogen storage raw materials tend to use metal powders. However, known magnesium-based, titanium-based, vanadium-based, and rare earth-based metals are highly reactive. Directly producing them as powders results in poor safety and low production capacity. Furthermore, the subsequent hydrogenation processing of metal powders has a long cycle and even lower production capacity, seriously affecting the development of metal hydrides. Summary of the Invention

[0004] The present invention aims to provide a metal hydride powder preparation system and method to simplify the production process of metal hydrides, thereby shortening the processing cycle of metal hydrides and increasing the production capacity of metal hydrides.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: a metal hydride powder preparation system, comprising a gas heating device, an atomizing hydrogenation powder preparation device, and a gas circulation pressurization device; the gas heating device includes an inlet end and an outlet end, the inlet end is connected to a gas generating device, the gas generating device is used to provide gas for preparing hydrogenated mixed gas to the gas heating device, the outlet end is connected to the atomizing hydrogenation powder preparation device, the atomizing hydrogenation powder preparation device includes a gas atomization structure connected to molten metal, the gas atomization structure is connected to the outlet end and can use the gas introduced at the outlet end to convert the molten metal into hydrogenated metal powder, and the gas circulation pressurization device is set between the atomizing hydrogenation powder preparation device and the gas generating device and can introduce the gas discharged from the atomizing hydrogenation powder preparation device into the gas heating device for recycling through the gas generating device.

[0006] The beneficial effects of this solution are as follows: Currently, the preparation of metal hydrides tends to use metal powders. However, known magnesium-based, titanium-based, vanadium-based, and rare earth-based metals are highly reactive, and directly producing them as powders results in poor safety and low production capacity. Furthermore, the subsequent hydrogenation processing of the metal powders is time-consuming and has even lower production capacity, severely hindering the development of metal hydride production. Compared to current metal hydride preparation technologies, the solution proposed in this application utilizes a heating device to heat the hydrogenation mixture to the temperature required for the hydrogenation reaction. This allows the gas atomization structure to directly utilize the hydrogenation mixture to convert molten metal into hydrogenated metal powder. The molten metal reacts directly with the hydrogenation mixture during the conversion process to generate hydrogenated metal powder. Traditional gas-phase methods for preparing metal hydrides require first preparing reactive metals into metal powders using inert gases such as argon. Under the protection of the inert gas, the metal... Heating the powder to a certain temperature and then introducing hydrogen gas for reaction poses certain risks due to the high reactivity of the metal powder, making it difficult to increase the yield of metal hydrides. The technical solution of this application omits the process of preparing metal powder in the current preparation of metal hydrides, reducing the risks in the preparation and storage of metal powder. At the same time, by directly converting the metal powder into metal hydrides during the preparation process, the efficiency and capacity of metal hydride preparation are improved, solving the problems of low production efficiency and batch-to-batch inconsistency in powder quality. This also improves the effective utilization rate of gas and energy, reduces production costs, and enhances the safety and controllability of large-scale production. It provides a safe and efficient new approach for the production of metal hydride powders and also provides high-quality, low-cost raw materials for fields such as hydrogen storage materials.

[0007] Furthermore, the gas rapid heating device is located to the side of the atomizing powder-making device and is on the same horizontal plane; an air inlet controller is provided at the air inlet end, which is connected to the gas generating device and can control the proportion of gas introduced into the gas generating device.

[0008] Beneficial effects:

[0009] Furthermore, the gas rapid heating device also includes a gas rapid heating pipeline, which is located between the inlet and outlet ends. A temperature detection and regulation instrument is installed at the outlet end to detect the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipeline and provide feedback to the gas rapid heating pipeline heater. The gas generating device includes a high-pressure hydrogen station for replenishing hydrogen in the gas rapid heating device, a high-pressure argon station for replenishing argon in the gas rapid heating device, and an inlet controller. The high-pressure hydrogen station and the high-pressure argon station are both located below the gas rapid heating device and are connected to the gas heating device through the inlet controller.

[0010] Furthermore, the gas circulation booster device can process the gas discharged from the atomization hydrogenation powder making device and feed back the hydrogen content and flow rate data of the processed gas to the intake controller. The intake controller can control the high-pressure hydrogen station or replenish the gas processed by the high-pressure argon station based on the feedback hydrogen content and flow rate data.

[0011] Furthermore, the gas circulation booster device includes a gas filter, an oxygen content detector, a deoxygenation system, a gas booster, a hydrogen content detector, and a gas flow meter connected in sequence. The gas filter is used to filter out dust from the gas. The oxygen content detector is used to detect the oxygen content in the gas. The deoxygenation system is electrically connected to the oxygen content detector and is activated when the oxygen content detector detects that the gas oxygen content is unqualified, processing the unqualified gas before it is input back to the gas filter until the oxygen content meets the standard. When the oxygen content detector detects that the gas oxygen content is qualified, the gas booster pressurizes the incoming gas. The hydrogen content detector is used to detect the hydrogen content in the gas after it has been pressurized by the gas booster. The gas flow meter is used to detect the gas flow rate after it has been pressurized by the gas booster. The intake controller is electrically connected to the hydrogen content detector and the gas flow meter and can receive the hydrogen content data detected by the hydrogen content detector and the gas flow rate data detected by the gas flow meter, and supplement the corresponding hydrogen and argon gas according to the data to ensure that the hydrogen content and gas pressure of the gas introduced into the gas heating device meet the process standards.

[0012] A method for preparing a magnesium-based hydride powder includes the following steps:

[0013] S1 Preparation: The atomized hydrogenation powdering raw material is put into the melting crucible of the atomized hydrogenation powdering device. The melting crucible melts the atomized hydrogenation powdering raw material and raises the temperature to the atomized hydrogenation powdering process temperature to obtain molten metal.

[0014] S2 Atomization and Hydrogenation: Hydrogenation mixed gas that meets the process parameters is supplied through a gas generating mechanism and introduced into an atomization and hydrogenation powder making device. The hydrogenation mixed gas is used to convert the molten metal obtained in S1 into magnesium-based hydride powder.

[0015] The beneficial effects of this scheme are as follows: The existing magnesium-based hydride powder process route requires the preparation of reactive magnesium powder first, followed by hydrogenation of the magnesium powder to prepare magnesium hydride. When preparing magnesium hydride by hydrogenation of magnesium powder, a certain catalyst needs to be added, and the reaction is carried out under medium temperature (200℃ and above) and low pressure (0.5MPa and above) conditions for a long time (more than 5 hours). The entire process cycle is relatively long. This scheme directly prepares stable magnesium hydride with a certain hydrogen content from magnesium ingots, reducing the process cycle of deep hydrogenation of powder. The process route is safer and more controllable, thus replacing the existing process route.

[0016] Furthermore, the gas generating mechanism includes a gas heating device and a gas generating device. The gas heating device includes a gas rapid heating pipe and a temperature regulator. The two ends of the gas rapid heating pipe are respectively connected to the gas inlet controller and the atomization hydrogenation powder making device, and can control the temperature of the gas entering the atomization hydrogenation powder making device according to the temperature regulator. The gas generating device includes a high-pressure hydrogen station, a high-pressure argon station and a gas inlet controller. The high-pressure hydrogen station and the high-pressure argon station are respectively connected to the gas inlet controller. The gas inlet controller is connected to the gas rapid heating pipe and can control the ratio of hydrogen and argon entering the gas rapid heating pipe.

[0017] Furthermore, the gas generating mechanism also includes a gas circulation booster device, which includes a gas filter, a detection component, and a gas booster. The gas filter is connected to the exhaust port of the atomizing hydrogenation powder making device, the gas booster is connected to the intake controller, and an oxygen removal system is provided between the detection component and the gas booster.

[0018] Furthermore, it also includes S3 material circulation: S3 material circulation includes S31 gas-material circulation, which is: the gas discharged from S2 atomization and hydrogenation and which has passed the inspection is introduced into the gas rapid heating device through the gas circulation pressurization device to form a gas-material circulation system.

[0019] Furthermore, the process parameters for the hydrogenation mixed gas are as follows: gas pressure is 3-8 MPa, the mixed gas is hydrogen and argon, the hydrogen content is controlled at 20-200 ppm, the temperature is 100-400℃, and the gas flow rate is controlled at 500-3000 m³ / h; the atomization hydrogenation powder production gas pressure is controlled at 3-8 MPa, and the process temperature for magnesium-based metal molten liquid atomization hydrogenation powder production is 700-1200℃; the atomization hydrogenation powder production device also includes a guide pipe, which can withstand the continuous scouring of molten metal above 1200℃ and high-pressure hydrogen-argon mixed gas at 8 MPa and below 400℃ for 8 hours with an inner diameter change of less than 2%. Argon is used as a diluent for hydrogen, ensuring the hydrogen content in the mixed gas is between 20-200 ppm. This avoids the situation where the produced powder is mostly in the form of magnesium powder due to excessively low hydrogen content. When exposed to the atmosphere, magnesium powder readily reacts with oxygen, resulting in high reactivity and hazard. Conversely, excessively high hydrogen content causes the atomized gas to become flammable, posing a significant safety hazard. When other inert gases are used as diluents: nitrogen, for example, readily reacts with magnesium at high temperatures, increasing the nitrogen content in the powder and reducing its final hydrogen storage capacity. Other inert gases are expensive, and helium, for instance, has a relatively long hydrogenation reaction time and good heat transfer properties, causing the metal powder produced by gas atomization to cool rapidly. This shortens the hydrogenation reaction time, affecting the hydrogenation effect and increasing the proportion of magnesium powder in the produced powder, thus compromising product safety. Attached Figure Description

[0020] Figure 1 is a schematic diagram of the metal hydride powder preparation system according to an embodiment of the present invention;

[0021] Figure 2 is a flowchart of the cyclic process for preparing metal hydride powder according to an embodiment of the present invention;

[0022] Figure 3 is a flowchart of the method for preparing magnesium-based hydride powder according to an embodiment of the present invention;

[0023] Figure 4 is a schematic diagram of the morphology detection results of magnesium-based hydride powder obtained in the embodiment of the present invention.

[0024] Figure 5 is a schematic diagram of the particle size detection results of magnesium-based hydride powder prepared according to the embodiment of the present invention.

[0025] The reference numerals in the accompanying drawings include: 1. Gas rapid heating device; 11. Temperature detection and regulation instrument; 12. Gas rapid heating pipeline; 2. Atomizing hydrogenation powder making device; 21. Melter; 22. Atomizer; 23. Atomization chamber; 24. Cyclone separator; 25. Exhaust fan; 31. High-pressure hydrogen station; 32. High-pressure argon station; 33. Inlet controller; 4. Gas circulation and pressurization device; 41. Gas filtration device; 42. Oxygen content detector; 43. Deoxygenation system; 44. Gas booster; 45. Hydrogen content detector; 46. Gas flow meter. The best embodiment of the present invention

[0026] Example 1

[0027] Example 1 is basically as shown in Figures 1-2. As shown in Figures 1-2, a metal hydride powder preparation system includes an atomizing hydrogenation powder preparation device 2, a rapid gas heating device 1, a gas generating device, and a gas circulation pressurization device 4. The rapid gas heating device 1 is located to the side of the atomizing powder preparation device and at the same horizontal plane to reduce the gas pipeline between the rapid gas heating device 1 and the atomizing powder preparation device, thereby minimizing the reduction in heat energy and pressure of the heated gas. The gas circulation pressurization device is located between the atomizing hydrogenation powder preparation device 2 and the gas heating device and can guide the gas discharged from the atomizing hydrogenation powder preparation device 2 into the gas heating device for recycling.

[0028] The atomizing hydrogenation powder-making device 2 includes a gas atomization structure and a separation structure. The gas atomization structure includes a melter 21, an atomizer 22, and an atomization chamber 23. The separation structure includes a cyclone separator 24 and an exhaust fan 25. In this embodiment, the atomizing hydrogenation powder-making device 2 is an induction melting inert gas atomization powder-making device. The working principle and connection relationship are not described in detail here. The guide pipe is fixedly installed in the atomizer 22 and is connected to the gas rapid heating device 1 and the melter 21 respectively, so that the hydrogenated mixed gas input through the gas rapid heating device 1 can be atomized.

[0029] The gas rapid heating device 1 includes a gas rapid heating pipe 12, which includes a heating tube body and a heater. The heater is fixed to the inner wall of the heating tube body and can heat the gas inside the heating tube body. The gas rapid heating pipe 12 body includes an inlet end and an outlet end. The outlet end is connected to the atomizer 22 and is equipped with a temperature detection and regulation instrument 11 for detecting the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipe 12. The temperature detection and regulation instrument 11 is fixedly installed at the outlet end and can provide feedback to the heater of the gas rapid heating pipe 12 to ensure that the temperature of the gas input to the atomizer 22 meets the process requirements.

[0030] The gas generating device is used to supply the gas heating device with the gas for preparing the hydrogenated mixed gas. It includes an inlet controller 33, a high-pressure hydrogen station 31, and a high-pressure argon station 32. The inlet controller 33 is fixedly installed at the inlet end of the gas rapid heating pipeline 12 and is connected to the gas rapid heating pipeline 12. The high-pressure hydrogen station 31 and the high-pressure argon station 32 are both located below the side of the gas rapid heating device 1 and are connected to the gas rapid heating device 1 through the inlet controller 33, thereby adjusting the proportion of gas entering the gas rapid heating pipeline 12 through the inlet controller 33 to ensure that the gas entering the gas rapid heating pipeline 12 meets the process parameters.

[0031] The gas circulation booster device 4 includes a gas filter 41, an oxygen content detector 42, a deoxygenation system 43, a gas booster 44, a hydrogen content detector 45, and a gas flow meter 46. These components are connected sequentially. The gas filter 41 removes dust from the gas, the oxygen content detector 42 detects the oxygen content in the gas, and the deoxygenation system 43 activates when the oxygen content detector 42 detects an unqualified oxygen content, processes the unqualified gas, and then re-introduces it to the gas filter 41 until... When the oxygen content meets the standard, the gas booster 44 pressurizes the incoming gas when the oxygen content detector 42 detects that the gas oxygen content is qualified. The hydrogen content detector 45 is used to detect the hydrogen content in the gas after being pressurized by the gas booster 44, and the gas flow detector 46 is used to detect the gas flow rate after being pressurized by the gas booster 44. The intake controller 33 is connected to the hydrogen content detector 45 and the gas flow detector 46, and can receive the hydrogen content data detected by the hydrogen content detector 45 and the gas flow data detected by the gas flow detector 46, and supplement the corresponding hydrogen and argon according to the data so that the hydrogen content and gas pressure of the gas meet the process standards.

[0032] The specific implementation process is as follows:

[0033] Taking the preparation of titanium hydride as an example, as shown in Figure 2, when the atomized hydrogenation powder making device 2 reaches the powder making start requirement, the gas rapid heating device 1 is turned on. The controller mixes hydrogen and argon according to the process requirements and rushes them into the heating channel. The gas rapid heating pipe 12 is used to quickly heat the hydrogenated mixed gas to the process required temperature. In this embodiment, the hydrogenated mixed gas hydrogen and argon are charged into the gas rapid heating pipe 12 at a gas flow rate ratio of 1:9 (hydrogen content of about 50ppm) and a gas pressure of 5MPa. The gas rapid heating pipe 12 is used to quickly heat the gas to the process required temperature of 100-120℃. The temperature detection and regulation instrument 11 detects that the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipe 12 has reached 100-120℃ and feeds back the collected signal to the heater of the gas rapid heating pipe 12 for adjusting the heating power.

[0034] After the hydrogenation gas flows normally, the melter 21 melts the end of the titanium-iron alloy rod by induction heating. The molten metal flows into the atomized hydrogenation powder making device 2. Under the action of high-speed, heated mixed gas flow, the molten metal is broken into fine droplets. These droplets cool and solidify rapidly into micron-sized powder particles during flight, thus producing titanium hydride powder.

[0035] The production of titanium hydride powder continues. The exhaust gas after hydrogenation enters the gas circulation and pressurization device through a pipeline. The gas circulation and pressurization device first filters the exhaust gas, that is, it cleans the metal powder in the recovered gas. Then it detects the oxygen content of the recovered gas. If the oxygen content of the recovered gas is less than 20 ppm, it proceeds to the next step. If the oxygen content is higher than 20 ppm, the collected oxygen content signal is fed back to the deoxygenation system 43. The deoxygenation system 43 is then activated to process the unqualified gas, and then it is input into the gas filtration device 41 until the oxygen content meets the standard.

[0036] The recovered gas with qualified oxygen content enters the gas pressurization device through a pipeline, pressurizing the gas to 6MPa. The hydrogen content detector 45 and the gas flow detector 46 detect the hydrogen content and flow rate of the pressurized gas and feed the data back to the gas inlet controller 33 of the gas rapid heating device 1. The gas inlet controller 33 replenishes the required gas volume from the high-pressure hydrogen station 31 and the high-pressure argon station 32 according to the demand, ensuring that the gas pressure of 5MPa and the hydrogen content of 50ppm required for the atomization hydrogenation powder making process are achieved. The gas is then introduced into the gas rapid heating pipeline 12 and rapidly heated to the required process temperature of 100-120℃. The temperature detection and regulation instrument 11 detects that the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipeline 12 has reached 100-120℃ and feeds the collected signal back to the heater of the gas rapid heating pipeline 12 for adjusting the heating power. The heated gas is then input into the atomization hydrogenation powder making device 2, thereby realizing gas recycling and reducing gas loss.

[0037] Example 2

[0038] A method for preparing magnesium-based hydride powder, as shown in Figure 3, includes the following steps: S1 Material preparation: The raw material for atomized hydrogenation powder preparation is put into the melting crucible of the atomized hydrogenation powder preparation device 2. The raw material for atomized hydrogenation powder preparation is melted and heated to the atomized hydrogenation powder preparation process temperature through the melting crucible to obtain molten metal.

[0039] S2 Atomization and Hydrogenation: Hydrogenation mixed gas that meets the process parameters is supplied through a gas generating mechanism and introduced into the atomization and hydrogenation powder making device 2. The molten metal obtained in S1 is converted into magnesium-based hydride powder using the hydrogenation mixed gas.

[0040] The specific implementation process is as follows:

[0041] S1 Material Preparation: Prepare 20 kg of metallic magnesium as raw material; load it into the melting crucible of the atomizing hydrogenation powder-making device 2. In this embodiment, the raw material is magnesium ingot with a purity of 99.95%. The atomizing hydrogenation powder-making device 2 is a gas atomization powder-making device. Operate according to the operating procedures, evacuate to 10⁻¹ Pa, and then start heating to melt the magnesium ingot; wait until the magnesium ingot is completely melted and heated to the powder-making process temperature. In this embodiment, the powder-making process temperature is 810℃; at the same time, through the gas inlet controller 33, hydrogen and argon gas of a specific ratio and pressure are injected into the gas rapid heating pipe 12 according to the process requirements. The gas rapid heating pipe 12 is used to heat the gas... The gas is rapidly heated to the required process temperature, which in this embodiment is 150-180℃. The temperature detection and regulation instrument 11 is used to detect the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipeline 12, and feeds back the collected temperature information to the heater of the gas rapid heating pipeline 12 through an electrical signal, thereby adjusting the heating power so that the temperature of the output gas meets the process requirements. During gas circulation, the gas inlet controller 33 controls the replenishment flow of the high-pressure hydrogen station 31 and the gas inlet controller 33 according to the hydrogen content of the hydrogen content detector 45 of the gas circulation booster device 4, so as to ensure that the hydrogen content of the hydrogenated mixed gas is controlled between 20-200ppm.

[0042] S2 Atomization and Hydrogenation: Molten magnesium flows into the atomization and hydrogenation powder-making device 2. A hydrogenation mixed gas conforming to the process parameters is supplied through a gas generating mechanism. The process parameters of the hydrogenation mixed gas are: gas pressure of 5 MPa, hydrogen to argon ratio of 15:85 (hydrogen content of about 88 ppm), temperature of 150-180℃, and gas flow rate controlled at 1200-1300 m3 / h. The hydrogenation mixed gas is then introduced into the atomization and hydrogenation powder-making device 2 to start hydrogenation and atomization powder-making. In this embodiment, the hydrogenation and atomization pressure is controlled at 4.9-5.1 MPa, that is, the gas pressure of the hydrogenation mixed gas is 4.9-5.1 MPa. Under the action of high-speed, heated mixed gas flow, the molten metal is broken into fine droplets. These droplets rapidly cool and solidify into micron-sized powder particles during flight, thus obtaining magnesium hydride powder. The prepared magnesium hydride powder is collected using a powder storage tank, and powder with a particle size of 0-150 μm is selected through powder classification.

[0043] After the atomization and hydrogenation powdering process is completed, the selected magnesium hydride powder is tested for hydrogen content, powder morphology, and particle size. The hydrogen content of the magnesium hydride powder is 2.78-3.16 wt%. The powder morphology test results are shown in Figure 4, and the powder particle size test results are shown in Figure 5.

[0044] Example 3

[0045] Example 3 is basically the same as Example 2, except that the raw material is magnesium-aluminum alloy MgAl10, and it also includes S3 material circulation. S3 material circulation includes S31 gas-material circulation and S32 solid material circulation. S31 gas-material circulation is: the gas discharged from S2 atomization powdering and hydrogenation and tested and qualified is introduced into the gas rapid heating device 1 through the gas circulation pressurization device to form a gas-material circulation system.

[0046] The S32 solid material cycle is as follows: the magnesium-based hydride powder obtained in S2 atomization and hydrogenation is classified into powders, and the magnesium-based hydride powder that fails to pass the powder classification is used as raw material for atomization and hydrogenation powdering and then fed back into the gas atomization powdering equipment to form a solid material cycle.

[0047] The specific implementation process is as follows:

[0048] S1 material preparation and S2 atomization powder production and hydrogenation are basically the same as in Example 1, with the following differences:

[0049] In S1 preparation, the raw material is magnesium-aluminum alloy MgAl10 or magnesium-based hydride powder obtained by S2 atomization and hydrogenation. After powder classification, the magnesium-based hydride powder with a particle size greater than 150μm is added as raw material for atomization and hydrogenation powdering and re-powdering, thereby forming S32 solid material recycling, so as to improve the utilization rate of solid materials and reduce the waste disposal cost.

[0050] In S2 atomization and hydrogenation, the exhaust gas after hydrogenation enters the gas circulation and pressurization device through a pipeline. The powder recovered from the gas is filtered and purified. The oxygen content is empirically measured to be less than 20 ppm. The qualified recovered gas is pressurized to 5.5 MPa, the hydrogen content is empirically measured to be 75 ppm, and the gas flow rate is 1128 m3 / h. The system feeds back the collected data to the gas rapid heating device 1. By supplementing hydrogen and argon at a gas flow rate ratio of 15:85 to 1200-1300 m3 / h, and then heating to a temperature of 150-180℃, the mixed gas is again injected into the atomization and hydrogenation powder production device 2, thus forming the S31 gas-material circulation, realizing gas circulation atomization and hydrogenation powder production, thereby reducing gas and material loss.

[0051] Example 4

[0052] Based on Example 1, the atomizing hydrogenation powder making device 2 also includes a guide tube, which can withstand the scouring of molten metal above 1200°C and high-pressure hydrogen-argon mixture gas at 8MPa and below 400°C for 8 hours with an inner diameter change of less than 2%.

[0053] The guide tube is formed by machining a composite ceramic rod. The manufacturing process of the composite ceramic rod is as follows:

[0054] S1. Mix the dispersant with deionized water, then add zirconium oxychloride and magnesium chloride to the solution and stir to prepare a dispersion solution. Continue stirring until the zirconium ion concentration in the dispersion solution is 0.1~0.5 mol / L and the magnesium ion concentration is 0.02~0.2 mol / L. Heat the dispersion solution to 40~80℃. Specifically, anhydrous ethanol is used as the dispersant, and the volume of anhydrous ethanol is 8%~12% of the volume of the dispersion solution.

[0055] S2, preheat the raw material tank of the centrifugal spray dryer to 40~80℃, add the dispersion solution to the raw material tank of the centrifugal spray dryer and stir; add ammonia water to the auxiliary material tank of the centrifugal spray dryer, and feed the dispersion solution and ammonia water at a rate of 0.1-0.3 L / min and a rate of 0.5-2 L / min respectively, and mix them before entering the centrifugal atomizer 22 to obtain a mixed solution. During this process, the temperature of the raw material tank is maintained at 40~80℃; in actual implementation, the dispersion solution is stirred while atomizing, and step 1 is repeated again, adding the newly prepared dispersion solution and ammonia water to the raw material tank and auxiliary material tank respectively; specifically, the ammonia water is used with a concentration of 25%;

[0056] S3. The dispersion solution is atomized using a centrifugal spray dryer. During atomization, the centrifugal spray dryer sprays the mixed solution at a speed of 12,000-18,000 rpm / min to form fine droplets of the mixed solution. The droplets generated by atomization are dried using dry air or inert gas at a temperature of 150-300℃ to obtain a mixed powder.

[0057] S4. A mixed powder of ZrO(OH)2 and Mg(OH)2 is spread evenly in a zirconium oxide ceramic crucible boat and heated in an atmospheric environment using a muffle furnace for decomposition. The residual solid ammonium chloride is completely volatilized, producing pure zirconium oxide and magnesium oxide. The principle is as follows: under heating conditions, ZrO(OH)2 → ZrO2 + H2O, Mg(OH)2 → MgO + H2O. Under the action of temperature, zirconium oxide and magnesium oxide will form a mixed powder block. The heating decomposition process is as follows: in an atmospheric environment, the temperature is raised uniformly at a rate of 10-20℃ / min to the decomposition temperature of 500-700℃ and held for 1-3 hours. After the holding time, it is naturally cooled to room temperature to obtain powder blocks.

[0058] S5. The powder block is ball-milled and then hot-pressed and sintered into a composite ceramic rod. The sintering temperature is 1600-1800℃. Before sintering, it is pre-sintered at 600-800℃ and held for 0.5-1h. Then it is heated to the sintering temperature for sintering. During the entire heating process, the heating rate is controlled at 10-20℃ / min and the temperature is controlled to rise at a uniform rate. After reaching the sintering temperature, the powder is pressed at a pressure of 100-150 tons and held at the temperature and pressure for 1-3h before being cooled with the furnace to obtain the composite ceramic rod.

[0059] The above descriptions are merely embodiments of the present invention, and common knowledge such as specific technical solutions and / or characteristics are not described in detail here. It should be noted that the technical means for solving problems in the above embodiments of the present invention can be used in combination to solve multiple technical problems simultaneously. For those skilled in the art, several modifications and improvements can be made without departing from the technical solutions of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the implementation of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. A metal hydride powder preparation system, characterized in that: The device includes a gas heating device, an atomizing hydrogenation powder-making device, and a gas circulation pressurization device. The gas heating device includes an inlet end and an outlet end. The inlet end is connected to a gas generator, which provides gas for preparing the hydrogenated mixture to the gas heating device. The outlet end is connected to the atomizing hydrogenation powder-making device, which includes a gas atomization structure connected to molten metal. The gas atomization structure is connected to the outlet end and can use the gas introduced at the outlet end to convert the molten metal into hydrogenated metal powder. The gas circulation pressurization device is located between the atomizing hydrogenation powder-making device and the gas generator and can introduce the gas discharged from the atomizing hydrogenation powder-making device into the gas heating device for recycling.

2. The metal hydride powder preparation system according to claim 1, characterized in that: The gas rapid heating device is located to the side of the atomizing powder making device and is on the same horizontal plane; the air inlet end is equipped with an air inlet controller, which is connected to the gas generating device and can control the proportion of gas introduced into the gas generating device.

3. The metal hydride powder preparation system according to claim 2, characterized in that: The gas rapid heating device also includes a gas rapid heating pipeline, which is located between the inlet and outlet ends. A temperature detection and regulation instrument is installed at the outlet end to detect the temperature of the hydrogenated mixed gas at the outlet of the gas rapid heating pipeline and provide feedback to the gas rapid heating pipeline heater. The gas generating device includes a high-pressure hydrogen station for replenishing hydrogen in the gas rapid heating device, a high-pressure argon station for replenishing argon in the gas rapid heating device, and an inlet controller. The high-pressure hydrogen station and the high-pressure argon station are both located below the gas rapid heating device and are connected to the gas heating device through the inlet controller.

4. A metal hydride powder preparation system according to claim 3, characterized in that: The gas circulation booster can process the gas discharged from the atomization hydrogenation powder making device and feed back the hydrogen content and flow rate data of the processed gas to the intake controller. The intake controller can control the high-pressure hydrogen station or replenish the gas processed by the high-pressure argon station based on the feedback hydrogen content and flow rate data.

5. A metal hydride powder preparation system according to claim 4, characterized in that: The gas circulation booster device includes a gas filter, an oxygen content detector, a deoxygenation system, a gas booster, a hydrogen content detector, and a gas flow meter connected in sequence. The gas filter removes dust from the gas. The oxygen content detector detects the oxygen content in the gas. The deoxygenation system is electrically connected to the oxygen content detector and activates when the oxygen content detector detects that the gas oxygen content is unqualified, processing the unqualified gas before it is fed back to the gas filter until the oxygen content meets the standard. When the oxygen content detector detects that the gas oxygen content is qualified, the gas booster pressurizes the incoming gas. The hydrogen content detector detects the hydrogen content in the gas after it has been pressurized by the gas booster. The gas flow meter detects the flow rate of the gas after it has been pressurized by the gas booster. The intake controller is electrically connected to the hydrogen content detector and the gas flow meter and can receive the hydrogen content data detected by the hydrogen content detector and the gas flow meter detected by the gas flow meter. Based on this data, it replenishes the corresponding hydrogen and argon gas to ensure that the hydrogen content and pressure of the gas entering the gas heating device meet the process standards.

6. A method for preparing magnesium-based metal hydride powder, characterized in that: Includes the following steps: S1 Preparation: The magnesium-based metal raw material is put into the melting crucible of the atomizing hydrogenation powder making device. The magnesium-based metal raw material is melted and heated to the temperature of the atomizing hydrogenation powder making process through the melting crucible to obtain molten metal. S2 Atomization and Hydrogenation: Hydrogenation mixed gas that meets the process parameters is supplied through a gas generating mechanism and introduced into an atomization and hydrogenation powder making device. The hydrogenation mixed gas is used to convert the molten metal obtained in S1 into magnesium-based hydride powder.

7. A method for preparing a magnesium-based hydride powder according to claim 6, characterized in that: The gas generating mechanism includes a gas heating device and a gas generating device. The gas heating device includes a gas rapid heating pipeline and a temperature controller. The two ends of the gas rapid heating pipeline are connected to the gas inlet controller and the atomization hydrogenation powder making device, respectively, and the temperature controller can control the temperature of the gas entering the atomization hydrogenation powder making device. The gas generating device includes a high-pressure hydrogen station, a high-pressure argon station and a gas inlet controller. The high-pressure hydrogen station and the high-pressure argon station are connected to the gas inlet controller, and the gas inlet controller is connected to the gas rapid heating pipeline and can control the ratio of hydrogen and argon entering the gas rapid heating pipeline.

8. A method for preparing a magnesium-based hydride powder according to claim 7, characterized in that: The gas generating mechanism also includes a gas circulation booster device, which includes a gas filter, a detection component, and a gas booster. The gas filter is connected to the exhaust port of the atomizing hydrogenation powder making device, and the gas booster is connected to the intake controller. An oxygen removal system is provided between the detection component and the gas booster.

9. A method for preparing a magnesium-based hydride powder according to claim 8, characterized in that: It also includes S3 material circulation: S3 material circulation includes S31 gas-material circulation. S31 gas-material circulation is: the gas discharged from S2 atomization powder making and hydrogenation and which has passed the inspection is introduced into the gas rapid heating device through the gas circulation pressurization device to form a gas-material circulation system.

10. A method for preparing a magnesium-based hydride powder according to claim 6, characterized in that: The process parameters for hydrogenation mixed gas are as follows: gas pressure is 3-8 MPa, the mixed gas is hydrogen and argon, the hydrogen content is controlled at 20-200 ppm, the temperature is 100-400℃, and the gas flow rate is controlled at 500-3000 m3 / h; the atomization hydrogenation powder production gas pressure is controlled at 3-8 MPa, and the process temperature for magnesium-based metal molten liquid atomization hydrogenation powder production is 700-1200℃; the atomization hydrogenation powder production device also includes a guide pipe, which must withstand the continuous scouring of molten metal above 1200℃ and high-pressure hydrogen and argon mixed gas at 8 MPa and below 400℃ for 8 hours with an inner diameter change of less than 2%.

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