CN114436213B - Method for preparing magnesium hydride powder in large scale and integrated device - Google Patents
Method for preparing magnesium hydride powder in large scale and integrated device Download PDFInfo
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- CN114436213B CN114436213B CN202111598758.6A CN202111598758A CN114436213B CN 114436213 B CN114436213 B CN 114436213B CN 202111598758 A CN202111598758 A CN 202111598758A CN 114436213 B CN114436213 B CN 114436213B
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- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
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Abstract
The invention discloses a method for preparing magnesium hydride powder in a large scale and an integrated device, which comprise an air flow grinding chamber, an intermediate product collecting chamber, a reaction chamber and a product collecting chamber, wherein one side of the lower end of the air flow grinding chamber is connected with the intermediate product collecting chamber, the upper end of the air flow grinding chamber and the lower end of the intermediate product collecting chamber are both connected with the reaction chamber, and the lower end of the reaction chamber is connected with the product collecting chamber; the air flow grinding device is characterized in that one side of the upper end of the air flow grinding chamber is connected with a compressor, an electric heating layer is sleeved on the outer wall of the reaction chamber, an upper sealing head and a lower sealing head are respectively arranged at the upper end and the lower end of the reaction chamber, the lower end of the reaction chamber is connected with a hydrogen supply tank, and a heat insulation antistatic device is arranged inside the upper end of the collection chamber. The invention utilizes the characteristics of good brittleness and good ductility of magnesium cores of magnesium hydride, and can obtain finer high-purity magnesium hydride powder through grinding by circulating air flow.
Description
Technical Field
The invention relates to the technical field of magnesium hydride preparation, in particular to a method for preparing magnesium hydride powder in a large scale and an integrated device.
Background
Direct hydrogenation of magnesium powder is an effective method for preparing magnesium hydride at low cost, and it is generally considered that the size of magnesium powder material determines the reaction efficiency of magnesium powder and hydrogen and the yield of magnesium hydride, and magnesium nanocrystallization is a key for efficiently preparing high-purity magnesium hydride powder.
Through mass search, the prior art is found that the publication number is: CN109795987a discloses an integrated apparatus for preparing magnesium hydride powder and a method for preparing magnesium hydride powder. The apparatus of the present invention comprises a heating chamber for heating a magnesium-based metallic material to produce metallic droplets; the powder preparation chamber comprises an atomizing device, and the atomizing device is used for atomizing metal liquid drops and then cooling the metal liquid drops to form metal powder; a collection chamber for collecting and screening metal powder; and a reaction chamber for subjecting the metal powder to a hydrogenation reaction to form magnesium hydride powder. The device is of an integrated structure, and is simple in structure and convenient to operate; the whole process for preparing the magnesium hydride powder can be completed in one device, and the automation control can be realized. The method is simple and easy to implement, and the obtained product has moderate size, uniform particles and excellent performance.
In summary, because magnesium has good ductility and is very active in aerobic and water environments, and the large-scale efficient preparation of nano-scale magnesium ultrafine powder under a low-water and low-oxygen inert atmosphere is very difficult, an effective method for large-scale efficient preparation of magnesium hydride powder is still lacking at present.
Disclosure of Invention
The invention aims to provide a method for preparing magnesium hydride powder in a large scale and an integrated device, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the integrated device for preparing the magnesium hydride powder on a large scale comprises an air flow grinding chamber, an intermediate product collecting chamber, a reaction chamber and a product collecting chamber, wherein one side of the lower end of the air flow grinding chamber is connected with the intermediate product collecting chamber, the upper end of the air flow grinding chamber and the lower end of the intermediate product collecting chamber are both connected with the reaction chamber, and the lower end of the reaction chamber is connected with the product collecting chamber;
the air flow grinding device is characterized in that one side of the upper end of the air flow grinding chamber is connected with a compressor, an electric heating layer is sleeved on the outer wall of the reaction chamber, an upper sealing head and a lower sealing head are respectively arranged at the upper end and the lower end of the reaction chamber, the lower end of the reaction chamber is connected with a hydrogen supply tank, and a heat insulation antistatic device is arranged inside the upper end of the collection chamber.
Preferably, the upper end of the air flow grinding chamber is provided with a hatch cover for inputting materials, and a material returning valve is arranged between the air flow grinding chamber and the reaction chamber.
Preferably, a rotary valve is arranged at the joint of the air flow grinding chamber and the intermediate product collecting chamber.
Preferably, an emergency evacuation port is formed in the upper end of the upper seal head.
Preferably, a product blanking valve is arranged between the lower seal head and the product collecting chamber.
The method for preparing magnesium hydride powder on a large scale comprises the steps that the air flow grinding chamber is used for grinding magnesium-based metal materials to generate magnesium-based metal material ultrafine powder, wherein the magnesium-based metal materials are magnesium powder, magnesium-aluminum alloy, magnesium-nickel alloy, magnesium-rare earth alloy, magnesium-ferric oxide mixture, magnesium-graphite mixture, magnesium-aluminum oxide mixture and the like, the magnesium content of the alloy is 80-99.9wt%, the particle size of the air flow grinding chamber for the magnesium-based metal materials is 35 micrometers-2 millimeters, and the air flow grinding chamber can be used for preparing the magnesium-based metal material ultrafine powder with the size of 1-6 micrometers;
the intermediate product collecting chamber is used for collecting the prepared magnesium-based metal material ultrafine powder so as to obtain metal powder with a specified particle size range, so that the reaction efficiency of magnesium powder and hydrogen is improved, and the particle size of the magnesium hydride powder is more uniform;
the reaction chamber is used for preparing high-purity magnesium hydride powder by reacting magnesium-based metal material ultrafine powder with hydrogen, the reaction pressure is 2-5Mpa, and the reaction temperature is 200-450 ℃;
the product collecting chamber is used for collecting products with the particle size range meeting the requirement of the magnesium hydride powder, and the heat-insulating antistatic device is used for maintaining the temperature and the humidity of the product collecting chamber.
Preferably, the compressor is used for filling inert gas argon into the air flow grinding chamber, and the inert gas serves as initial purge gas of the system to remove moisture and oxygen in the system; secondly, the fluidized gas is used as a grinding chamber;
the material returning valve is used for controlling the airflow of the partially hydrogenated magnesium-based metal material ultrafine powder to be conveyed back to the airflow grinding chamber for secondary grinding.
Preferably, the electric heating layer is used for providing heat for the reaction of the magnesium-based metal material and the hydrogen, and the controllable temperature range is 30-500 ℃;
the product blanking valve is used for controlling magnesium hydride powder produced by the reaction chamber to be collected into the product collecting chamber.
Preferably, the air flow grinding chamber can prepare superfine magnesium-based metal material powder with the size of 1-6 microns, the superfine magnesium-based metal material powder enters the reaction chamber to react with hydrogen for 3-15 hours under the pressure of 250-400 ℃ and 2-3.5Mpa, and then a product with magnesium hydride as a shell and magnesium as a core is formed;
the reacted product is returned to the air flow grinding chamber for secondary grinding, the brittleness of the magnesium hydride is better, the shell layer of the magnesium hydride is peeled off, and the ductility of the magnesium core is better, and the particle size is reserved completely and further refined; the intermediate product after secondary grinding enters a reaction chamber to react again for 2-8 hours under the same condition, and after 2-5 times of circulation, the 1-3.5 micron grade high-purity magnesium hydride powder can be obtained.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, by utilizing the characteristics of better brittleness of magnesium hydride, falling off of a magnesium hydride shell layer and good ductility of a magnesium core, the superfine powder of a magnesium-based metal material with the size of 1-6 microns can be prepared by adopting the air flow grinding chamber, and then the superfine powder enters the reaction chamber to react with hydrogen for 3-15 hours under the pressure of 2-3.5Mpa at the temperature of 250-400 ℃ to form a product taking magnesium hydride as a shell and magnesium as a core, and the reacted product returns to the air flow grinding chamber to be ground for the second time, because the brittleness of the magnesium hydride is better, the magnesium shell layer is fallen off, the magnesium core is kept more completely because of good ductility, the grain size is further thinned, and the intermediate product after the second grinding enters the reaction chamber to react for the second time for 2-8 hours under the same condition. After 2-5 times of circulation, the high-purity magnesium hydride powder with the size of 1-3.5 microns can be obtained.
Drawings
FIG. 1 is a schematic diagram of a preparation apparatus according to the present invention.
In the figure: 1. an air flow grinding chamber; 11. a hatch cover; 12. a compressor; 13. a return valve; 2. an intermediate collection chamber; 21. rotating the valve; 3. a reaction chamber; 31. an emergency evacuation port; 32. an upper end enclosure; 33. an electrical heating layer; 34. a lower end enclosure; 35. a product blanking valve; 36. a hydrogen supply tank; 4. a product collection chamber; 41. a heat-insulating antistatic device.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific direction, be configured and operated in the specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "provided," "connected," and the like are to be construed broadly, and may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Referring to fig. 1, two embodiments of the present invention are provided:
embodiment one:
the integrated device for preparing the magnesium hydride powder in a large scale comprises an air flow grinding chamber 1, an intermediate product collecting chamber 2, a reaction chamber 3 and a product collecting chamber 4, wherein one side of the lower end of the air flow grinding chamber 1 is connected with the intermediate product collecting chamber 2, the upper end of the air flow grinding chamber 1 is provided with a hatch cover 11 for inputting materials, a material returning valve 13 is arranged between the air flow grinding chamber 1 and the reaction chamber 2, the upper end of the air flow grinding chamber 1 and the lower end of the intermediate product collecting chamber 2 are both connected with the reaction chamber 3, a rotary valve 21 is arranged at the joint of the air flow grinding chamber 1 and the intermediate product collecting chamber 2, and the lower end of the reaction chamber 3 is connected with the product collecting chamber 4;
the upper end side of the air flow grinding chamber 1 is connected with a compressor 12, the compressor 12 is used for filling inert gas argon into the air flow grinding chamber 1, and the inert gas serves as initial purge gas of the system to remove moisture and oxygen in the system; secondly, the fluidized gas is used as a grinding chamber;
the outer wall of the reaction chamber 3 is sleeved with an electric heating layer 33, the upper end and the lower end of the reaction chamber 3 are respectively provided with an upper sealing head 32 and a lower sealing head 34, the upper end of the upper sealing head 32 is provided with an emergency emptying port 31, a product blanking valve 35 is arranged between the lower sealing head 34 and the product collecting chamber 4, the lower end of the reaction chamber 3 is connected with a hydrogen supply tank 36, the reaction chamber 3 is used for preparing high-purity magnesium hydride powder by reacting magnesium-based metal material ultrafine powder with hydrogen, the reaction pressure is 2-5Mpa, the reaction temperature is 200-450 ℃, and the emergency emptying port 31 is used for pressure relief under emergency conditions. The upper head 32 and lower head 34 are used to link and seal the reaction chamber and other components. The electric heating layer 33 is used for providing heat for the reaction of the magnesium-based metal material with hydrogen, and the temperature can be controlled to be in the range of 30-500 ℃. The product discharge valve 35 is used to control the collection of magnesium hydride powder produced in the reaction chamber into the product collection chamber 4. The hydrogen supply tank 36 is used to supply hydrogen for the reaction. The inside thermal-insulated antistatic device 41 that is provided with in the upper end of product collection room 4 realizes antistatic measure through the double-deck airtight metal cavity ground connection that the intermediate level is inert gas for the temperature and the humidity of maintaining product collection room 4.
Embodiment two:
the method for preparing magnesium hydride powder on a large scale comprises the steps that an air flow grinding chamber 1 is used for grinding magnesium-based metal materials to generate magnesium-based metal material ultrafine powder, wherein the magnesium-based metal materials are magnesium powder, magnesium-aluminum alloy, magnesium-nickel alloy, magnesium-rare earth alloy, magnesium-ferric oxide mixture, magnesium-graphite mixture, magnesium-aluminum oxide mixture and the like, the magnesium content of the alloy is 80-99.9wt%, the grain size of the air flow grinding chamber 1 for the magnesium-based metal materials is 35 micrometers-2 millimeters, and the size of the magnesium-based metal material ultrafine powder can be 1-6 micrometers;
the jet milling chamber 1 is a chamber for fluidized milling by closed circulation using argon gas as a milling medium. Argon is sprayed into the crushing chamber at high speed through the nozzle, magnesium-based metal material ultrafine powder is accelerated in the supersonic jet flow, and repeatedly impacted and collided in the crushing chamber to crush.
The intermediate product collecting chamber 2 is used for collecting the prepared magnesium-based metal material ultrafine powder, when the magnesium-based metal material ultrafine powder reaches the particle size range meeting the requirement, the rotary valve 21 is opened, and the ultrafine powder falls into the intermediate product collecting chamber 2 under the action of gravity to obtain metal powder in the specified particle size range, so that the reaction efficiency of magnesium powder and hydrogen is improved, and the particle size of magnesium hydride powder is more uniform;
the reaction chamber 3 is used for preparing high-purity magnesium hydride powder by reacting magnesium-based metal material ultrafine powder with hydrogen, the electric heating layer 33 heats the reaction chamber 3 to 200-450 ℃, hydrogen is filled into the reaction chamber 3, the magnesium-based metal powder with specified particle size range and the hydrogen are subjected to hydrogenation reaction under the pressure of 2-5Mpa, the reaction temperature of 200-450 ℃, the reaction pressure of 2-5Mpa and the reaction temperature of 200-450 ℃;
the product collection chamber 4 is used for collecting the product with the particle size range of magnesium hydride powder meeting the requirement, and the heat-insulating antistatic device 41 is used for maintaining the temperature and humidity of the product collection chamber 4.
The compressor 12 is used for filling inert gas argon into the air flow grinding chamber 1, and the inert gas serves as initial system purge gas to remove moisture and oxygen in the system; secondly, the fluidized gas is used as a grinding chamber;
the return valve 13 is used for controlling the air flow of the partially hydrogenated magnesium-based metal material ultrafine powder to be conveyed back to the air flow grinding chamber 1 for secondary grinding.
The electric heating layer 33 is used for providing heat for the reaction of the magnesium-based metal material and hydrogen, and the controllable temperature range is 30-500 ℃;
the product discharge valve 35 is used to control the collection of magnesium hydride powder produced in the reaction chamber 3 into the product collection chamber 4.
The air flow grinding chamber 1 can prepare superfine powder of magnesium-based metal material with the size of 1-6 microns, the superfine powder enters a reaction chamber to react with hydrogen for 3-15 hours under the pressure of 2-3.5Mpa at the temperature of 250-400 ℃, and then a product with magnesium hydride as a shell and magnesium as a core is formed;
the reacted product is returned to the air flow grinding chamber 1 for secondary grinding, the brittleness of the magnesium hydride is better, the shell layer of the magnesium hydride is peeled off, the ductility of the magnesium core is better, and the particle size is reserved completely for further refinement; the intermediate product after secondary grinding enters a reaction chamber 3 to react again for 2-8 hours under the same condition, and after 2-5 times of circulation, the 1-3.5 micron grade high-purity magnesium hydride powder can be obtained.
Working principle: the air flow grinding chamber 1 is used for grinding magnesium-based metal materials to generate magnesium-based metal material ultrafine powder, wherein the magnesium-based metal materials are magnesium powder, magnesium-aluminum alloy, magnesium-nickel alloy, magnesium-rare earth alloy, magnesium-ferric oxide mixture, magnesium-graphite mixture, magnesium-aluminum oxide mixture and the like, the magnesium content of the alloy is 80-99.9wt%, the particle size of the air flow grinding chamber 1 for the magnesium-based metal materials is 35 micrometers-2 millimeters, and the size of the air flow grinding chamber 1 for the magnesium-based metal materials can be 1-6 micrometers; the compressor 12 is used for filling inert gas argon into the air flow grinding chamber 1, the return valve 13 is used for controlling the air flow of the partially hydrogenated magnesium-based metal material ultrafine powder to be conveyed back to the air flow grinding chamber 1 for secondary grinding, the intermediate product collecting chamber 2 is used for collecting the prepared magnesium-based metal material ultrafine powder so as to obtain metal powder with a specified particle size range, so that the efficiency of the reaction of magnesium powder and hydrogen is improved, and the particle size of the magnesium hydride powder is more uniform; the reaction chamber 3 is used for preparing high-purity magnesium hydride powder by reacting magnesium-based metal material ultrafine powder with hydrogen, the reaction pressure is 2-5Mpa, and the reaction temperature is 200-450 ℃;
the product collection chamber 4 is used for collecting the product with the particle size range of magnesium hydride powder meeting the requirement, and the heat-insulating antistatic device 41 is used for maintaining the temperature and humidity of the product collection chamber 4. The reacted product is returned to the air flow grinding chamber 1 for secondary grinding, the brittleness of the magnesium hydride is better, the shell layer of the magnesium hydride is peeled off, the ductility of the magnesium core is better, and the particle size is reserved completely for further refinement; the intermediate product after secondary grinding enters a reaction chamber 3 to react again for 2-8 hours under the same condition, and after 2-5 times of circulation, the 1-3.5 micron grade high-purity magnesium hydride powder can be obtained.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. The utility model provides an integrated device of scale preparation magnesium hydride powder, includes air current grinding chamber (1), intermediate product collection room (2), reaction chamber (3) and product collection room (4), its characterized in that: one side of the lower end of the air flow grinding chamber (1) is connected with an intermediate product collecting chamber (2), the upper end of the air flow grinding chamber (1) and the lower end of the intermediate product collecting chamber (2) are both connected with a reaction chamber (3), and the lower end of the reaction chamber (3) is connected with a product collecting chamber (4);
the air flow grinding device is characterized in that one side of the upper end of the air flow grinding chamber (1) is connected with a compressor (12), an electric heating layer (33) is sleeved on the outer wall of the reaction chamber (3), an upper sealing head (32) and a lower sealing head (34) are respectively arranged at the upper end and the lower end of the reaction chamber (3), the lower end of the reaction chamber (3) is connected with a hydrogen supply tank (36), and a heat insulation antistatic device (41) is arranged in the upper end of the collecting chamber (4);
the upper end of the air flow grinding chamber (1) is provided with a hatch cover (11) for inputting materials, and a material return valve (13) is arranged between the air flow grinding chamber (1) and the reaction chamber (3);
the rotary valve (21) is arranged at the joint of the air flow grinding chamber (1) and the intermediate product collecting chamber (2).
2. An integrated apparatus for the large-scale production of magnesium hydride powder according to claim 1, wherein: an emergency evacuation port (31) is arranged at the upper end of the upper sealing head (32).
3. An integrated apparatus for the large-scale production of magnesium hydride powder according to claim 1, wherein: a product blanking valve (35) is arranged between the lower sealing head (34) and the product collecting chamber (4).
4. A method for producing magnesium hydride powder by an integrated apparatus for producing magnesium hydride powder on a large scale according to any one of claims 1 to 3, characterized in that: the airflow grinding chamber (1) is used for grinding magnesium-based metal materials to generate magnesium-based metal material ultrafine powder, wherein the magnesium-based metal materials are magnesium powder, magnesium-aluminum alloy, magnesium-nickel alloy, magnesium-rare earth alloy, magnesium-ferric oxide mixture, magnesium-graphite mixture and magnesium-aluminum oxide mixture, the magnesium content of the alloy is 80-99.9wt%, the particle size of the magnesium-based metal materials is 35 micrometers-2 millimeters, and the size of the magnesium-based metal material ultrafine powder prepared by the airflow grinding chamber (1) is 1-6 micrometers;
the intermediate product collecting chamber (2) is used for collecting the prepared magnesium-based metal material ultrafine powder to obtain metal powder with a specified particle size range, so that the reaction efficiency of magnesium powder and hydrogen is improved, and the particle size of magnesium hydride powder is more uniform;
the air flow grinding chamber (1) prepares superfine powder of magnesium-based metal material with the size of 1-6 microns, and the superfine powder enters a reaction chamber to react with hydrogen for 3-15 hours under the pressure of 2-3.5Mpa at the temperature of 250-400 ℃, and then a product with magnesium hydride as a shell and magnesium as a core is formed;
the reacted product returns to the air flow grinding chamber (1) for secondary grinding, the brittleness of magnesium hydride is better, the shell layer of the magnesium hydride is peeled off, the ductility of the magnesium core is better, and the particle size is remained completely for further refinement; allowing the secondary ground intermediate product to enter a reaction chamber (3) for reacting again for 2-8 hours under the same condition, and obtaining 1-3.5 micron grade high-purity magnesium hydride powder through 2-5 times of circulation;
the product collecting chamber (4) is used for collecting products with the particle size range of magnesium hydride powder meeting the requirement, and the heat-insulating antistatic device (41) is used for maintaining the temperature and the humidity of the product collecting chamber (4).
5. The method for preparing magnesium hydride powder on a large scale according to claim 4, wherein: the compressor (12) is used for filling inert gas argon into the airflow grinding chamber (1), and the inert gas acts as initial system purge gas to remove moisture and oxygen in the system; secondly, the fluidized gas is used as a grinding chamber;
the material returning valve (13) is used for controlling the airflow conveying and returning of the partially hydrogenated magnesium-based metal material ultrafine powder to the airflow grinding chamber (1) for secondary grinding.
6. The method for preparing magnesium hydride powder on a large scale according to claim 4, wherein: the electric heating layer (33) is used for providing heat for the reaction of the magnesium-based metal material and the hydrogen, and the temperature is controlled to be 30-500 ℃;
the product blanking valve (35) is used for controlling magnesium hydride powder produced by the reaction chamber (3) to be collected into the product collecting chamber (4).
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| US7998454B2 (en) * | 2007-05-10 | 2011-08-16 | Bio Coke Lab. Co. Ltd. | Method of producing magnesium-based hydrides and apparatus for producing magnesium-based hydrides |
| JP2014015346A (en) * | 2012-07-06 | 2014-01-30 | Bio Coke Lab Co Ltd | Method and apparatus for producing powder of magnesium-based hydride |
| CN103435041A (en) * | 2013-08-27 | 2013-12-11 | 北京化工大学 | Method and system for producing calcium carbide with biomass fuel |
| CN109795987B (en) * | 2017-11-16 | 2023-11-07 | 上海镁源动力科技有限公司 | Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder |
| CN110980740A (en) * | 2019-11-01 | 2020-04-10 | 新疆东方希望新能源有限公司 | Trichlorosilane production process and production system |
| CN112645284B (en) * | 2020-12-28 | 2022-04-19 | 山东国邦药业有限公司 | Preparation method of diborane |
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