CN207659078U - Magnesium hydride preparation equipment - Google Patents
Magnesium hydride preparation equipment Download PDFInfo
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- CN207659078U CN207659078U CN201721181631.3U CN201721181631U CN207659078U CN 207659078 U CN207659078 U CN 207659078U CN 201721181631 U CN201721181631 U CN 201721181631U CN 207659078 U CN207659078 U CN 207659078U
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- magnesium
- preparation equipment
- collecting chamber
- transitional storehouse
- heater
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Abstract
The utility model proposes a kind of magnesium hydride Preparation equipment, which includes：Transitional storehouse, transitional storehouse include feeding port；Room is heated, heating room is connected by the first valve with transitional storehouse；Heater, heater upper end opening and can be moved by the first valve between transitional storehouse and heating room, and heater is used for the magnesium raw material wherein placed in oven heats；Collecting chamber, collecting chamber are connected with heating room to collect magnesium powder by conduit；And reative cell, reative cell is connected with collecting chamber by the second valve to receive magnesium powder, and reative cell is connected with external hydrogen air source to receive hydrogen.The utility model proposes magnesium hydride Preparation equipment by magnesium powder prepare and hydrogenation be attached to an equipment, and it is succinct using the magnesium hydride preparation method step of the magnesium hydride Preparation equipment, and wherein can be by the size controlling of hydrogenation magnesium granules obtained in the range of 1 μm 60 μm by the control of the conditions such as temperature, pressure.
Description
Technical field
The utility model is related to the preparations of magnesium hydride, more particularly, to a kind of magnesium hydride Preparation equipment.
Background technology
Magnesium hydride (MgH2), pale powder is single light metal hydride, and normal temperature and pressure stability inferior is higher, density
For 1.45g/cm3, hydrogen storage content 7.6%, far above Mg base hydrogen bearing alloy hydride and other metal hydrides.Magnesium hydride can be with
It is reacted at normal temperatures with water, generates hydrogen.It also is used as catalyst, reducing agent etc. simultaneously.
Mg-based material belongs to medium temperature type hydrogen storage alloy, easily stores, reaction condition is mild, and by-product is environmental-friendly, is to have
The hydrogen storage material of development prospect.Relative to other metal hydrogen storage materials, magnesium-base hydrogen storage material has the following advantages：Hydrogen storage content is high；
It is resourceful, it is cheap；It is good that magnesium-base hydrogen storage material inhales hydrogen release platform so that the utilization rate of hydrogen improves；Hydride is relatively stablized, and puts
Hydrogen needs higher temperature, and most of hydrogen discharging temperatures are at 200 DEG C or more.
The preparation method of magnesium hydride includes thermally decomposing to be made under magnesium hydride, magnesium powder normal pressure using alkyl magnesium to catalyze and synthesize hydrogenation
Magnesium and suppress to obtain magnesium hydride etc. using magnesium powder heating plus hydrogen.
The particle size of commercially available magnesium hydride is larger and expensive, is easily generated in unreacted hydrogenation magnesium surface when hydrolytic hydrogen production
Passivating film and hinder reaction continue, cannot be used directly for hydrogen manufacturing.Accordingly, it is considered to using magnesium powder made from magnesium-base metal, then
Hydrogenated obtained magnesium hydride.
Existing magnesium hydride preparation method is the equipment or instrument for sequentially or simultaneously using two kinds or more, realizes powder
It prepares, collect, the process of hydrogenation.Such as need the operations such as ultrasound, centrifugation, cleaning, heating and thermal insulation using sol-gal process.No
Specified otherwise is simultaneously based on existing common sense, it is believed that these operations need to realize on the instrument and equipment of different function, for example surpass
Sound machine, centrifuge etc.；For another example precursor is first obtained using ball mill grinding or lapping mode after being sintered, is placed into real in hydrogen environment
It now hydrogenates, and the hydrogenation process is also required to realize on different instrument and equipments, for example uses ball mill, mortar, tube furnace
Deng.It is standby that any one method cannot achieve hydrogenation magnesium dust integration system in a single device, to give processing band
Difficulty is carried out.Therefore it is particularly necessary with the device of hydrogenation to propose prepared by a kind of integrated powder.
On the other hand, that there are granulation uniformities is poor for the hydrogenation magnesium dust that existing magnesium hydride preparation method is prepared, or
Particle size excessive (being usually 150 μm or more) or too small (being usually 1 μm or less) etc., particle size is crossed conference and is led to not directly
For hydrogen manufacturing, and the too small then magnesium hydride low yield of particle and severe reaction conditions, danger.Therefore it needs more perfect and advanced
Technology of preparing and device realize the control being distributed to diameter of particle.
Utility model content
In order to solve the above technical problems, the utility model proposes a kind of magnesium hydride Preparation equipment, magnesium hydride preparation is set
It is standby to include：
Transitional storehouse, transitional storehouse include feeding port；
Room is heated, heating room is connected by the first valve with transitional storehouse, it is preferable that heating room further includes the inflation of heating room
Mouth is to be filled with inert gas；
Heater, the upper end opening of heater can simultaneously be moved between transitional storehouse and heating room by the first valve, added
The magnesium raw material that hot device is used to place in the oven heats heaters；
Collecting chamber, collecting chamber are connected with heating room to collect magnesium powder by conduit；With
Reative cell, reative cell are connected by the second valve with collecting chamber to receive magnesium powder, and reative cell and external hydrogen
Air source is connected to receive hydrogen.
In one embodiment, magnesium hydride Preparation equipment further includes vacuum extractor, and vacuum extractor is connected with transitional storehouse
It connects, and transitional storehouse is additionally provided with transitional storehouse inflating port to be filled with inert gas.
In one embodiment, magnesium hydride Preparation equipment further includes guide rail, and guide rail passes through the first valve to be arranged in transitional storehouse
It is indoor with heating, and guide rail is connected with the first control power supply to transmit heater.
In one embodiment, heater includes：
Crucible, crucible is for holding magnesium raw material, it is preferable that the material of crucible is boron nitride, graphite, magnesia and stainless
One kind in steel；
Inductance coil, inductance coil are arranged around the outside of crucible to heat magnesium raw material；With
Second control power supply, the second control power supply are connect with inductor wire astragal to control heating temperature.
In one embodiment, one end that conduit is connected to heating room has ever-expanding first opening of cross-sectional area,
First opening is arranged towards the upper end of heater to collect magnesium steam.
In one embodiment, first resistor silk insulating layer, and first resistor silk insulating layer are provided on the outside of conduit
It is connected with third control power supply.
In one embodiment, collecting chamber further includes：
Electric whitewashing, electric whitewashing have horizon bar and vertical bar, and being provided at both ends with for horizon bar can be with collecting chamber
The brush head of inner wall contact, vertical bar are connected to the point midway of horizon bar, so that horizon bar can be in the control of the 4th control power supply
System is lower to be rotated horizontally and can be moved up and down along the axial direction of vertical bar around vertical bar；
Magnesium powder exports, and magnesium powder outlet is arranged in the bottom of collecting chamber and is connected with the second valve；With
Cooling layer is provided with cooling layer on the outside of collecting chamber and collects indoor magnesium steam with cooling, it is preferable that cooling layer is
Circulating water layer, circulating water layer are connected with external water source.
In one embodiment, one end that conduit is connected to collecting chamber has ever-expanding second opening in cross section.
In one embodiment, reative cell further includes second resistance silk insulating layer, second resistance silk insulating layer and the 5th control
Power supply processed is connected.
In one embodiment, magnesium raw material is in pure magnesium, magnesium alloy, magnesium-rare earth, Mg-Zr alloys, magnesium-nickel, magnesium-alliance
One or more combinations, and in magnesium raw material magnesium content between 60wt%-99.999wt%, other constituent contents exist
Between 0.001wt%-40wt%.
The utility model proposes magnesium hydride Preparation equipment overcome in existing magnesium hydride preparation process powder collect it is difficult
The problem of, and preparation process is simple, and spacing collects the integration of magnesium powder and hydrogenation automatically；By controlling adding for magnesium raw material
The cooling temperature of hot temperature, the argon pressure of transitional storehouse, the holding temperature of first resistor silk insulating layer on the outside of conduit, cooling layer
Realize the control of magnesium hydride diameter of particle distribution, ensure by the particle diameter distribution of equipment hydrogenation magnesium dust obtained 1 μm-
In the range of 60 μm, solve the problems, such as that grain size is excessive and too small.
Description of the drawings
Fig. 1 shows the structural schematic diagram of the magnesium hydride Preparation equipment according to one exemplary embodiment of the utility model；
Fig. 2 shows the XRD spectras of the hydrogenation magnesium dust prepared according to the utility model first embodiment；
Fig. 3 shows the size distribution plot of the hydrogenation magnesium dust prepared according to the utility model first embodiment；
Fig. 4 shows the XRD spectra of the hydrogenation magnesium dust prepared according to the utility model second embodiment；
Fig. 5 shows the size distribution plot of the hydrogenation magnesium dust prepared according to the utility model second embodiment；
Fig. 6 shows the XRD spectra of the hydrogenation magnesium dust prepared according to the utility model 3rd embodiment；With
Fig. 7 shows the size distribution plot of the hydrogenation magnesium dust prepared according to the utility model 3rd embodiment.
Specific implementation mode
Illustrative, non-limiting embodiment of the utility model are described in detail with reference to the accompanying drawings, to new according to this practicality
The magnesium hydride Preparation equipment of type is further described.
Referring to Fig.1, according to the utility model proposes magnesium hydride Preparation equipment include transitional storehouse 1, heating room 2, heater 6
(including crucible 61 and inductance coil 62), collecting chamber 4 and reative cell 5, wherein transitional storehouse 1 pass through the first valve 12 and heating room 2
It is connected, heating room 2 is connected by conduit 3 with collecting chamber 4, and collecting chamber 4 is connected by the second valve 44 with reative cell 5,
Heater 6 can move between transitional storehouse 1 and heating room 2 to complete input and the heating of magnesium raw material.
Transitional storehouse 1 enters the transition warehouse before reative cell 5 as heater 6, for completing dosing operation.Transitional storehouse 1
Including feeding port 11, in the heater 6 that magnesium raw material input is parked in transitional storehouse 1 by feeding port 11.Furthermore it is also possible to
Transitional storehouse 1 manufactures vacuum environment and inert gas environment reacts to avoid magnesium elements in magnesium raw material with the oxygen etc. in air, under
It will elaborate to this in text.In one embodiment, magnesium raw material be pure magnesium, magnesium alloy, magnesium-rare earth, Mg-Zr alloys,
One or more combinations in magnesium-nickel and magnesium-manganese, and in magnesium raw material magnesium elements content in 60wt%-99.999wt%
Between, other constituent contents are between 0.001wt%-40wt%.It will be understood by those skilled in the art that for making
The magnesium raw material of standby magnesium hydride is not limited to enumerating above.
Heating room 2 is connected by the first valve 12 with transitional storehouse 1.Preferably, heating room 2 further includes that heating room 2 is inflated
Mouth (not shown), to be filled with inert gas, to manufacture inert atmosphere in heating room 2.Feeding is completed in transitional storehouse 1
Afterwards, heater 6 enters heating room 2 by the first valve 12, is then turned off the first valve 12 with interior to magnesium therein in heating room 2
Raw material is heated.
Heater 6 is the container that can be heated to the magnesium raw material wherein held, and 6 upper end opening of heater so that
The magnesium steam of vaporization rises and enters collecting chamber 4 by conduit 3.In one embodiment, which further includes
Guide rail 63.The setting of guide rail 63 is in transitional storehouse 1 and heating room 2 and passes through the first valve 12.As such, it is desirable to by heater 6 from
When transitional storehouse 1 is transferred to heating room 2, sends control signal by the first control power supply direction guiding rail 63 and electric energy is provided and led with starting
Heater 6 is sent to heating room 2 by rail 63, guide rail 63, and realization automatically controls.
Collecting chamber 4 is connected to heating room 2 to receive magnesium steam by conduit 3.Magnesium steam can be gradually cold in collecting chamber 4
It coagulates as magnesium powder, and then collects the magnesium powder for hydrogenation.
Reative cell 5 is connected to collecting chamber 4 to receive magnesium powder by the second valve 44, and reative cell 5 passes through hydrogen inlet
52 are connected to external hydrogen air source (not shown), external hydrogen air source can to the hydrogenation in reative cell 5 provide hydrogen and
It is adapted to the hydrogen pressure of hydrogenation.Magnesium powder is entered by the second valve 44 after reative cell 5 reacts with the hydrogen in reative cell 5
Obtain hydrogenation magnesium granules.
With continued reference to Fig. 1, in one embodiment of the utility model, which further includes vacuum means
13 are set, is connected with transitional storehouse 1 to carry out vacuum pumping to transitional storehouse 1.Transitional storehouse 1 be additionally provided with transitional storehouse inflating port with
Pour inert gas.In this way, after the heater 6 into transitional storehouse 1 launches magnesium raw material, closes the first valve 12 and use vacuumizes
Device 13 executes vacuum pumping to transitional storehouse 1, then pours inert gas into transitional storehouse 1 by transitional storehouse inflating port, from
And manufacture inert environments enter heating room 2 to avoid air from the first valve 12 in transitional storehouse 1.
In one embodiment, heater 6 controls power supply including crucible 61, inductance coil 62 and second and (does not show in figure
Go out).
Crucible 61 is the container of upper end opening, for holding magnesium raw material.Inductance coil 62 is arranged around the outside of crucible 61
To carry out electrical induction to the magnesium raw material in crucible 61 in energization.Second control power supply connects with 62 line of inductance coil
It connects, which can vaporize required temperature according to the magnesium in magnesium raw material and provide electric energy to inductance coil 62, to
Realize automatically controlling for magnesium raw material heating temperature.The material of crucible 61 disclosed by the utility model can be boron nitride, graphite, oxygen
Change one kind in magnesium and stainless steel, but not limited to this.
In one embodiment, there is cross-sectional area ever-expanding first to open for one end that conduit 3 is connected to heating room 2
Mouthful, and the first opening is arranged towards the upper end (opening of crucible 61) of heater 6 to collect magnesium steam.Further, conduit 3
The one end for being connected to collecting chamber 4 has ever-expanding second opening in cross section.In this way, passing through cross-sectional area ever-expanding
One opening can as often as possible collect the magnesium steam vaporized in heater 6, improve the utilization rate of magnesium raw material；Not by cross-sectional area
Disconnected widened second opening can accelerate the speed that magnesium steam is discharged into collecting chamber 4, to accelerate magnesium steam condensation rate.Into one
Step ground is arranged to ensure not condensed during magnesium steam flow to collecting chamber 4 from heating room 2 in the outside of conduit 3
First resistor silk insulating layer 31.First resistor silk insulating layer 31 is connected with third control power supply (not shown), third control
The temperature for the current control first resistor silk insulating layer 31 that power supply processed is provided by control to first resistor silk insulating layer 31, to protect
The temperature in conduit 3 is demonstrate,proved on the condensation point of magnesium steam；In addition, after the magnesium powder in collecting chamber 4 fully enters reative cell 5,
Third control power supply stops powering to first resistor silk insulating layer 31.
With continued reference to Fig. 1, the utility model proposes magnesium hydride Preparation equipment in collecting chamber 4 further include electric whitewashing
42, magnesium powder outlet 43 and cooling layer 41.
Electric whitewashing 42 is arranged inside collecting chamber 4, and has horizon bar and vertical bar.Horizon bar is provided at both ends with
The brush head that can be contacted with the inner wall of collecting chamber 4；The point midway of vertical bar and horizon bar connects, so that horizon bar can be the
Four control power supply (not shown)s control under around vertical bar rotate horizontally and can be along the axial direction of vertical bar
Lower movement.In this way, under the control of the 4th control power supply, horizon bar does not move up and down simultaneously or simultaneously around vertical bar
With horizontally rotate, magnesium powder on 4 inner wall of collecting chamber is adsorbed on to clean, to improve the collection efficiency of magnesium powder.Magnesium powder outlet 43
It is arranged in the bottom of collecting chamber 4 and is connected with the second valve 44, the magnesium powder collected in collecting chamber 4 exports 43 Hes by magnesium powder
Second valve 44 enters reative cell 5.Meanwhile in order to improve the condensation rate of magnesium steam, cooling layer is set in the outside of collecting chamber 4
41.Preferably, cooling layer 41 is circulating water layer 41, and circulating water layer 41 is connected with external water source (not shown)
It is logical.
Referring to Fig.1, the reative cell 5 in magnesium hydride Preparation equipment disclosed by the utility model further includes and the 5th control power supply
(not shown) is connected second resistance silk insulating layer 51.In this way, with hydrogen hydrogenation occurs for the magnesium powder in reative cell 5
When, temperature of the 5th control power supply needed for hydrogenation is suitable to ensure to the offer electric energy of second resistance silk insulating layer 51
Reaction temperature, to achieve the purpose that improve hydrogenation efficiency.
As shown in the above description, magnesium powder is prepared and is integrated with hydrogenation by magnesium hydride Preparation equipment provided by the utility model
In same complete equipment, overcomes powder in conventional manufacturing process and collect difficult problem.In addition, the magnesium hydride Preparation equipment knot
Structure is simple, and the conditions realization such as temperature, pressure in each step prepared to magnesium powder preparation, magnesium hydride automatically controls.
The step of magnesium hydride being prepared with reference to Fig. 1 explanations using above-mentioned magnesium hydride Preparation equipment.
First, heater 6 is moved to transitional storehouse 1, is put into magnesium raw material in heater 6 by feeding port 11.It is feeding intake
In the process, it closes transitional storehouse 1 and heats the first valve 12 between room 2.After the completion of feeding intake, transitional storehouse 1 is taken out using vacuum pump
Vacuum is to pressure 10-4Pa-10-2Between Pa, and inert gas (example is filled with into transitional storehouse 1 by transitional storehouse inflating port
Such as, argon gas), the pressure of inert gas is filled between 0.005MPa-0.1MPa.
Then, the first valve 12 is opened, is transmitted heater 6 in transitional storehouse 1 and the guide rail 63 in heating room 2 by being arranged
To heating room 2, the first valve 12 is closed, inert gas is passed through (for example, argon gas, fills into heating room 2 by heating room inflating port
The pressure of the inert gas entered is between 0.01MPa-0.1MPa), magnesium raw material is heated with life using heater 6 in heating room 2
At magnesium steam.It is using the method that heater 6 heats magnesium raw material：It is powered to inductance coil 62 by the second control power supply, and
Second control power supply by control the heating temperature of current control inductance coil 62 provided to inductance coil 62 650 DEG C-
Between 1100 DEG C, realize that the magnesium vaporization in magnesium raw material generates magnesium steam.
Then, the magnesium steam generated in heating room 2 enters collecting chamber 4 by conduit 3 and is condensed into gradually in collecting chamber 4
Magnesium powder, and then magnesium powder is collected in collecting chamber 4.During magnesium steam flows in conduit 3, in order to ensure that magnesium steam does not occur
Condensation controls the first resistor silk insulating layer 31 that power supply is wrapped up to 3 outside of conduit by third and powers so that first resistor silk is protected
31 pairs of magnesium steam of warm layer play the role of heat preservation, and third control power supply is provided by control to first resistor silk insulating layer 31
Electric current the holding temperature of first resistor silk insulating layer 31 is controlled between 650 DEG C -1000 DEG C.Collecting chamber 4 collects magnesium powder
Step further includes：Magnesium steam enters collecting chamber 4 by conduit 3；Cooling layer 41 is opened so that magnesium steam is condensed into magnesium powder；Pass through
Four control power initiation electric whitewashings 42, horizon bar is rotated horizontally around vertical bar simultaneously or non-concurrently along vertical bar
Axial direction moves up and down, to clean the magnesium powder on attachment 4 side wall of collecting chamber；The magnesium powder of collection is by being arranged in collecting chamber 4
The magnesium powder outlet 43 of bottom and the second valve 44 enter reative cell 5.The temperature of the cooling water of cooling layer 41 is passed through at 20 DEG C -50 DEG C
Between, pressure between 0.5MPa-2MPa, to realize best cooling effect.
Finally, it after the magnesium powder that collecting chamber 4 is collected enters reative cell 5 by the second valve 44, is passed through into reative cell 5
Hydrogen generates hydrogenation magnesium granules to be reacted with magnesium powder.In hydrogenation process, the 5th control power supply is protected by control to second resistance silk
The electric current that warm layer 51 provides controls the holding temperature of second resistance silk insulating layer 51 between 200 DEG C -450 DEG C.In reative cell 5
The reaction time of hydrogen and magnesium powder is between -40 hours 1 hour.In addition, collecting chamber 4 collect magnesium powder by the second valve 44 into
After entering reative cell 5, before being passed through hydrogen into reative cell 5, stop the heating of heater 6, stop third and control power supply to the
The power supply of one resistance wire insulating layer 31 stops the 4th control power supply to the power supply of electric whitewashing 42 and closes the second valve 44.
Illustrate the example that magnesium hydride is prepared using magnesium hydride Preparation equipment provided by the utility model below in conjunction with the accompanying drawings.
Embodiment one
The feeding port 11 of transitional storehouse 1 is opened, pure magnesium raw material is put into the heater 6 into transitional storehouse 1, closes transitional storehouse 1
Feeding port 11, simultaneously close off the first valve 12.Vacuum environment is manufactured in transitional storehouse 1 using vacuum extractor 13, is led to simultaneously
Transitional storehouse inflating port is crossed to the argon gas that 1 charged pressure of transitional storehouse is 0.02MPa.
The first valve 12 is opened, by the first control power initiation guide rail 63, heater 6 is made to be moved to heating along guide rail 63
Room 2 is then shut off the first valve 12.It is the argon gas of 0.02MPa to heating 2 charged pressure of room by heating 2 inflating port of room, and leads to
Cross second control power supply to the inductance coil 62 of heater 6 power so that heater 6 crucible 61 in temperature rise to 800 DEG C, earthenware
Pure magnesium raw material in crucible 61 melts, evaporates magnesium steam.
Magnesium steam enters collecting chamber 4 by conduit 3, at the same by temperature be 20 DEG C, the recirculated cooling water that pressure is 2MPa leads to
Enter cooling layer 41, so that the magnesium steam in cooling collecting chamber 4 is condensed into magnesium powder, and electric whitewashing 42 is controlled by the 4th control power supply
Rotation is to collect magnesium powder.
After magnesium powder enters reative cell 5 by the second valve 44, the heating of the heating, closing conduit 3 that stop heater 6 is protected
Temperature closes the second valve 44, is powered to second resistance silk insulating layer 51 so that 5 temperature of reative cell maintains by the 5th control power supply
At 400 DEG C, while the hydrogen for being passed through to reative cell 5 4MPa starts to hydrogenate.
After hydrogenation 10 hours, hydrogen inlet 52 is closed, from 5 collecting reaction product powder of reative cell.
XRD tests are carried out to powder made from embodiment one, as shown in Fig. 2, the XRD spectrum is shown made from embodiment one
Pure magnesium hydride (MgH in powder2) content is higher, there is MgH2Crystal face characteristic peak and a small amount of Mg characteristic peaks.Embodiment one is made
Powder carries out nano particle size test, as shown in figure 3, powder particle volume average particle size is 15.211 μm, has higher consistent
Property.
Embodiment two
The feeding port 11 of transitional storehouse 1 is opened, magnesium alloy raw material is put into the heater 6 into transitional storehouse 1, closes transition
The feeding port 11 in storehouse 1 simultaneously closes off the first valve 12.Vacuum environment is manufactured in transitional storehouse 1 using vacuum extractor 13, simultaneously
By transitional storehouse inflating port to 1 charged pressure of transitional storehouse be 0.03MPa argon gas.
The first valve 12 is opened, by the first control power initiation guide rail 63, heater 6 is made to be moved to heating along guide rail 63
Room 2 is then shut off the first valve 12.It is the argon gas of 0.03MPa to heating 2 charged pressure of room by heating 2 inflating port of room, and leads to
Cross second control power supply to the inductance coil 62 of heater 6 power so that heater 6 crucible 61 in temperature rise to 750 DEG C, earthenware
Magnesium alloy raw material in crucible 61 melts, generates magnesium steam.
Power supply is controlled by third to power to first resistor silk insulating layer 31, and the temperature in conduit 3 is made to maintain 750 DEG C.
Magnesium steam enters collecting chamber 4 by conduit 3, at the same by temperature be 30 DEG C, the recirculated cooling water that pressure is 1MPa is passed through cooling layer
41, so that the magnesium steam in cooling collecting chamber 4 is condensed into magnesium powder, and by the 4th control power supply control the rotation of electric whitewashing 42 with
Collect magnesium powder.
After magnesium powder enters reative cell 5 by the second valve 44, the heating of the heating, closing conduit 3 that stop heater 6 is protected
Temperature closes the second valve 44, is powered to second resistance silk insulating layer 51 so that 5 temperature of reative cell maintains by the 5th control power supply
At 360 DEG C, while the hydrogen for being passed through to reative cell 5 3MPa starts to hydrogenate.
After hydrogenation 15 hours, hydrogen inlet 52 is closed, from 5 collecting reaction product powder of reative cell.
XRD tests are carried out to powder made from embodiment two, as shown in figure 4, the XRD spectrum is shown made from embodiment two
Contain MgH in powder simultaneously2And Mg, and main component is MgH2.Powder is made to embodiment two and carries out nano particle size test,
As shown in figure 5, powder particle volume average particle size is 18.646 μm, particle size is in normal distribution.
Embodiment three
The feeding port 11 of transitional storehouse 1 is opened, magnesium alloy raw material is put into the heater 6 into transitional storehouse 1, closes transition
The feeding port 11 in storehouse 1 simultaneously closes off the first valve 12.Vacuum environment is manufactured in transitional storehouse 1 using vacuum extractor 13, simultaneously
By transitional storehouse inflating port to 1 charged pressure of transitional storehouse be 0.03MPa argon gas.
The first valve 12 is opened, by the first control power initiation guide rail 63, heater 6 is made to be moved to heating along guide rail 63
Room 2 is then shut off the first valve 12.It is the argon gas of 0.03MPa to heating 2 charged pressure of room by heating 2 inflating port of room, and leads to
Cross second control power supply to the inductance coil 62 of heater 6 power so that heater 6 crucible 61 in temperature rise to 750 DEG C, earthenware
Magnesium alloy raw material in crucible 61 melts, generates magnesium steam.
Power supply is controlled by third to power to first resistor silk insulating layer 31, and the temperature in conduit 3 is made to maintain 750 DEG C.
Magnesium steam enters collecting chamber 4 by conduit 3, at the same by temperature be 25 DEG C, the recirculated cooling water that pressure is 1MPa is passed through cooling layer
41, so that the magnesium steam in cooling collecting chamber 4 is condensed into magnesium powder, and by the 4th control power supply control the rotation of electric whitewashing 42 with
Collect magnesium powder.
After magnesium powder enters reative cell 5 by the second valve 44, the heating of the heating, closing conduit 3 that stop heater 6 is protected
Temperature closes the second valve 44, is powered to second resistance silk insulating layer 51 so that 5 temperature of reative cell maintains by the 5th control power supply
At 380 DEG C, while the hydrogen for being passed through to reative cell 5 3MPa starts to hydrogenate.
After hydrogenation 5 hours, hydrogen inlet 52 is closed, from 5 collecting reaction product powder of reative cell.
XRD tests are carried out to powder made from embodiment three, as shown in fig. 6, the XRD spectrum is shown made from embodiment three
Powder is MgH2Content reaches 95% MgH2With Mg combined grindings.Nano particle size test is carried out to powder made from embodiment three,
As shown in fig. 7, powder particle volume average particle size is 5.922 μm, particle size is in normal distribution.
By above-described embodiment it is found that using the utility model proposes magnesium hydride Preparation equipment overcome existing magnesium hydride system
Powder collects difficult problem during standby, and preparation process is simple, and spacing collects magnesium powder and the one of hydrogenation automatically
Change；Pass through the heat preservation of the first resistor silk insulating layer on the outside of the control heating temperature of magnesium raw material, the argon pressure of transitional storehouse, conduit
Temperature, cooling layer cooling temperature realize the control of magnesium hydride diameter of particle distribution, ensure using equipment hydrogenation obtained
The particle diameter distribution of magnesium dust solves the problems, such as that grain size is excessive and too small in the range of 1 μm -60 μm.
Claims (13)
1. a kind of magnesium hydride Preparation equipment, wherein the magnesium hydride Preparation equipment includes：
Transitional storehouse, the transitional storehouse include feeding port；
Room is heated, the heating room is connected by the first valve with the transitional storehouse；
Heater, the upper end opening of the heater simultaneously can be by first valves in the transitional storehouse and the heating room
Between move, the heater in the heating room for heating the magnesium raw material placed in the heater；
Collecting chamber, the collecting chamber are connected with the heating room to collect magnesium powder by conduit；With
Reative cell, the reative cell are connected by the second valve with the collecting chamber to receive the magnesium powder, and described anti-
Room is answered to be connected to receive hydrogen with external hydrogen air source.
2. magnesium hydride Preparation equipment according to claim 1, wherein the heating room further includes heating room inflating port to fill
Enter inert gas.
3. magnesium hydride Preparation equipment according to claim 1, wherein the magnesium hydride Preparation equipment further includes vacuum means
It sets, the vacuum extractor is connected with the transitional storehouse, and the transitional storehouse is additionally provided with transitional storehouse inflating port to be filled with
Inert gas.
4. magnesium hydride Preparation equipment according to claim 1, wherein the magnesium hydride Preparation equipment further includes guide rail, institute
It is indoor in the transitional storehouse and the heating across first valve setting to state guide rail, and the guide rail and the first control electricity
Source is connected to transmit the heater.
5. magnesium hydride Preparation equipment according to claim 1, wherein the heater includes：
Crucible, the crucible is for holding magnesium raw material；
Inductance coil, the inductance coil are arranged around the outside of the crucible to heat magnesium raw material；With
Second control power supply, the second control power supply are connect with the inductor wire astragal to control heating temperature.
6. magnesium hydride Preparation equipment according to claim 5, wherein the material of the crucible is boron nitride, graphite, oxidation
One kind in magnesium and stainless steel.
7. magnesium hydride Preparation equipment according to claim 1, wherein the conduit is connected to one end tool of the heating room
There are ever-expanding first opening of cross-sectional area, first opening to be arranged towards the upper end of the heater to collect magnesium steaming
Vapour.
8. magnesium hydride Preparation equipment according to claim 7, wherein be provided with first resistor silk guarantor on the outside of the conduit
Warm layer, and the first resistor silk insulating layer is connected with third control power supply.
9. magnesium hydride Preparation equipment according to claim 1, wherein the collecting chamber further includes：
Electric whitewashing, the electric whitewashing have horizon bar and vertical bar, the horizon bar be provided at both ends with can with it is described
The brush head of the inner wall contact of collecting chamber, the vertical bar is connected to the point midway of the horizon bar, so that the horizon bar energy
It is enough to be rotated horizontally around the vertical bar under the control of the 4th control power supply and be along the axial direction of the vertical bar
Lower movement；
Magnesium powder exports, and the magnesium powder outlet is arranged in the bottom of the collecting chamber and is connected with second valve；With
Cooling layer is provided with cooling layer on the outside of the collecting chamber and collects indoor magnesium steam so that cooling is described.
10. magnesium hydride Preparation equipment according to claim 9, wherein the cooling layer is circulating water layer, described to follow
Ring water cooling layer is connected with external water source.
11. magnesium hydride Preparation equipment according to claim 1, wherein the conduit is connected to one end of the collecting chamber
With ever-expanding second opening in cross section.
12. magnesium hydride Preparation equipment according to claim 1, wherein the reative cell further includes the heat preservation of second resistance silk
Layer, the second resistance silk insulating layer are connected with the 5th control power supply.
13. magnesium hydride Preparation equipment according to claim 1, wherein the magnesium raw material is that pure magnesium, magnesium alloy, magnesium-are dilute
One kind in soil, Mg-Zr alloys, magnesium-nickel, magnesium-manganese.
Priority Applications (1)
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| CN201721181631.3U CN207659078U (en) | 2017-09-15 | 2017-09-15 | Magnesium hydride preparation equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585742A (en) * | 2017-09-15 | 2018-01-16 | 上海镁源动力科技有限公司 | Magnesium hydride Preparation equipment and magnesium hydride preparation method |
| CN112723309A (en) * | 2020-12-30 | 2021-04-30 | 榆林学院 | Industrial production device for magnesium hydride |
-
2017
- 2017-09-15 CN CN201721181631.3U patent/CN207659078U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585742A (en) * | 2017-09-15 | 2018-01-16 | 上海镁源动力科技有限公司 | Magnesium hydride Preparation equipment and magnesium hydride preparation method |
| CN107585742B (en) * | 2017-09-15 | 2019-06-28 | 上海镁源动力科技有限公司 | Magnesium hydride Preparation equipment and magnesium hydride preparation method |
| CN112723309A (en) * | 2020-12-30 | 2021-04-30 | 榆林学院 | Industrial production device for magnesium hydride |
| CN112723309B (en) * | 2020-12-30 | 2023-08-01 | 榆林学院 | Industrial production device of magnesium hydride |
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Granted publication date: 20180727 Effective date of abandoning: 20190628 |