CN102583244A - Method and device for preparing magnesium hydride - Google Patents
Method and device for preparing magnesium hydride Download PDFInfo
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- CN102583244A CN102583244A CN2012100375376A CN201210037537A CN102583244A CN 102583244 A CN102583244 A CN 102583244A CN 2012100375376 A CN2012100375376 A CN 2012100375376A CN 201210037537 A CN201210037537 A CN 201210037537A CN 102583244 A CN102583244 A CN 102583244A
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- reaction kettle
- magnesium hydride
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Abstract
The invention relates to a method for preparing magnesium hydride and also relates to a device for preparing the magnesium hydride. The device for preparing the magnesium hydride comprises a reaction kettle, an inserted plate valve, a first heating coil, a second heating coil, a first gas inlet, a gas inlet and outlet port and a gas outlet, wherein the inserted plate valve is arranged in the reaction kettle and is positioned at the middle part of the reaction kettle to divide the reaction kettle into an upper part and a lower part; the first heating coil is arranged at the lower part of the reaction kettle; the second heating coil is arranged at the upper part of the reaction kettle; the first gas inlet is arranged on the side wall of the upper part of the reaction kettle; the gas inlet and outlet port is arranged on the side wall of the upper part of the reaction kettle; and the gas outlet is arranged on the side wall of the upper part of the reaction kettle. In the method for preparing the magnesium hydride, the device for preparing the magnesium hydride is adopted. The device disclosed by the invention solves the technical problem that a high temperature and a high hydrogen pressure are required for preparing the magnesium hydride currently.
Description
Technical field
The present invention relates to a kind of method for preparing magnesium hydride, also relate to a kind of device for preparing magnesium hydride.
Background technology
Magnesium hydride (MgH
2), claim magnesium hydride again, be a kind of inorganic salt, outward appearance is pale powder, and crystalline structure is a tetragonal system, and density is 1.45g/cm
3
MgH
2Belong to covalant hydrides, it forms enthalpy is-74.5kJ/mol that stable at normal temperatures and pressures higher, the suction hydrogen discharging temperature is generally up to 623-673K.MgH
2Under vacuum, 280 ℃ of decomposition.MgH
2Be weakly alkaline, be insoluble to common organic solvents, inflammable and have a pungency.MgH
2Can not be used for replacing hydrolith as hydrogen source or siccative, can not replace sodium hydride in organic reaction as alkaline condensing agent, because of its alkalescence too a little less than, but can form polymkeric substance, so can be used to prepare inorganic aggretion type hydrogenate and be used for fireworks.MgH
2Be very strong reductive agent, contacting with water is enough to produce hydrogen; Contact with methyl alcohol, generate magnesium alkoxide and hydrogen.With hydroborons or aluminum hydride effect, can generate two hydrogenate.
MgH
2Hydrogen content up to 7.65%, have potential use widely: as hydrogen storage material, from theoretical hydrogen storage capability, it is the first-selection in the metal hydrogen storage material; Be used for hydrogen manufacturing, it at normal temperatures hydrolytic reactions discharge hydrogen, be suitable for portable nitrogenous source as instant hydrogen manufacturing; In addition, MgH
2Because above-mentioned character can also be used as catalyzer, reductive agent and produce high pure metal powder etc.
At present, MgH
2The preparation method mainly contain two kinds: a kind of is to carry out thermolysis with alkyl magnesium; Another kind is to be raw material with the magnesium powder, the direct down and H-H reaction in pressurization, heating and getting.
But the hydrogenation process of above-mentioned magnesium powder need conditions such as higher temperature and hydrogen pressure (temperature 300-400 ℃, 10-15MPa).Present commercially available polycrystalline MgH
2Powder not only costs an arm and a leg, and grain-size is thick, and during as hydrogen storage material, it is extremely slow to inhale hydrogen desorption kinetics; During hydrolytic hydrogen production also owing to generate Mg (OH)
2Passive film is coated on unreacted MgH
2The surface causes hydrolysis reaction speed significantly to descend or reaction can't be proceeded, and therefore can't directly be used to store up hydrogen or hydrolytic hydrogen production.
Summary of the invention
First aspect present invention technical problem to be solved provides a kind of device for preparing magnesium hydride.
The present invention solves the problems of the technologies described above through following technical scheme, reaches the object of the invention.
A kind of device for preparing magnesium hydride comprises:
Reaction kettle, said reaction kettle comprise open reaction kettle body and close said open lid;
The plate valve, said plate valve is arranged in the said reaction kettle, is positioned at the middle part of said reaction kettle, and said reaction kettle is divided into the upper and lower;
First heater coil, said first heater coil is arranged at the bottom of said reaction kettle;
Second heater coil, said second heater coil is arranged at the top of said reaction kettle;
First inlet mouth, said first inlet mouth is arranged at the sidewall on the top of said reaction kettle;
Air inlet/outlet, said air inlet/outlet is arranged at the sidewall on the top of said reaction kettle;
The air outlet, said air outlet is arranged at the sidewall on the top of said reaction kettle.
The device of preparation magnesium hydride of the present invention, simple in structure.Because be provided with said reaction kettle and said first heater coil, can allow the magnesium powder in device of the present invention, to become magnesium steam and meet condensation and form magnesium granules, again with hydrogen reaction.The effect of first heater coil is in order to become the Mg powder with Mg piece evaporation and condensation; The effect of second heater coil is that heating makes Mg and H
2Reaction; Reaction kettle is divided into top and the bottom, and two heater coils, the control that helps reacting are set.
When the present invention implemented, preferably, the device of said preparation magnesium hydride also comprised vacuum pump, and said vacuum pump is connected with said air outlet.Said vacuum pump is used for said reaction kettle is vacuumized.
When the present invention implemented, preferably, the device of said preparation magnesium hydride also comprised sources of hydrogen, and said sources of hydrogen is connected with said first inlet mouth.Said sources of hydrogen is responsible in said reaction kettle, hydrogen being provided, and forms hydrogen pressure.
When the present invention implemented, preferably, the device of said preparation magnesium hydride also comprised thermofin, and said thermofin wraps up said second heater coil.Said thermofin is used for heat insulation, to keep the temperature of reaction in the said reaction kettle.Further, said thermofin is an asbestos layer.
When the present invention implemented, preferably, the device of said preparation magnesium hydride also comprised the first control power supply, and the said first control power supply is connected with said first heater coil.The said first control power supply is used to control the electric current that flows to said first heater coil.
When the present invention implemented, preferably, the device of said preparation magnesium hydride also comprised the second control power supply, and the said second control power supply is connected with said second heater coil.The said second control power supply is used to control the electric current that flows to said second heater coil.
The technical problem of second aspect to be solved of the present invention provides a kind of method for preparing magnesium hydride.
A kind of method for preparing magnesium hydride adopts the device of foregoing preparation magnesium hydride, may further comprise the steps:
1) with the MAG block open container of packing into, places said first heater coil then;
2) sealing said reaction kettle and close said first inlet mouth, air inlet/outlet and said air outlet;
3) from said air outlet said reaction kettle is vacuumized, close said air outlet then;
4) in the vacuum environment of said reaction kettle, through said first heater coil said MAG block heating evaporation is become magnesium vapor, the said magnesium vapor of part condenses into the magnesium powder on the top of said reaction kettle;
5) close said plate valve and break off said first heater coil, to said reaction kettle, charge into hydrogen from said first inlet mouth;
6) through said second heater coil heating, and insulation, let said magnesium powder, said magnesium vapor and said hydrogen react;
7) break off said second heater coil, cooling lets the said magnesium hydride that generates be deposited on the inwall of said reaction kettle;
8) passivation is collected and is obtained said magnesium hydride.
When the present invention implemented, preferably, in said step 3), said reaction kettle is vacuumized was to be evacuated to 10
-3-10
-2Pa.
When the present invention implemented, preferably, in said step 4), said the MAG block heating evaporation is become magnesium vapor was to be heated to 650-750 ℃.
When the present invention implemented, preferably, in said step 6), said heating was to be heated to 350-420 ℃, and the time of said insulation is 10h～20h.
The present invention utilizes magnesium powder, magnesium vapor to prepare magnesium hydride, and the technology of preparation is simple, efficient, only needs that the Mg piece is put into equipment and just can original position produce magnesium hydride, and the magnesium hydride purity that makes is high.
Below will combine accompanying drawing that the technique effect of design of the present invention, concrete characteristic and generation is described further, so that those skilled in the art understands the object of the invention, characteristic and effect fully.
Description of drawings
Fig. 1 is the structural representation of the device of preparation magnesium hydride of the present invention.
Fig. 2 is the XRD figure spectrum of the white powder that reaction generates among the embodiment 1.
Fig. 3 is the XRD figure spectrum of the white powder that reaction generates among the embodiment 2.
Fig. 4 is the DSC/TGA graphic representation of the white powder that reaction generates among the embodiment 1.
Embodiment
The method for preparing magnesium hydride of the present invention in general, may further comprise the steps:
A) reaction vessel is vacuumized;
B) in the vacuum environment of reaction vessel, the MAG block heating evaporation is become magnesium vapor, the magnesium vapor of part condenses into the magnesium powder on the top of reaction vessel;
C) in reaction vessel, charge into hydrogen;
D) heating, and insulation let magnesium powder, magnesium vapor and hydrogen react;
E) cooling lets the magnesium hydride that generates be deposited on the inwall of reaction vessel;
F) passivation is collected and is obtained magnesium hydride.
In step a), it is to be evacuated to 10 that reaction vessel is vacuumized
-3-10
-2Pa.In step b), it is to be heated to 650-750 ℃ that the MAG block heating evaporation is become magnesium vapor.In step c), charging into hydrogen is 5-8MPa until pressure.In step d), heating is to be heated to 350-420 ℃ of insulation then, and the time of insulation is 10h～20h.
As shown in Figure 1, in order to realize top method, the present invention proposes following a kind of device for preparing magnesium hydride.The device of this preparation magnesium hydride comprises: reaction kettle 1, plate valve 2, first heater coil 3, second heater coil, first inlet mouth 121, air inlet/outlet (not shown), air outlet 122, vacuum pump 5, sources of hydrogen 6, thermofin 7, the first control power supply 8, the second control power supply 9.
Use the device of this embodiment, practical implementation is of the present invention, and to prepare the step of method of magnesium hydride following:
1) opens lid, the plate valve 2 of reaction kettle 1,, place first heater coil 3 then, open container 4 preferably ceramic crucibles the MAG block open container 4 of packing into;
2) lid of off-response still 1, sealed reactor 1 is also closed inlet mouth 121, air inlet/outlet and air outlet 122;
3) open air outlet 122,121 reaction kettle 1 is evacuated to 10 from the air outlet with vacuum pump 5
-3-10
-2Pa closes air outlet 122 then;
4) through the first control power supply, 8 closed first heater coils 3, in the vacuum environment of reaction kettle 1, through first heater coil 3 MAG block is heated to 650-750 ℃, makes MAG block flash to magnesium vapor, the magnesium vapor of part condenses into the magnesium powder on the top of reaction kettle;
5) close plate valve 2 and break off first heater coil 3, to reaction kettle, charge into hydrogen from inlet mouth 121 with vacuum pump 5 through the first control power supply 8, to air pressure be 5-8MPa;
6) through the second control power supply, 9 closed second heater coils, be heated to 350-420 ℃ of insulation then through second heater coil, let magnesium powder, magnesium vapor and hydrogen react, the time of insulation is 10h～20h;
7) break off second heater coil through the second control power supply 9, cooling lets the magnesium hydride that generates be deposited on the inwall of reaction kettle 1;
8) lid of reaction kettle 1 is opened in passivation then, scrapes the settling that is deposited on reaction kettle 1 inwall with stainless steel steel spoon, collects and obtains magnesium hydride.Concrete passivation mode is to open air inlet/outlet, the remaining H of extraction reaction
2, put into air.
In following examples, adopt D/max 2550VL/PCX x ray diffractometer x (Cu-K α) to carry out the XRD test.
1) opens lid, the plate valve 2 of reaction kettle 1, go into ceramic crucible (bore is slightly less than first heater coil 3) with pure Mg is packaged, place first heater coil 3 of reaction kettle 1 bottom 11 then;
2) lid of off-response still 1, inlet mouth 121, air inlet/outlet and air outlet 122 are with reaction kettle 1 sealing;
3) open vacuum pump 5 and air outlet 122, be evacuated to 10
-2Pa closes vacuum pump 5 and air outlet 122 then;
4) open 3 work of the first control power supply, 8, the first heater coils, be heated to 650 ℃, make the evaporation of Mg piece, the Mg steam is met cold meeting to reaction kettle 1 top 12 and is deposited on the inwall of reaction kettle, and being heated to 650 ℃ of used times is 5 hours;
5) close the plate valve 2 and the first control power supply 8, charge into H
2To 6MPa;
6) open 9, the second heater coil work of the second control power supply, be heated to 350 ℃ of insulations then, make Mg and H
2Fully reaction, soaking time is 20 hours;
7) close second heater coil, make reaction kettle 1 naturally cooling, powder deposition is on reaction kettle 1 inwall;
8) collect the powder that obtains white after the passivation.
Powder to above-mentioned prepared white carries out XRD (X-ray diffraction spectrum) test.As shown in Figure 2, at following angle place MgH appears successively
2The crystal face characteristic peak (be angle before the bracket; Be corresponding crystal face in the bracket): 28.1 (110), 35.920 (101), 40.089 (200), 54.747 (211), 57.543 (220), 61.539 (002), 64.425 (310), 68.766 (112), 70.178 (301), 75.891 (202), 83.599 (321), 89.333 (222), 92.790 (330), 96.011 (312), 96.966 (411), 99.301 (420); As shown in Figure 2, MgH
2The crystal face characteristic peak explain that very sharply crystalline content is more, crystal is purer; Mg and MgO have a spot of characteristic peak to occur and also relative intensity low; So the XRD figure spectrum shows MgH in the powder that makes
2Purity is high.Fig. 4 is the DSC/TGA graphic representation of the powder (be 25 hours heat-up time) of the white that makes, and test is carried out test condition in the anti-STA of the speeding 449F3 of Germany type DSC/TGA instrument: argon gas atmosphere, flow velocity 30ml/min; 10 ℃/min of temperature rise rate; TR is 20-550 ℃.DSC curve among Fig. 4 has an endotherm(ic)peak about 440 ℃, with MgH
2Hydrogen discharging temperature conform to, proved MgH
2Generation.
1) opens lid, the plate valve 2 of reaction kettle 1, go into ceramic crucible (bore is slightly less than first heater coil 3) with pure Mg is packaged, place first heater coil 3 of reaction kettle 1 bottom 11 then;
2) lid of off-response still 1, inlet mouth 121, air inlet/outlet and air outlet 122 are with reaction kettle 1 sealing;
3) open vacuum pump 5 and air outlet 122, be evacuated to 10
-2Pa closes vacuum pump 5 and air outlet 122 then;
4) open 3 work of the first control power supply, 8, the first heater coils, be heated to 700 ℃, make the evaporation of Mg piece, the Mg steam is met cold meeting to the top 12 of reaction kettle 1 and is deposited on the inwall of reaction kettle, and being heated to 700 ℃ of used times is 5 hours;
5) close the plate valve 2 and the first control power supply 8, charge into H
2To 8MPa;
6) open 9, the second heater coil work of the second control power supply, be heated to 400 ℃ of insulations then, make Mg and H
2Fully reaction, soaking time is 20 hours;
7) close second heater coil, make reaction kettle 1 naturally cooling, powder deposition is on reaction kettle 1 inwall;
8) collect the powder that obtains white after the passivation.
Powder to above-mentioned prepared white carries out XRD (X-ray diffraction spectrum) test: as shown in Figure 3, and at following angle place MgH appears successively
2Crystal face characteristic peak (being angle before the bracket, is corresponding crystal face in the bracket): 28.1 (110), 35.920 (101), 40.089 (200), 54.747 (211), 57.543 (220), 61.539 (002), 64.425 (310), 68.766 (112), 70.178 (301), 75.891 (202), 83.599 (321), 89.333 (222), 92.790 (330), 96.011 (312), 96.966 (411), 99.301 (420).As shown in Figure 3, the XRD figure spectrum shows MgH in the powder that makes
2Purity is high.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area need not creative work and just can design according to the present invention make many modifications and variation.Therefore, all technician in the art all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology through the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. a device for preparing magnesium hydride is characterized in that, comprising:
Reaction kettle, said reaction kettle comprise open reaction kettle body and close said open lid;
The plate valve, said plate valve is arranged in the said reaction kettle, is positioned at the middle part of said reaction kettle, and said reaction kettle is divided into the upper and lower;
First heater coil, said first heater coil is arranged at the bottom of said reaction kettle;
Second heater coil, said second heater coil is arranged at the top of said reaction kettle;
First inlet mouth, said first inlet mouth is arranged at the sidewall on the top of said reaction kettle;
Air inlet/outlet, said air inlet/outlet is arranged at the sidewall on the top of said reaction kettle;
The air outlet, said air outlet is arranged at the sidewall on the top of said reaction kettle.
2. the device of preparation magnesium hydride as claimed in claim 1 is characterized in that, also comprises: vacuum pump, said vacuum pump is connected with said air outlet.
3. the device of preparation magnesium hydride as claimed in claim 1 is characterized in that, also comprises: sources of hydrogen, said sources of hydrogen is connected with said first inlet mouth.
4. the device of preparation magnesium hydride as claimed in claim 1 is characterized in that, also comprises: thermofin, said thermofin wrap up said second heater coil.
5. the device of preparation magnesium hydride as claimed in claim 1 is characterized in that, also comprises: the first control power supply, the said first control power supply is connected with said first heater coil.
6. the device of preparation magnesium hydride as claimed in claim 1 is characterized in that, also comprises: the second control power supply, the said second control power supply is connected with said second heater coil.
7. a method for preparing magnesium hydride is characterized in that, adopts the device like each described preparation magnesium hydride of claim 1-6, may further comprise the steps:
1) with the MAG block open container of packing into, places said first heater coil then;
2) sealing said reaction kettle and close said first inlet mouth, air inlet/outlet and said air outlet;
3) from said air outlet said reaction kettle is vacuumized, close said air outlet then;
4) in the vacuum environment of said reaction kettle, through said first heater coil said MAG block heating evaporation is become magnesium vapor, the said magnesium vapor of part condenses into the magnesium powder on the top of said reaction kettle;
5) close said plate valve and break off said first heater coil, to said reaction kettle, charge into hydrogen from said first inlet mouth;
6) through said second heater coil heating, and insulation, let said magnesium vapor, said magnesium powder and said hydrogen react;
7) break off said second heater coil, cooling lets the said magnesium hydride that generates be deposited on the inwall of said reaction kettle;
8) passivation is collected and is obtained said magnesium hydride.
8. the method for preparing magnesium hydride as claimed in claim 7 is characterized in that: in said step 3), said reaction kettle is vacuumized is to be evacuated to 10
-3-10
-2Pa.
9. the method for preparing magnesium hydride as claimed in claim 7 is characterized in that: in said step 4), said the MAG block heating evaporation is become magnesium vapor is to be heated to 650-750 ℃.
10. the method for preparing magnesium hydride as claimed in claim 7 is characterized in that: in said step 6), said heating is to be heated to 350-420 ℃, and the time of said insulation is 10h～20h.
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|---|---|---|---|
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| CN103028734A (en) * | 2013-01-14 | 2013-04-10 | 北京科技大学 | Method for preparing nanometer magnesium |
| 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 |
| CN109616617A (en) * | 2018-11-30 | 2019-04-12 | 中国计量大学 | A kind of foam conductive net/silicium cathode material preparation facilities and control method |
| WO2019095627A1 (en) * | 2017-11-16 | 2019-05-23 | 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 |
| CN109972159A (en) * | 2019-04-08 | 2019-07-05 | 镁格氢动能源技术(苏州)有限公司 | Water power energy-storage system based on solid hydrogen technology |
| CN110067702A (en) * | 2019-04-08 | 2019-07-30 | 镁格氢动能源技术(苏州)有限公司 | Wind-powered electricity generation energy-storage system based on solid hydrogen technology |
| CN112723309A (en) * | 2020-12-30 | 2021-04-30 | 榆林学院 | Industrial production device for magnesium hydride |
| CN115709972A (en) * | 2022-12-13 | 2023-02-24 | 上海氢美健康科技有限公司 | Method for preparing hydrogen magnesium element by adopting hydrogen air breaking equipment |
| US11813675B2 (en) | 2017-11-16 | 2023-11-14 | Shanghai Mg Power Technology Co., Ltd | Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder |
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|---|---|---|---|---|
| CN103028734A (en) * | 2013-01-14 | 2013-04-10 | 北京科技大学 | Method for preparing nanometer magnesium |
| CN103028734B (en) * | 2013-01-14 | 2015-02-11 | 北京科技大学 | Method for preparing nanometer magnesium |
| 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 |
| WO2019052120A1 (en) * | 2017-09-15 | 2019-03-21 | 上海镁源动力科技有限公司 | Magnesium hydride preparation apparatus and magnesium hydride preparation method |
| 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 |
| JP2020534228A (en) * | 2017-09-15 | 2020-11-26 | シャンハイ エムジー パワー テクノロジー カンパニー リミテッド | Magnesium hydride production equipment and magnesium hydride production method |
| JP7013485B2 (en) | 2017-09-15 | 2022-01-31 | シャンハイ エムジー パワー テクノロジー カンパニー リミテッド | Magnesium hydride production equipment and magnesium hydride production method |
| WO2019095627A1 (en) * | 2017-11-16 | 2019-05-23 | 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 |
| US11813675B2 (en) | 2017-11-16 | 2023-11-14 | Shanghai Mg Power Technology Co., Ltd | Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder |
| CN109616617A (en) * | 2018-11-30 | 2019-04-12 | 中国计量大学 | A kind of foam conductive net/silicium cathode material preparation facilities and control method |
| CN109972159A (en) * | 2019-04-08 | 2019-07-05 | 镁格氢动能源技术(苏州)有限公司 | Water power energy-storage system based on solid hydrogen technology |
| CN110067702A (en) * | 2019-04-08 | 2019-07-30 | 镁格氢动能源技术(苏州)有限公司 | Wind-powered electricity generation energy-storage system based on solid hydrogen technology |
| 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 |
| CN115709972A (en) * | 2022-12-13 | 2023-02-24 | 上海氢美健康科技有限公司 | Method for preparing hydrogen magnesium element by adopting hydrogen air breaking equipment |
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