CN103787276A - Composite material for preparing hydrogen through Mg-salt hydrolysis and preparation method of composite material - Google Patents
Composite material for preparing hydrogen through Mg-salt hydrolysis and preparation method of composite material Download PDFInfo
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- CN103787276A CN103787276A CN201310717778.XA CN201310717778A CN103787276A CN 103787276 A CN103787276 A CN 103787276A CN 201310717778 A CN201310717778 A CN 201310717778A CN 103787276 A CN103787276 A CN 103787276A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a composite material for preparing hydrogen through Mg-salt hydrolysis and a preparation method of the composite material. The composite material for preparing the hydrogen through the Mg-salt hydrolysis is prepared from magnesium powder and salts with the mole ratio of 1 to (0.01-0.045); the salts are one or more than two of AlCl3, KCl, NaCl, LiCl and MgCl2; the magnesium powder and the salts are grinded to prepare the composite material for preparing the hydrogen through the Mg-salt hydrolysis. The composite material for preparing the hydrogen through the Mg-salt hydrolysis can be used for a high-activity magnesium-based composite hydrogen production material for a vehicle-mounted mobile hydrogen source. According to the method, the salts and the metal magnesium powder are subjected to high-energy grinding and the reaction cavity of Mg is improved, so that a lot of hydrogen can be rapidly released under a room temperature and the speed is rapid at the high temperature. The method has the advantages that the cost of raw materials is low and the preparation process is simple, and is an ideal magnesium-based composite hydrogen production material capable of being industrially applied.
Description
Technical field
The present invention relates to magnesium base hydrogen manufacturing material field, be specifically related to a kind of Mg-salt hydrolysis hydrogen manufacturing matrix material and preparation method thereof.
Background technology
Hydrogen Energy, as a kind of desirable new forms of energy, is the substitute that replaces traditional fossil oil.Therefore, the development of Hydrogen Energy industry attracts wide attention in recent years.Hydrogen can pass through engine (ICEs) electrogenesis in next life of fuel cell (FCs) or hydrogen internal combustion engine, and this can be used for drive electronics, automobile, household electrical appliances etc.The hydrogen generation heat that also can directly burn, for housed device.The method of utilizing of this hydrogen is very environmental protection, and because it does not produce carbon emission, being therefore widely used of hydrogen fuel will significantly be reduced the negative impact of carbon emission to environment.But promote Hydrogen Energy and be still faced with many obstacles, namely lack the enough cost, efficient storage and the transporting method of hydrogen of low hydrogen production technology.
The industrial hydrogen of most is by chemical process, produces, for example hydrogen making by natural gas reformation from fossil oil.But these methods can be brought serious environmental pollution equally, and because it is still based on traditional fossil oil, this method can not continue muchly.At present, can pass through the Mg base hydrogen manufacturing material of method for hydrolysis hydrogen manufacturing, because its low consumption, relatively high hydrogen storage property and simple hydrogen change system attract wide attention.Such route of producing hydrogen is applicable to portable fuel battery very much.The hydrolysis reaction hydrogen manufacturing of Mg can have following reaction equation to represent:
Mg+2H
2O→Mg(OH)
2+H
2；
The activity of simple substance Mg in water is very low, can only discharge the hydrogen of little amount.But by the mode of ball milling, Mg powder can obviously be activated.Also can be together with other metals such as Ni ball milling, in the process of ball milling, the particle size of Mg can reduce, thereby has improved reactive behavior.What the metal of doping had simultaneously can form miniature galvanic cell with Mg, in suitable electrolyte solution, can aggravate its corrosion.Can also pass through Hydride Doped, use acidic solution, the ultrasonic means such as peel off improve Mg put hydrogen output and speed in water.But still to exist cost high for these methods at present, reactor caused to corrosion, the problem such as recovery and difficult treatment of hydrolysising by-product.
Application publication number is that CN101811667A(application number is 201010147696.2) Chinese invention patent application a kind of magnesium base hydride composite system for hydrolysis hydrogen production and its preparation method and application is disclosed, get magnesium powder and nickel powder, mol ratio is 30:1～49:1, be that under the catalyzer of magnesium powder and nickel powder mixture total weight amount 3～10% and the effect of appropriate organic dispersing agent, hydrogenation burnt together becomes at consumption, carry out again powerful mechanical ball milling, it is 95%～98% that magnesium hydride in gained magnesium base hydride composite system for hydrolysis hydrogen production accounts for hydride total weight percent, Magnesium nickel hydride is 2%～5%, described catalyzer is graphite, B, Al, La, Ca, V, Ce, one in Nb, magnesium hydride is MgH
2, Magnesium nickel hydride is Mg
2niH
4and Mg
2niH
0.3with arbitrarily than mixture.Magnesium powder, nickel powder are obtained to Magnesium nickel hydride and then be placed in MgCl after over hydrogenation burns till
2in solution, hydrolysis to be to obtain higher hydrogen manufacturing productive rate, but this method step complexity, cost is high, and gained hydride is oxidizable thereby and be not suitable for use in onboard hydrogen source and industrial applications in air.
Summary of the invention
The invention provides a kind of Mg-salt hydrolysis hydrogen manufacturing matrix material and preparation method thereof, can be used for the high activity magnesium-base composite hydrogen manufacturing material of vehicle-mounted mobile hydrogen source.The method is by salt and metal M g powder are carried out to high-energy ball milling, and the reactive behavior of the Mg of raising, makes it at room temperature just can put hydrogen by rapid, high volume, and when high temperature, speed is faster.The method raw materials cost is low, and preparation process is simple, is a kind of desirable magnesium base composite hydrogen manufacturing material that can industrial applications.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of Mg-salt hydrolysis hydrogen manufacturing matrix material, the magnesium powder and the salt that are 1:0.01-0.045 by mole proportioning are made, and described salt is AlCl
3, KCl, NaCl, LiCl, MgCl
2in one or more.
Using salt as additive and pure Mg powder carry out ball milling to obtain Mg-salt hydrolysis hydrogen manufacturing matrix material.The hydrogen manufacturing of Mg-salt hydrolysis is M (Mg): M (salt)=x:y by mole proportioning of matrix material, x=1, y=0.01-0.045; The method this matrix material is hydrolyzed in 25 ℃～80 ℃ tap water reaction.Mg is pure magnesium powder; Salt is AlCl
3, KCl, NaCl, LiCl, MgCl
2in one or more.
As preferably, described salt is AlCl
3.AlCl
3can fine catalysis magnesium powder react with water and generate hydrogen as additive, speed of reaction is stable, reaction temperature and, can control well, and reactive magnesium is comparatively complete, hydrogen yield is high.
As preferably, described Mg-salt hydrolysis hydrogen manufacturing matrix material, the magnesium powder and the salt that are 1:0.03 by mole proportioning are made.Mg-salt hydrolysis hydrogen manufacturing matrix material under this concrete mole of proportioning, hydrogen yield is ideal.
A preparation method for matrix material for the hydrogen manufacturing of Mg-salt hydrolysis, comprises the following steps:
Magnesium powder and salt ball milling are obtained to Mg-salt hydrolysis hydrogen manufacturing matrix material.
Claim to obtain magnesium powder and salt by a required composition mole proportioning, as preferably, described ball milling carries out in ball grinder, and at the mid-abrading-ball that is placed with of described ball grinder, further preferred, described ball grinder and abrading-ball are stainless steel.As preferably, described ball milling adopts planetary ball mill (model is QM-3SP4), the condition of described ball milling is: ratio of grinding media to material is that 25:1(is the mass ratio of abrading-ball and magnesium powder and salt quality sum), rotating speed is 350-450rpm, Ball-milling Time is 0.5h-10h.Before ball milling, in ball grinder, be filled with argon gas airtight protection.
The Mg-salt hydrolysis hydrogen manufacturing matrix material obtaining after ball milling carries out the hydrolysis hydrogen discharging performance test under normal temperature or higher temperature in tap water.The matrix material reaction that can be hydrolyzed in 25 ℃～80 ℃ tap water for the hydrogen manufacturing of Mg-salt hydrolysis.
Use ADM2000 type under meter (Agilent Technologies) to test and record the hydrogen manufacturing amount of matrix material, hydrolysising experiment carries out in the water bath that sets temperature.What adopt is ordinary tap water, and the water adding and the hydrogen manufacturing of Mg-salt hydrolysis are 200:1 with the mass ratio of matrix material, and the test duration is 1h.In experiment, see, by add the Mg-salt hydrolysis hydrogen manufacturing matrix material that obtains after salt ball milling activation can be at 25 ℃ of room temperatures with water rapid reaction and discharge hydrogen, initial maximum hydrogen manufacturing speed can reach 455.9mlmin
-1g
-1(Mg).Wherein, add 3mol%AlCl
3matrix material productive rate at 25 ℃ of normal temperature be 93.86%, initial maximum hydrogen manufacturing speed is 455.9ml min
-1g
-1(Mg), activation effect is best.Along with the rising of temperature, hydrogen manufacturing productive rate and hydrogen discharging rate have further lifting.At 45 ℃, can realize and in 1h, put hydrogen completely, hydrolysis reaction can complete fast in 1min at 80 ℃.
Compared with prior art, the present invention has following advantage:
One, raw materials cost is low, cheap and easy to get.Metal M g is cheap, and the salt of required use is also more cheap, is well suited for large-scale application.
Two, preparation process is simple.Be the method for ball milling due to what adopt, only need take in proportion raw material is put into ball milling certain hour on ball mill again, simple to operate.Technique of the present invention is simple, and gained matrix material puts that hydrogen response is fast, output is high, is a kind of onboard hydrogen source that can industrial applications.
Three, normal temperature can be put hydrogen fast, and output is high.By add obtain after salt ball milling matrix material can be at room temperature just can with water rapid reaction, discharge a large amount of hydrogen, productive rate can reach 93.86%.By adding salt ball milling, the activity of metal magnesium powder is greatly improved, under normal temperature, just can be hydrolyzed and put in a large number hydrogen, can be used for vehicle-mounted mobile hydrogen source.
Four, green energy conservation.Than modes such as electrolysis, the more simple environmental protection of magnesium hydrolytic hydrogen production flow process, does not produce hydrogen foreign gas in addition, simultaneously by product environmentally safe.
Accompanying drawing explanation
Fig. 1 is pure Mg and the Mg-salt hydrolysis hydrogen manufacturing matrix material that adds the different salt ball milling of 3mol% 6h gained in the Mg powder hydrolysis Hydrogen desorption isotherms comparison diagram in the time of 25 ℃ in embodiment 1;
Fig. 2 be pure Mg powder in embodiment 2 (under) and embodiment 1 in Mg-salt hydrolysis hydrogen manufacturing matrix material put hydrogen by product (on) XRD figure spectrum;
Fig. 3 is pure Mg and add different amount AlCl in Mg powder in embodiment 3
3the hydrogen manufacturing of ball milling 6h gained Mg-salt hydrolysis is the hydrolysis Hydrogen desorption isotherms comparison diagram in the time of 25 ℃ with matrix material;
Fig. 4 is Mg-3mol%AlCl in embodiment 4
3the hydrogen manufacturing of ball milling 3h gained Mg-salt hydrolysis is hydrolyzed Hydrogen desorption isotherms comparison diagram under differing temps with matrix material.
Embodiment
Compound front by the required salt powder of using 110 ℃ of oven dry 6h in vacuum drying oven, to remove the moisture (lower same) that wherein may contain.
Under protectiveness Ar atmosphere, weigh magnesium powder and the salt powder of designated ratio, mole proportioning of magnesium powder and salt is 1:0.03, puts into steel ball grinder (ball grinder and abrading-ball are stainless steel), and ratio of grinding media to material is 25:1, and tighten the screws is airtight.Ball grinder is put on QM-3SP4 planetary ball mill, setting speed 400rpm, it is even that the high speed ball milling that carries out 6h obtains composition, obtains active high Mg-salt hydrolysis hydrogen manufacturing matrix material.
Setting bath temperature is 25 ℃, takes 0.05g sample (being Mg-salt hydrolysis hydrogen manufacturing matrix material) and puts into reaction flask, by bottle sealing, adds 10ml ordinary tap water.The water adding contacts with bottom sample to trigger puts hydrogen, and the hydrogen of generation is derived via conduit, passes through under meter by condensation, drying installation after removing water vapour.The instant flow velocity of gas is determined, and under meter is connected with computer, and these data of specific software real time record are installed.After reaction 1h, add AlCl
3sample productive rate the highest, be 93.86%, initial maximum hydrogen manufacturing speed is 455.9ml min
-1g
-1(Mg).
The Mg-AlCl of maximum output will be had in embodiment 1
3the filtration of hydrogen product is put in the hydrolysis of composite hydrogen manufacturing material 1h, with after alcohol drip washing 3 times, after 65 ℃ of vacuum-drying, obtains filter cake, and it is carried out to XRD sign.Also pure Mg powder has been done to XRD and tested to contrast, scanning angle unification is 10 ° to 90 ° simultaneously.Can obviously find out by contrast, reaction product is magnesium hydroxide substantially, has no other impurity.
Embodiment 3
Under protectiveness Ar atmosphere, be M (Mg) by mole proportioning: M (AlCl
3)=x:y, x=1, y 0,0.01,0.02,0.03,0.045 the ratio of being respectively joins each component in steel ball grinder, and tighten the screws is airtight.It is all identical with embodiment 1 that the setting of ball milling parameter and sample are put hydrogen testing method.See and add AlCl
3can obviously improve Mg powder hydrogen manufacturing productive rate, the AlCl of Different adding amount
3there is different activation effects.Hydrogen manufacturing productive rate is along with AlCl
3the increase of addition is to rise and fall, and the addition of 3mol% (is magnesium powder and AlCl
3mole proportioning be 1:0.03) be experiment in activation effect best.
Embodiment 4
Under protectiveness Ar atmosphere, be M (Mg) by mole proportioning: M (AlCl
3)=x:y, x=1, the ratio of y=0.03 joins each component in steel ball grinder, and tighten the screws is airtight.Ball grinder is put on QM-3SP4 planetary ball mill, setting speed 400rpm, it is even that the high speed ball milling that carries out 3h obtains composition, obtains active high Mg-salt hydrolysis hydrogen manufacturing matrix material.Except the bath temperature difference setting, sample test method is consistent with embodiment 1.Along with the rising of temperature, it is faster that hydrolysis reaction becomes, and productive rate is higher.45 ℃ time Mg can be in 1h complete reaction, be swift in response at 80 ℃, can within the 1min time, react rapidly to productive rate 100%.
Claims (8)
1. a Mg-salt hydrolysis hydrogen manufacturing matrix material, is characterized in that, the magnesium powder and the salt that are 1:0.01-0.045 by mole proportioning are made, and described salt is AlCl
3, KCl, NaCl, LiCl, MgCl
2in one or more.
2. Mg-salt hydrolysis hydrogen manufacturing matrix material according to claim 1, is characterized in that, described salt is AlCl
3.
3. Mg-salt hydrolysis hydrogen manufacturing matrix material according to claim 1, is characterized in that, the magnesium powder and the salt that are 1:0.03 by mole proportioning are made.
4. the preparation method with matrix material according to the Mg-salt hydrolysis hydrogen manufacturing described in claim 1～3 any one, is characterized in that, comprises the following steps:
Magnesium powder and salt ball milling are obtained to Mg-salt hydrolysis hydrogen manufacturing matrix material.
5. the preparation method of matrix material for Mg-salt hydrolysis hydrogen manufacturing according to claim 4, is characterized in that, described ball milling carries out in ball grinder, at the mid-abrading-ball that is placed with of described ball grinder.
6. the preparation method of matrix material for Mg-salt hydrolysis hydrogen manufacturing according to claim 5, is characterized in that, described ball grinder and abrading-ball are stainless steel.
7. the preparation method of matrix material for Mg-salt hydrolysis hydrogen manufacturing according to claim 4, is characterized in that, the condition of described ball milling is: ratio of grinding media to material is 25:1, and rotating speed is 350-450rpm, and Ball-milling Time is 0.5h-10h.
8. the preparation method of matrix material for Mg-salt hydrolysis hydrogen manufacturing according to claim 1, is characterized in that, is filled with argon gas airtight protection before ball milling in ball grinder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107512701A (en) * | 2016-06-16 | 2017-12-26 | 常君辉 | The multi-electrode activation Catalytic processes of magnesium granules hydrolytic hydrogen production |
| CN107777661A (en) * | 2017-11-21 | 2018-03-09 | 桂林电子科技大学 | A kind of Al LiCl Bi2O3The preparation method and applications of aluminum-based composite hydrogen manufacturing material |
| WO2018148157A1 (en) * | 2017-02-07 | 2018-08-16 | Kuwait Institute For Scientific Research | Method of synthesizing mgh2/ni nanocomposites |
| CN111573621A (en) * | 2020-06-05 | 2020-08-25 | 南京工业大学 | Method for preparing hydrogen by hydrolysis |
| CN112981199A (en) * | 2021-02-06 | 2021-06-18 | 陕西科技大学 | Salt-made porous magnesium-nickel hydrolysis hydrogen production alloy and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491265A (en) * | 2011-12-06 | 2012-06-13 | 南京工业大学 | Method for producing hydrogen by carrying out hydrolysis on magnesium-based material |
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2013
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| CN102491265A (en) * | 2011-12-06 | 2012-06-13 | 南京工业大学 | Method for producing hydrogen by carrying out hydrolysis on magnesium-based material |
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|---|
| MARIE-HELENE GROSJEAN ET AL.: "Hydrolysis of Mg–salt and MgH2–salt mixtures prepared by ball milling for hydrogen production", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 416, 10 October 2005 (2005-10-10), pages 296 - 302 * |
| YONGAN LIU ET AL.: "Hydrogen generation from the hydrolysis of Mg powder ball-milled with AlCl3", 《ENERGY》, vol. 53, 7 March 2013 (2013-03-07), XP028547716, DOI: 10.1016/j.energy.2013.01.073 * |
| 沈品等: "镁基材料水解制氢研究进展", 《电源技术》, vol. 35, no. 7, 31 July 2011 (2011-07-31), pages 876 - 879 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107512701A (en) * | 2016-06-16 | 2017-12-26 | 常君辉 | The multi-electrode activation Catalytic processes of magnesium granules hydrolytic hydrogen production |
| WO2018148157A1 (en) * | 2017-02-07 | 2018-08-16 | Kuwait Institute For Scientific Research | Method of synthesizing mgh2/ni nanocomposites |
| CN107777661A (en) * | 2017-11-21 | 2018-03-09 | 桂林电子科技大学 | A kind of Al LiCl Bi2O3The preparation method and applications of aluminum-based composite hydrogen manufacturing material |
| CN107777661B (en) * | 2017-11-21 | 2020-10-02 | 桂林电子科技大学 | Al-LiCl-Bi2O3Preparation method and application of aluminum-based composite hydrogen production material |
| CN111573621A (en) * | 2020-06-05 | 2020-08-25 | 南京工业大学 | Method for preparing hydrogen by hydrolysis |
| CN112981199A (en) * | 2021-02-06 | 2021-06-18 | 陕西科技大学 | Salt-made porous magnesium-nickel hydrolysis hydrogen production alloy and preparation method thereof |
| CN112981199B (en) * | 2021-02-06 | 2022-05-13 | 陕西科技大学 | Salt porous magnesium-nickel hydrolysis hydrogen production alloy and preparation method thereof |
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Application publication date: 20140514 |