CN102408096A - Aluminum-based composite hydrogen manufacturing material and preparation method thereof - Google Patents
Aluminum-based composite hydrogen manufacturing material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an aluminum-based composite hydrogen manufacturing material and a preparation method thereof and belongs to the technical field of energy sources. The invention provides a novel aluminum-based composite material with high hydrogen manufacturing velocity, and the novel aluminum-based composite material is manufactured by a mechanical ball milling method; and different aluminum-based raw materials and additives are selected in the manufacturing process, and the reaction activity of products and water is improved by optimizing the content of each component and ball milling conditions. The aluminum-based composite hydrogen manufacturing material manufactured by the preparation method provided by the invention can quickly react with the water to release hydrogen at normal temperature, the initial hydrogen manufacturing velocity is larger than 2,000ml/g.min, and the hydrogen yield is close to a theoretical value. The aluminum-based composite hydrogen manufacturing material can be used for solving the problem of low hydrogen manufacturing velocity at the normal temperature reported at present, the hydrogen manufacturing method is simple and fast, and the products are portable and can supply hydrogen to fuel batteries, movable devices and the like.
Description
Technical field
The present invention relates to energy technology field.Be specifically related to a kind of composition and preparation method of aluminium base composite hydrogen manufacturing material of quick product hydrogen.
Background technology
Environmental pollution at present is serious day by day, and people are also increasing to the demands for energy amount, yet the amount of Nonrenewable resources is limited, considers from long-term interest, and the problem that we face is the energy problem that how to solve environmental problem, how to solve future.Show through big quantity research: hydrogen be future the most potential energy it
Utilize Hydrogen Energy, preparation hydrogen is most important.Bibliographical information, the hydrogen 95% that uses in the market derives from chemical hydrogen manufacturing, as: Sweet natural gas, coal gas reformation hydrogen production, what its raw material still used is fossil oil.And the whole world is being faced with the energy dilemma of fossil oil and the environmental pollution that use brought thereof.In the last few years, metal hydrogen manufacturing had caused people's extensive concern.In the hydrogen manufacturing research of the Mg that has reported, Zn and Al, aluminium or aluminum matrix composite are considered to a kind of preferably at present hydrogen manufacturing material, especially for mobile hydrogen making.Because bauxite resource is abundant, low price, to be prone to storage, light weight and hydrogen output high; And water is cooked hydrogen source, aboundresources, cleanliness without any pollution, and hydrogen content is high; The reaction product of its secondary aluminium and water is the oxide compound, oxyhydroxide of aluminium etc., and is nontoxic, is prone to handle reusable edible.
But the aluminium surface is prone to form the fine and close sull of one deck, stops itself and water to react, and for overcoming this fatal problem, the various countries scholar has done a lot of researchs, like people such as Kaname
[1]Studied the method with the water-soluble generation hydrogen of metallic aluminium, elder generation carries out the amalgamation processing with the aluminium sheet of certain size before reaction, makes and encloses the very thin mercury film of one deck on the aluminium, places the water of differing temps to react aluminium sheet then.People such as Kolbenev in 1988
[2]With people such as Kravchenko in 2005
[3]Find to add in the duraluminum activity that some low melting point metals help to improve duraluminum, alloy can with 75-82 ℃ hydrothermal reaction.2009, people such as Parmuzina
[4]Process the 85%Al-Ca-In/Sn/Zn alloy with the mechanical ball milling method, and make the water reaction of itself and differing temps.2010, people such as Mahmoodi
[5]Prepared Al-NaCl-Si/C (graphite)/Bi alloy with the mechanical ball milling method, and made the water reaction of itself and differing temps.
A large amount of work was also being done aspect the development hydrogen manufacturing material in recent years by this study group.Aluminium bismuth, aluminium tin, aluminium indium, aluminium mercury series alloy hydrolytic hydrogen production have been studied.From reporting about the research of aluminium and water reaction hydrogen producing technology at present, through aluminium is transformed, can realize that it produces the hydrogen rate near 100%, but its maximum hydrogen-producing speed is also lower, the maximum hydrogen-producing speed of reporting in the document at present is 936
[6], 1380ml/g.min
[7](all being lower than 1500ml/g.min).For being onboard hydrogen source hydrogen supply gas, improving hydrogen-producing speed is an important indicator.
Summary of the invention
In order to address the above problem, improve the hydrogen-producing speed of aluminium water reaction, the invention provides a kind of aluminium base composite hydrogen manufacturing material of novel quick product hydrogen, its maximum hydrogen-producing speed can reach more than the 2000ml/g.min.
The present invention relates to a kind of preparation method of aluminium base composite hydrogen manufacturing material, its concrete operations step is following:
A. take by weighing raw material;
The composition of said raw material and quality percentage composition are:
Additive 0～10w%
Said additive is a kind of simple substance in metal, basic metal and the transition metal;
B. under argon shield, in ball grinder, in mass ratio 30～60: 1 ratio charging feedstock and steel ball;
C., it is 450r/min that rotational speed of ball-mill is set, and the ball milling time is 1～4h.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, the preferred ball milling time is 3h.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, the mass ratio of preferred steel ball and raw material is 60: 1.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, preferred raw material is aluminium and the tindichloride mixed by 78w%: 22w%.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, preferred raw material is aluminium, tindichloride and the additive mixed by 78w%: 17w%: 5w%.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, preferred additives is following a kind of: magnesium, titanium, bismuth, cadmium, zinc.
In above-mentioned method with the aluminium base composite hydrogen manufacturing material of Prepared by Ball Milling, preferred additives is a bismuth.
The present invention's purpose on the other hand is to go out a kind of aluminium base composite hydrogen manufacturing material through method for preparing, and the aluminium base composite hydrogen manufacturing material of present method preparation is kept in the ar gas environment, can keep its activity.
The present invention has used SnCl in raw material
2, SnCl
2Adding prevented the reunion of each component of composite hydrogen manufacturing material in the preparation process, to realize each component uniform distribution,, thereby increase its specific surface area simultaneously through reducing the size of al particulate, reached the effect that improves aluminium base composite hydrogen manufacturing material hydrolysis rate; Composite hydrogen manufacturing material of the present invention contacts immediate response with water, and start time was less than 5 seconds; Its initial reaction rate is greater than 2000ml/g.min; In the gaseous product of water reaction, except hydrogen and a spot of water vapour, do not contain other foreign gas;
Beneficial effect:
1. the aluminium base composite hydrogen manufacturing material of the present invention's preparation is easy to carry about with one, and hydrogen making and hydrogen supply can be hydrogen supplies such as fuel cell, moving device at any time.
2. the aluminium base composite hydrogen manufacturing material of the present invention's preparation has very high activity, and normal temperature descends and the rapid reaction of water discharges hydrogen, is lower than 5 seconds start time.
3. the invention solves the storage problem of hydrogen, and reduced storage cost.Because aluminium base composite hydrogen manufacturing material is easy to carry, stores, and the storage of water is more convenient;
Below in conjunction with several embodiment, the present invention done further describing.
Description of drawings
The Al-SnCl of Fig. 1 a. different mass ratio
2The product hydrogen rate curve of aluminium base composite hydrogen manufacturing material normal temperature and water reaction
The Al-SnCl of Fig. 1 b. different mass ratio
2The hydrogen-producing speed curve of aluminium base composite hydrogen manufacturing material normal temperature and water reaction
Fig. 1 c.Al-SnCl
2XRD curve before aluminium base composite hydrogen manufacturing material and the water reaction
Fig. 1 d.Al-SnCl
2The reacted XRD curve of aluminium base composite hydrogen manufacturing material and water
The different ball milling time Al-SnCl of Fig. 2 a.
2The product hydrogen rate curve of aluminium base composite hydrogen manufacturing material normal temperature and water reaction
The different ball milling time Al-SnCl of Fig. 2 b.
2The hydrogen-producing speed curve of aluminium base composite hydrogen manufacturing material normal temperature and water reaction
Fig. 3 a.Al-SnCl
2And Al-Sn-AlCl
3The product hydrogen rate curve of milled product normal temperature and water reaction
Fig. 3 b.Al-SnCl
2And Al-Sn-AlCl
3The hydrogen-producing speed curve of milled product normal temperature and water reaction
Fig. 4 Al-SnCl
2The product hydrogen curve of aluminium base composite hydrogen manufacturing material normal temperature of-M and water reaction
The Al-SnCl that the different ball-to-powder weight ratio of Fig. 5 a. make
2The hydrogen output of-Bi composite hydrogen manufacturing material normal temperature and water reaction
The Al-SnCl that the different ball-to-powder weight ratio of Fig. 5 b. make
2The hydrogen-producing speed of-Bi composite hydrogen manufacturing material normal temperature and water reaction
Fig. 5 c.Al-SnCl
2XRD curve before aluminium base composite hydrogen manufacturing material of-Bi and the water reaction
Fig. 5 d.Al-SnCl
2The reacted XRD curve of aluminium base composite hydrogen manufacturing material of-Bi and water
Embodiment
Dress appearance in glove box is under argon shield, in ball grinder, in pack into the raw material of 150g steel ball and 5g of 30: 1 ratio; Rotational speed of ball-mill is made as 450r/min, and the ball milling time is 3h, prepares different composite hydrogen manufacturing materials; Said raw material is: Al and SnCl
2Mix with the ratio of the different mass shown in the table 1.
Table 1.Al-SnCl
2Mix with the different mass ratio
The different composite hydrogen manufacturing material that makes is reacted with water at normal temperatures, promptly take by weighing the composite hydrogen manufacturing material of about 0.1g, add water 10ml, measure it and produce the hydrogen performance, the result sees Fig. 1 a and Fig. 1 b.
Fig. 1 a is the Al-SnCl of different mass ratio
2The product hydrogen rate curve of aluminium base composite hydrogen manufacturing material normal temperature and water reaction, wherein, the volume the when volume of hydrogen all is converted into 273.15K.The result shows: work as SnCl
2Content when being respectively 20wt%, 22wt%, 24wt%, 26wt% and 30wt%, the product hydrogen rate of the composite hydrogen manufacturing material of acquisition is respectively 43.7%, 55.9%, 47.4%, 47.8% and 48.8%.Thus it is clear that, work as SnCl
2The product hydrogen rate of the composite hydrogen manufacturing material that obtains during for 22wt% of content maximum.For this reason, choose SnCl
2The aluminium base composite hydrogen manufacturing material that obtains when being respectively 20wt%, 22wt% and 26wt% carries out the hydrogen-producing speed evaluation, and the result is shown in Fig. 1 b: work as SnCl
2Content when being respectively 20wt%, 22wt% and 26wt% its maximum hydrogen-producing speed be respectively 1306ml/g.min, 1820ml/g.min and 1647ml/g.min.Synthesizing map 1a and Fig. 1 b work as SnCl
2Content when being 22wt%, the product hydrogen performance of the composite hydrogen manufacturing material that obtains is best.
Through material phase analysis appearance Holland PANalytical company X-ray diffractometer (X ' Pert MPD PRO, CuKa, 40kV, 40mA), to Al-SnCl
2Aluminium base composite hydrogen manufacturing material is analyzed with the thing before and after the water reaction mutually, and sweep limit is respectively 5 °～80 ° (Fig. 1 c) and 5 °～90 ° (Fig. 1 d).Scanning result shows Al and SnCl
2Group of products behind the ball milling becomes Al-Sn-AlCl
3, according to scanning result mechanical milling process is analyzed: because SnCl
2Redox characteristic, Sn
2+In mechanical milling process, change Sn into, and produce a spot of AlCl
3
For detecting composite hydrogen manufacturing material product Hydrogen Energy denys that driver fuel is battery operated.Get an amount of aluminium base composite hydrogen manufacturing material and put into ampere bottle, in the ampere bottle, annotates a certain amount of water with syringe, when water with after composite hydrogen manufacturing material contacts, Al and water react generation hydrogen; Simultaneously, a spot of AlCl in the composite hydrogen manufacturing material
3Also with rapidly reaction and generate HCl of water, and the HCl that generates helps the activation of Al in the composite hydrogen manufacturing material again, thereby improves the hydrogen-producing speed of composite hydrogen manufacturing material.Make fuel cell can generate electricity, drive simultaneously small fan work rapidly.
Dress appearance in glove box is under argon shield, in ball grinder, in pack into the raw material of 150g steel ball and 5g of 30: 1 ratio of ball-to-powder weight ratio; Rotational speed of ball-mill is made as 450r/min, and the ball milling time prepares different composite hydrogen manufacturing materials when being respectively 1h, 2h, 3h and 4h; Said raw material is: 78wt%Al and 22wt%SnCl
2Mix.
The different composite hydrogen manufacturing material that makes is reacted with water at normal temperatures, promptly take by weighing the composite hydrogen manufacturing material of about 0.1g, add water 10ml, measure it and produce the hydrogen performance, the result sees Fig. 2 a and Fig. 2 b, the volume the when volume of hydrogen all is converted into 273.15K among the figure.
The result shows shown in Fig. 2 a and Fig. 2 b: when the ball milling time is respectively 1h, 2h, 3h and 4h; The product hydrogen rate of the composite hydrogen manufacturing material that obtains is respectively 29.3%, 39.6%, 55.9% and 45.1%, and its maximum hydrogen-producing speed has reached 1450ml/g.min, 2026ml/g.min, 1820ml/g.min, 1212ml/g.min respectively.Though the hydrogen-producing speed of the composite hydrogen manufacturing material during ball milling 2h is maximum, its product hydrogen rate is very low; Comprehensive hydrogen rate and two indexs of hydrogen-producing speed of producing, the product hydrogen performance of the composite hydrogen manufacturing material when the ball milling time is 3h is best.
Dress appearance in glove box under argon shield, in ball grinder, is pack into the raw material of 150g steel ball and 5g of 30: 1 ratio in ball-to-powder weight ratio; Rotational speed of ball-mill is made as 450r/min, and the ball milling time is 3h, prepares different composite hydrogen manufacturing materials;
Said raw material is: 1) 78wt%Al and 22wt%SnCl
2Mix; Or
2) 78wt%Al, 14wt%Sn and 8wt%AlCl
3Mix.
The different composite hydrogen manufacturing material that makes is reacted with water at normal temperatures, promptly take by weighing the composite hydrogen manufacturing material of about 0.1g, add water 10ml, measure it and produce the hydrogen performance, the result sees Fig. 3 a and Fig. 3 b.Volume when the volume of hydrogen all is converted into 273.15K among the figure.
Shown in Fig. 3 a and Fig. 3 b: Al, Sn and AlCl
3Under the same terms the composite hydrogen manufacturing material of ball milling gained its produce hydrogen rate and hydrogen-producing speed and be merely 20.5% and 652.8ml/g.min.Show Al and SnCl
2Composite hydrogen manufacturing material behind the ball milling produces the hydrogen performance and is superior to Al, Sn and AlCl
3Composite hydrogen manufacturing material behind the ball milling produces the hydrogen performance.Its reason belongs to: SnCl
2Redox characteristic, generated in-situ Sn distributes more evenly in Al in mechanical milling process, and is therefore more remarkable to the activation of Al.
Dress appearance in glove box is under argon shield, in ball grinder, in pack into the raw material of 150g steel ball and 5g of 30: 1 ratio; Rotational speed of ball-mill is made as 450r/min, and the ball milling time is 3h, prepares different composite hydrogen manufacturing materials;
Said raw material is: 78wt%Al and 17wt%SnCl
2Mix with 5wt% additive M, wherein additive M is following a kind of Mg, Ti, Zn, Bi and Cr.
The different composite hydrogen manufacturing material that makes is reacted with water at normal temperatures, promptly take by weighing the composite hydrogen manufacturing material of about 0.1g, add water 10ml, measure it and produce the hydrogen performance, the result is as shown in Figure 4.Volume when the volume of hydrogen all is converted into 273.15K among the figure.
As shown in Figure 4: as partly to substitute SnCl with Mg, Ti, Zn, Bi and Cr
2The prepared composite hydrogen manufacturing material in back, it produces the hydrogen rate and is respectively 22.2%, 21.5%, 34.9%, 100% and 26.3%.It is thus clear that the adding of metal Bi has obviously improved Al-SnCl
2The product hydrogen rate of composite hydrogen manufacturing material.Its reason belongs to: Bi can improve the electrochemical activity of aluminium base composite hydrogen manufacturing material, produces the hydrogen rate thereby improve it.
Embodiment 5
Dress appearance in glove box is under argon shield, in ball grinder, in pack into the raw material of 150g steel ball and 2.5g of 60: 1 ratio; In another ball grinder, in pack into the raw material of 150g steel ball and 5g of 30: 1 ratio; Rotational speed of ball-mill is 450r/min, and the ball milling time is 3h, prepares different composite hydrogen manufacturing materials; Said raw material is: 78wt%Al and 17wt%SnCl
2Mix with 5wt%Bi.
The different composite hydrogen manufacturing material that makes is reacted with water at normal temperatures, promptly take by weighing the composite hydrogen manufacturing material of about 0.1g, add water 10ml, measure its hydrogen output, the result is shown in Fig. 5 a.Volume when the volume of hydrogen all is converted into 273.15K among the figure.
Shown in Fig. 5 a, when ball-to-powder weight ratio was brought up to 60: 1 by 30: 1, hydrogen output and no change; But hydrogen-producing speed changes obviously; Shown in Fig. 5 b, ball-to-powder weight ratio is that 30: 1 o'clock hydrogen outputs are 1491.4ml/g.min, is 2138.6ml/g.min and ball-to-powder weight ratio is 60: 1 o'clock hydrogen outputs.It is thus clear that different ball-to-powder weight ratio do not have influence to the hydrogen output of aluminium base composite hydrogen manufacturing material; Only influence its hydrogen-producing speed.
Through material phase analysis appearance Holland PANalytical company X-ray diffractometer (X ' Pert MPD PRO, CuKa, 40kV, 40mA), to Al-SnCl
2The aluminium base composite hydrogen manufacturing material of-Bi is analyzed with the thing before and after the water reaction mutually, and sweep limit is respectively 5 °～80 ° (seeing Fig. 5 c), 5 °～90 ° (seeing Fig. 5 d).
Fig. 5 c is that Bi partly substitutes SnCl
2The X-ray diffraction spectrogram of the mixture that obtains behind the ball milling with Fig. 1 c ratio, except that aluminium and Sn crystalline diffraction peak, is also observed Bi crystalline diffraction peak.This does not change after showing metal Bi ball milling, and the product behind its ball milling consists of Al-Sn-Bi-AlCl
3Fig. 5 d is the reacted X-ray diffraction spectrogram of this mixture and water, and main peak is AlO (OH) and Al (OH)
3, and the peak of metal Sn and Bi still appears in the curve.Clearly, the reaction of metallic aluminium and water has produced AlO (OH) and Al (OH)
3, and metal Sn and Bi bismuth be only as cathode material and have neither part nor lot in reaction, only plays and accelerate the effect that Al and water react.
Reference
[1]Kaname，S.；Yoshiyuki，N.；Kazuo.Technology?Reports?of?the?Osaka?University?1989，38，179.
[2]Kolbenev，I.L.；Volybtsev，N.F.；Sarmurzina，R.G.；Dikov，V.V.Probl?Mashinostr(Probl.Eng)(Kiev)1988，29，96.
[3]Kravchenko，O.V.；Semenenko，K.N.；Bulychev，B.M.；Kalmykov，K.B.J?Alloy?Compd?2005，397，58.
[4]Parmuzina，A.V.；Kravchenko，O.V.；Bulychev，B.M.；Shkol′nikov，E.I.；Burlakova，A.G.Russ?Chem?B+2009，58，493.
[5]Mahmoodi，K.；Alinejad，B.Int?J?Hydrogen?Energ?2010，35，5227.
[6]Soler，L.；Macanas，J.；Munoz，M.；Casado，J.Int?J?Hydrogen?Energ?2007，32，4702.
[7]Ilyukhina，A.V.；Kravchenko，O.V.；Bulychev，B.M.；Shkolnikov，E.I.Int?J?Hydrogen?Energ?2010，35，1905.
Claims (8)
1. the preparation method of an aluminium base composite hydrogen manufacturing material is characterized in that the concrete operations step is following:
A. take by weighing raw material;
The composition of said raw material and quality percentage composition are:
Aluminium 60～95w%
Tindichloride 1～40w%
Additive 0～10w%
Said additive is a kind of simple substance in metal, basic metal and the transition metal;
B. under argon shield, in ball grinder, in mass ratio 30～60: 1 ratio charging feedstock and steel ball;
C., it is 450r/min that rotational speed of ball-mill is set, and the ball milling time is 1～4h.
2. aluminium base composite hydrogen manufacturing material according to claim 1 is characterized in that: the described ball milling time is 3h.
3. aluminium base composite hydrogen manufacturing material according to claim 1 is characterized in that: the mass ratio of described steel ball and raw material is 60: 1.
4. according to each described aluminium base composite hydrogen manufacturing material in the claim 1～3, it is characterized in that: described raw material is aluminium and the tindichloride mixed by 78w%: 22w%.
5. according to each described aluminium base composite hydrogen manufacturing material in the claim 1～3, it is characterized in that: described raw material is aluminium, tindichloride and the additive mixed by 78w%: 17w%: 5w%.
6. aluminium base composite hydrogen manufacturing material according to claim 5 is characterized in that: described additive is following a kind of: magnesium, titanium, bismuth, cadmium, zinc.
7. aluminium base composite hydrogen manufacturing material according to claim 6 is characterized in that: described additive is a bismuth.
8. the aluminium base composite hydrogen manufacturing material for preparing according to claim 1,2,3, each the method described in 7.
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| CN107188123A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of preparation method of silicon/alkali metal hydrogen manufacturing material |
| CN109133000A (en) * | 2018-08-23 | 2019-01-04 | 杭州氢源素生物科技有限公司 | A kind of micro-nano composite hydrolysis hydrogen manufacturing material of aluminium base |
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| CN103420336B (en) * | 2012-05-22 | 2015-12-16 | 中国科学院大连化学物理研究所 | A kind of Al-NaBiO 3hydrolytic hydrogen production matrix material and preparation thereof |
| CN105036075A (en) * | 2015-06-25 | 2015-11-11 | 桂林电子科技大学 | Al-BiBr3 aluminum base composite hydrogen production material and preparation method thereof |
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