CN111705241A - Al alloy for preparing hydrogen and preparation method and application thereof - Google Patents

Al alloy for preparing hydrogen and preparation method and application thereof Download PDF

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CN111705241A
CN111705241A CN202010631858.3A CN202010631858A CN111705241A CN 111705241 A CN111705241 A CN 111705241A CN 202010631858 A CN202010631858 A CN 202010631858A CN 111705241 A CN111705241 A CN 111705241A
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alloy
hydrogen
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张建斌
石玗
容煜
陆雨
焦凯
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Lanzhou University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses an Al alloy for preparing hydrogen and a preparation method and application thereof, and relates to the technical field of hydrogen production of Al alloys, wherein the Al alloy comprises metal Al, Mg, Ga and Sn; wherein the content of Sn is 0.6-1.2wt.%, the content of Mg is 0.41-1.7wt.%, the content of Ga is 0.2-2wt.%, and the balance is Al; in addition, 0.2-1.0wt.% of Cu can be added into the Al alloy to improve the hydrogen production performance of the aluminum alloy. The aluminum alloy of the invention not only reduces the production cost of the aluminum alloy for hydrogen production, but also improves the hydrogen production performance, and the hydrogen production capacity of the aluminum alloy at 30 ℃, 50 ℃, 70 ℃ and 90 ℃ is 927.4 mL/g, 1040.0mL/g, 1143.5mL/g and 1247.0 mL/g respectively.

Description

Al alloy for preparing hydrogen and preparation method and application thereof
Technical Field
The invention relates to the technical field of hydrogen production by using Al alloy, in particular to Al alloy for preparing hydrogen and a preparation method and application thereof.
Background
Fuel Cells (FC) are driven by pure, clean hydrogen gas, rather than being obtained by fossil fuel reformulation, and thus do not contaminate the surrounding environment. Although FC is used in the field of new energy electric vehicles on a small scale nowadays, FC has some engineering technical difficulties and lacks a reliable and efficient hydrogen supply system, so that FC cannot be popularized on a large scale. In the aspect of hydrogen production, at present, hydrogen production by fossil fuel, hydrogen production by biomass gasification, hydrogen production by water electrolysis, hydrogen production by photocatalysis, non-mineral energetic materials and the like are mainly used.
The traditional hydrogen production technology has the problems of cost, transportation, storage and the like. In practical application, the hydrogen production from fossil resources is most widely applied, however, the fossil resources are non-renewable resources, and the purity of hydrogen in the product is not high; the hydrogen production by water electrolysis needs continuous electric energy, and the energy conversion rate is low, and the safety is not high enough; although biomass hydrogen production is cleaner and easy to transport, the biomass hydrogen production has the natural defect of high energy consumption, the process flow is also more complex, the reaction is difficult to control, and a large amount of byproducts exist. Although the above hydrogen production technology is suitable for large-scale production, the demand of fuel cells for high-purity and safe hydrogen sources cannot be met.
With the continuous and intensive research, researchers find that metals and their compounds can generate a large amount of high-purity hydrogen under certain conditions, and that the metals do not have the problems of transportation safety (such as explosion, leakage, evaporation) and the like. At present, the metal hydrogen production mainly adopts Al-based alloy to produce hydrogen, because Al is the most abundant metal element in the earth crust, exists in the form of ore in nature, is easy to prepare and has price advantage, and has no harsh storage condition; but because the compact oxide film exists on the surface of the Al, the further reaction of the Al and water is hindered, in order to solve the problem, one method is to destroy the compact oxide film on the surface of the Al by traditional mechanical means such as grinding, ball milling and the like, and simultaneously change the specific surface area of the Al and the aluminum alloy to make the Al and the aluminum alloy powder, thereby improving the contact area of the reaction; however, the ball milling cost is high, and the specific surface area and the surface energy of the aluminum powder are high, so that the chemical property is active, and safety accidents are easy to happen, so that the storage (easy oxidation) and transportation of the Al powder limit the application of the aluminum powder in hydrogen production; the other method is to add Ga, Sn, In and other metals into aluminum to form low-melting-point activated aluminum alloy so as to reduce the activation energy of the reaction; and part of low-melting point metal destroys Al grain boundaries to improve the hydrogen production performance of Al, but Ga, Sn and In all belong to rare and precious metals, so that the hydrogen production cost is greatly increased.
Disclosure of Invention
In order to solve the problems, the invention provides an Al alloy for preparing hydrogen and a preparation method and application thereof, and the method improves the hydrogen production amount and the hydrogen production rate of the Al alloy by adding a small amount of Ga, Sn, Mg, Cu and other elements into Al, and has the advantages of small addition amount and low cost.
In order to achieve the purpose, one of the technical schemes adopted by the invention is as follows: an Al alloy for producing hydrogen, the Al alloy comprising the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 0.6-1.2wt.%, the content of Mg is 0.41-1.7wt.%, the content of Ga is 0.2-2wt.%, and the balance is Al.
Further, the Al alloy includes metals Al, Mg, Ga, and Sn;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, and the balance is Al.
The second technical scheme adopted by the invention is as follows: an Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 0.6-1.2wt.%, the content of Mg is 0.41-1.7wt.%, the content of Ga is 0.2-2wt.%, the content of Cu is 0.2-1.0wt.%, and the balance is Al.
Further, the Al alloy is composed of metals Al, Mg, Ga, Sn, and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.8wt.%, and the balance is Al.
The third technical scheme adopted by the invention is as follows: the preparation method of the Al alloy in any one of the above technical schemes comprises the following steps:
s1: weighing metal raw materials according to the component ratio;
s2: putting the weighed Al into a graphite crucible and transferring the graphite crucible into a box-type resistance furnace, wherein the temperature of the resistance furnace is 720-780 ℃, keeping the temperature for 5-6min after the Al is completely melted into a liquid state, taking out and adding other metal raw materials, and stirring the mixture to uniformly mix the metal raw materials after all the metal is completely dissolved. Then putting the mixture into a resistance furnace, heating the mixture to 630-680 ℃, adding 0.2-0.8wt.% of refining agent hexachloroethane to refine the mixture, and continuously stirring the mixture in the refining process to remove slag;
s3: pouring the alloy solution in the S2 into a mould after slagging-off is finished;
s4: after cooling, the samples were removed from the molds and numbered.
The fourth technical scheme adopted by the invention is as follows: the application of the Al alloy in the fuel cell according to any of the above technical solutions, wherein hydrogen is prepared by hydrolysis reaction of the Al alloy as a hydrogen source of the fuel cell.
The invention has the beneficial effects that:
according to the invention, low-melting-point metals Ga, Sn and Mg are added into aluminum to form the low-melting-point activated aluminum alloy, low-cost Mg is used for replacing high-price In, the using amounts of Sn and Ga are reduced, although the hydrogen production amount is slightly reduced, the production cost of the Al alloy is greatly reduced, and after a large number of experimental researches are carried out on the optimization of Al alloy components, the content of Sn In the Al alloy is 1.2wt.%, the content of Mg is 1.7wt.%, and the content of Ga is 1.5wt.%, the hydrogen production amount can reach 833.7mL/g at 30 ℃, and can reach 1102.1mL/g at 90 ℃.
In order to further reduce the production cost of the hydrogen-producing aluminum alloy and improve the hydrogen-producing performance of the aluminum alloy, the aluminum alloy is further added with Cu, so that the aluminum alloy reaches 99.3 percent at 90 ℃. Further, the hydrogen production amounts at 30 ℃, 50 ℃, 70 ℃ and 90 ℃ were 927.4 mL/g, 1040.0mL/g, 1143.5mL/g and 1247.0 mL/g, respectively.
In addition, the aluminum alloy block is prepared by smelting and casting, so that the safe transportation of the aluminum alloy is facilitated.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a graph showing the amount of hydrogen produced at 30 ℃ for Al alloys of examples 1 to 5 of the present invention;
FIG. 2 is a graph showing the amount of hydrogen produced at 90 ℃ for the Al alloys of examples 1 to 5 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the Al alloy of examples 6 to 10 of the present invention;
FIG. 4 is a back-scattered scanning electron microscopy (BSEM) image of an Al alloy of examples 6-10 of the present invention;
FIG. 5 is a graph showing the amount of hydrogen produced at 30 ℃ for the Al alloys of examples 6 to 10 of the present invention;
FIG. 6 is a graph showing the amount of hydrogen produced at 90 ℃ for the Al alloys of examples 6 to 10 of the present invention;
FIG. 7 is a graph showing the hydrogen production conversion ratios of Al alloys of examples 6 to 10 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 1.2wt.%, the content of Mg is 0.41wt.%, the content of Ga is 2wt.%, and the balance is Al.
Example 2
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 0.8wt.%, the content of Mg is 1.0wt.%, the content of Ga is 1.0wt.%, and the balance is Al.
Example 3
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 1.0wt.%, the content of Mg is 0.7wt.%, the content of Ga is 0.5wt.%, and the balance is Al.
Example 4
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 0.6wt.%, the content of Mg is 1.7wt.%, the content of Ga is 0.2wt.%, and the balance is Al.
Example 5
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, and the balance is Al.
Example 6
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.2wt.%, and the balance is Al.
Example 7
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.4wt.%, and the balance is Al.
Example 8
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.6wt.%, and the balance is Al.
Example 9
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.8wt.%, and the balance is Al.
Example 10
An Al alloy for the production of hydrogen, consisting of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 1.0wt.%, and the balance is Al.
Example 11
A method of making an Al alloy for use in making hydrogen as described in examples 1-10, said method comprising the steps of:
s1: weighing metal raw materials according to the component ratio;
s2: putting the weighed Al into a graphite crucible and transferring the graphite crucible into a box-type resistance furnace, wherein the temperature of the resistance furnace is 720-780 ℃, keeping the temperature for 5-6min after the Al is completely melted into a liquid state, taking out the Al and sequentially adding other metal raw materials, and stirring the Al and the other metal raw materials to uniformly mix the Al and the liquid raw materials after all the metals are completely dissolved. Then putting the mixture into a resistance furnace, heating the mixture to 630-680 ℃, adding a refining agent hexachloroethane (0.2-0.8 wt.%) for refining, continuously stirring the mixture in the refining process, and slagging off the mixture;
s3: pouring the alloy solution in the S2 into a mould after slagging-off is finished;
s4: after cooling, the samples were removed from the molds and numbered.
Experimental example 1
The hydrogen production of the Al alloys of examples 1-5 at different temperatures in simulated seawater (3.5 wt.% NaCl) is shown in Table 1 and FIGS. 1-2.
Table 1 hydrogen production by Al alloys of examples 1-5 at different temperatures in simulated seawater
Figure 987805DEST_PATH_IMAGE002
Fig. 1 and 2 are graphs showing the hydrogen production of the Al alloy samples of examples 1 to 5 at 30 ℃ and 90 ℃ In simulated seawater (3.5 wt.% NaCl), respectively, which are represented by the time-dependent change of the low-cost Mg for higher-cost In, and the amounts of Sn and Ga are reduced, and although the hydrogen production is slightly reduced, the production cost of the Al alloy is greatly reduced, and after the optimization of the Al alloy composition, when the content of Sn In the Al alloy is 1.2wt.%, the content of Mg In the Al alloy is 1.7wt.%, the content of Ga In the Al alloy is 1.5wt.%, and the balance is Al, the hydrogen production can reach 833.7mL/g at 30 ℃ and 1102.1mL/g at 90 ℃.
Experimental example 2
1. XRD analysis of the Al alloys of examples 6 to 10
FIG. 3 is an XRD pattern of the Al alloys of examples 6-10. As can be seen from the graph, the alloy samples containing different amounts of Cu elements all contained Alss (aluminum solid solution) and Mg2Sn and Ga5Mg2Phase (1); as the Cu element increases from 0.2wt.% to 1wt.%, no alloy phase of the Cu element is observed because the Cu content is low.
2. BSEM analysis of Al alloys of examples 6-10
After the Cu element is added, the alloy still can react with water, so that metallographic sample preparation is difficult, and therefore, a sample is analyzed by backscattering scanning. Fig. 4 is a back-scattered scanning electron microscope (BSEM) image of an as-cast Al alloy containing trace amounts of Cu elements, wherein the Cu content in graphs a, b, c, d, e is 0.2wt.%, 0.4wt.%, 0.6wt.%, 0.8wt.% and 1.0wt.%, respectively; the alloy is composed of an Al matrix, dendrites and a fishbone-shaped eutectic structure.
3. Influence of Cu content on Hydrogen Generation Performance
FIGS. 5-6 are graphs showing the hydrogen production of the Al alloys of examples 6-10 in simulated seawater (3.5 wt.% NaCl) at 30 ℃ and 90 ℃. As can be seen from the figure, when the Cu element is added, the hydrogen production amount increases first and then decreases, and reaches the maximum when the Cu content is 0.8wt.%, the hydrogen production effect is the best at this time; after 0.8wt.% Cu was added, the hydrogen production was increased by 93.7 mL/g and 145 mL/g at 30 ℃ and 90 ℃ respectively, as compared with the Al alloy of example 5. The hydrogen production conversion rate is shown in figure 7, and reaches 99.3% at 90 ℃. Among them, the Al alloy of example 9 was most suitable in terms of hydrogen production, and the hydrogen production amounts at 30 ℃, 50 ℃, 70 ℃ and 90 ℃ were 927.4 mL/g, 1040.0mL/g, 1143.5mL/g and 1247.0 mL/g, respectively.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. An Al alloy for the production of hydrogen, characterized in that the Al alloy comprises the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 0.6-1.2wt.%, the content of Mg is 0.41-1.7wt.%, the content of Ga is 0.2-2wt.%, and the balance is Al.
2. Al alloy for the production of hydrogen according to claim 1, characterized in that it comprises the metals Al, Mg, Ga and Sn;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, and the balance is Al.
3. An Al alloy for the production of hydrogen, characterized in that it consists of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 0.6-1.2wt.%, the content of Mg is 0.41-1.7wt.%, the content of Ga is 0.2-2wt.%, the content of Cu is 0.2-1.0wt.%, and the balance is Al.
4. Al alloy for the production of hydrogen according to claim 3, characterized in that it consists of the metals Al, Mg, Ga, Sn and Cu;
wherein the content of Sn is 1.2wt.%, the content of Mg is 1.7wt.%, the content of Ga is 1.5wt.%, the content of Cu is 0.8wt.%, and the balance is Al.
5. A method of producing the Al alloy according to any one of claims 1 to 4, characterized in that the method comprises the steps of:
s1: weighing metal raw materials according to the component ratio;
s2: putting the weighed Al into a graphite crucible and transferring the graphite crucible into a box-type resistance furnace, keeping the temperature of the resistance furnace at 720-780 ℃, keeping the temperature for 5-6min after the Al is completely melted into a liquid state, taking out and adding other metal raw materials, stirring the mixture after all the metals are completely dissolved to uniformly mix the metals, then putting the mixture into the resistance furnace, heating the mixture to 630-680 ℃, adding 0.2-0.8wt.% of refining agent hexachloroethane for refining, continuously stirring the mixture in the refining process, and removing slag;
s3: pouring the alloy solution in the S2 into a mould after slagging-off is finished;
s4: after cooling, the samples were removed from the molds and numbered.
6. The use of the Al alloy according to any one of claims 1 to 4 in a fuel cell, wherein a hydrogen gas is produced by hydrolysis of the Al alloy as a hydrogen source for the fuel cell.
CN202010631858.3A 2020-07-03 2020-07-03 Al alloy for preparing hydrogen and preparation method and application thereof Pending CN111705241A (en)

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Publication number Priority date Publication date Assignee Title
CN115652148A (en) * 2022-10-12 2023-01-31 山东海化集团有限公司 Aluminum alloy containing accordion-pleated nanosheet layer precipitated phase and used for hydrogen production through hydrolysis, and preparation method and application thereof
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CN116179898A (en) * 2023-01-16 2023-05-30 中南大学 Hydrogen-producing aluminum alloy material capable of being rapidly reacted with water and preparation method thereof

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