CN110980637A - Aluminum-based composite material and preparation method and application thereof - Google Patents
Aluminum-based composite material and preparation method and application thereof Download PDFInfo
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- CN110980637A CN110980637A CN201911282872.0A CN201911282872A CN110980637A CN 110980637 A CN110980637 A CN 110980637A CN 201911282872 A CN201911282872 A CN 201911282872A CN 110980637 A CN110980637 A CN 110980637A
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- 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
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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
- 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 relates to the field of new energy materials, and provides an aluminum-based composite material, and a preparation method and application thereof, wherein the preparation method comprises the following steps: and mixing aluminum, hydroxide and chloride, and performing ball milling in a protective atmosphere to obtain the aluminum-based composite material. The aluminum-based composite material provided by the invention takes hydroxide and chloride as additives, can destroy an oxide film on the surface of aluminum, provides an alkaline environment for promoting aluminum corrosion, forms a primary battery for promoting aluminum corrosion, and further promotes the aluminum corrosion by chloride ions in the chloride, thereby effectively improving the hydrogen production performance by hydrolysis of the aluminum-based composite material. The results of the examples show that the hydrogen yield of the aluminum matrix composite material provided by the invention can reach 935mL/g after reacting with water (30 ℃) for 600s under normal pressure.
Description
Technical Field
The invention relates to the field of new energy materials, in particular to an aluminum-based composite material and a preparation method and application thereof.
Background
Energy is the material basis on which human beings live and develop, but human beings use fossil energy such as oil, coal and natural gas in a large amount and cause more and more serious environmental pollution, and clean energy has aroused people's attention, becomes the research focus of development and utilization all over the world. Hydrogen is popular as a fuel with high heat value, no pollution and abundant resources, and is regarded as the most ideal energy source in the 21 st century.
The industrialization of hydrogen energy is mainly limited by hydrogen production technology and storage technology, so that the hydrogen energy is difficult to popularize and apply. In the aspect of hydrogen production, industrial hydrogen mainly adopts fossil fuel or electrolyzed water to produce hydrogen, wherein the fossil fuel is non-renewable and can not be used for a long time, and the produced hydrogen is impure and can cause pollution to the environment; the hydrogen with high purity can be obtained by electrolyzing water to prepare hydrogen, but the electric energy consumed in the hydrogen preparation process is larger. In the aspect of hydrogen storage, traditional high-pressure gaseous hydrogen storage and high-pressure liquid hydrogen storage have low hydrogen storage efficiency, and the establishment of a solid hydrogen storage material and a hydrogen station is the direction for solving the problem of hydrogen storage in the future, but at present, the solid hydrogen storage material is still in the research and development stage, the construction cost of the hydrogen station is extremely high, and the solid hydrogen storage material is still in the initial stage of construction.
Aluminum reacts with water to produce hydrogen, which can be used to produce hydrogen. However, in the air, a dense oxide film is formed on the surface of aluminum, and the oxide film can prevent the aluminum inside from further reacting, so how to remove the dense oxide film on the surface of aluminum or prevent the dense oxide film from being formed on the surface of aluminum in recent years to realize continuous and rapid hydrogen production by hydrolysis at normal temperature is a key point of extensive research at home and abroad. In the prior art, aluminum alloy/borohydride is used for hydrolysis hydrogen production, for example, patent CN102910582A provides a miniature hydrogen production system and a hydrogen production method based on aluminum alloy/borohydride hydrolysis reaction, but sodium borohydride is required to be used in the preparation process, and has great toxicity and potential safety hazard in use.
Disclosure of Invention
The aluminum-based composite material provided by the invention is in violent reaction after being contacted with water, can generate hydrogen and has high hydrogen production.
The invention provides a preparation method of an aluminum matrix composite, which comprises the following steps:
and mixing aluminum, hydroxide and chloride, and performing ball milling in a protective atmosphere to obtain the aluminum-based composite material.
Preferably, the aluminum, the hydroxide and the chloride are respectively in parts by mass as follows:
60-95 parts of aluminum;
5-25 parts of hydroxide;
0-15 parts of chloride.
Preferably, the aluminum is metallic aluminum powder, and the particle size of the metallic aluminum powder is 100-200 meshes.
Preferably, the hydroxide comprises one or more of bismuth hydroxide, aluminum hydroxide and calcium hydroxide.
Preferably, the chloride comprises one or more of magnesium chloride, stannous chloride, aluminum chloride, sodium chloride and bismuth chloride.
Preferably, the aluminum, the hydroxide and the chloride are respectively in parts by mass as follows:
60-95 parts of aluminum;
5-25 parts of hydroxide;
1-15 parts of chloride;
the hydroxide is a mixture of aluminum hydroxide, bismuth hydroxide and calcium hydroxide;
the chloride is a mixture of sodium chloride, aluminum chloride and stannous chloride.
Preferably, the ball-milling ball-material ratio is 10-30: 1, the ball-milling time is 3-20 h, and the ball-milling rotating speed is 300-550 r/min.
Preferably, the ball milling tank and the milling ball are made of corundum.
The invention also provides the aluminum matrix composite material prepared by the method of the technical scheme.
The invention also provides an application of the aluminum matrix composite material in the technical scheme in preparation of hydrogen, which comprises the following steps: mixing the aluminum matrix composite material with water for reaction, and collecting hydrogen; the temperature of the mixing reaction is 0-100 ℃.
The invention provides a preparation method of an aluminum matrix composite, which comprises the following steps: and mixing aluminum, hydroxide and chloride, and performing ball milling in a protective atmosphere to obtain the aluminum-based composite material. In the invention, the hydroxide and the chloride can destroy an oxide film on the surface of the aluminum in the ball milling process, so as to prevent the agglomeration of the aluminum powder; the hydroxide can provide an alkaline environment for promoting aluminum corrosion in the hydrolysis process, and part of the hydroxide (such as bismuth hydroxide) can react with aluminum in the ball milling process to generate metal simple substances in situ, and the metal simple substances can form a miniature primary battery with aluminum (cathode) in the hydrolysis process, so that the hydrolysis hydrogen production performance of the aluminum-based composite material is improved; the chloride can provide chloride ions for promoting aluminum corrosion in the hydrolysis process, so that the prepared aluminum-based composite material has high activity when reacting with water to prepare hydrogen. And partial chloride, such as stannous chloride, can generate a metal simple substance Sn in situ in the ball milling process, and the metal simple substance and aluminum form a miniature primary battery in the hydrolysis process, wherein the aluminum (cathode) is corroded, which is beneficial to improving the hydrolysis hydrogen production performance of the aluminum-based composite material. The aluminum-based composite material provided by the invention takes hydroxide and chloride as additives, and compared with noble metals such as gallium, indium and the like, the aluminum-based composite material is very low in price and easy to obtain raw materials; compared with high-toxicity raw materials such as sodium borohydride and the like, the raw materials of the invention are safer to use. In addition, the aluminum-based composite material provided by the invention has simple hydrogen production conditions and higher hydrogen production. The results of the examples show that the hydrogen yield of the aluminum matrix composite material provided by the invention can reach 935mL/g after reacting with water (30 ℃) for 600s under normal pressure.
Drawings
FIG. 1 is an SEM picture of the aluminum powder of example 3;
FIG. 2 is an SEM image of an aluminum matrix composite material of example 3;
FIG. 3 is a graph showing the change of hydrogen production with time of the aluminum matrix composite materials of examples 1 to 3.
Detailed Description
The invention provides a preparation method of an aluminum matrix composite, which comprises the following steps:
and mixing aluminum, hydroxide and chloride, and performing ball milling in a protective atmosphere to obtain the aluminum-based composite material.
In the present invention, the mass parts of the aluminum, the hydroxide and the chloride are preferably:
60-95 parts of aluminum;
5-25 parts of hydroxide;
0-15 parts of chloride.
In the present invention, the aluminum is preferably 60 to 95 parts by mass, more preferably 65 to 85 parts by mass, and most preferably 70 to 80 parts by mass. In the invention, the aluminum is preferably aluminum powder, the purity of the aluminum powder is preferably equal to or more than 99%, and the particle size of the aluminum powder is preferably 100-200 meshes, and more preferably 120-180 meshes. In the invention, the particle size of the aluminum metal powder is preferably controlled within the range, so that the aluminum can fully react with hydroxide and chloride, and the hydrogen production activity of the aluminum matrix composite material is improved.
In the present invention, the mass fraction of the hydroxide is preferably 5 to 25 parts, more preferably 10 to 20 parts, and even more preferably 12 to 18 parts, based on the mass fraction of aluminum. In the present invention, the hydroxide is preferably a metal hydroxide, and the hydroxide preferably includes one or more of bismuth hydroxide, aluminum hydroxide, and calcium hydroxide. When the hydroxide preferably comprises a plurality of substances, the proportion relation among the plurality of substances is not particularly required, and in the specific implementation, the following preferable scheme is adopted: when the hydroxide preferably comprises bismuth hydroxide, aluminum hydroxide and calcium hydroxide, the mass ratio of the bismuth hydroxide to the aluminum hydroxide to the calcium hydroxide is preferably 50-70: 20-30: 10-20 or 50-80: 10-30: 10-20; when the hydroxide preferably comprises bismuth hydroxide and aluminum hydroxide, the mass ratio of the bismuth hydroxide to the aluminum hydroxide is preferably 50-80: 20-50. The present invention preferably employs a combination of the above hydroxides to sufficiently exert their respective activating effects, thereby allowing aluminum to be efficiently activated. In the present invention, the hydroxide is preferably analytically pure or more.
In the present invention, the mass part of the chloride is preferably 0 to 15 parts, more preferably > 0 and not more than 15 parts, even more preferably 1 to 15 parts, and most preferably 5 to 12 parts, based on the mass part of aluminum. In the present invention, the chloride is preferably a metal chloride, and the chloride preferably includes one or more of magnesium chloride, stannous chloride, aluminum chloride, sodium chloride, and bismuth chloride. When the chloride preferably comprises a plurality of substances, the proportion relation among the plurality of substances is not particularly required, and when the chloride is specifically implemented, the following preferred scheme is adopted: when the chloride preferably comprises bismuth chloride, sodium chloride and stannous chloride, the mass ratio of the bismuth chloride to the sodium chloride to the stannous chloride is preferably 30-60: 30-50: 10-20; when the chloride preferably comprises sodium chloride, aluminum chloride and stannous chloride, the mass ratio of the sodium chloride to the aluminum chloride to the stannous chloride is preferably 40-70: 10-20: 20-40. The present invention preferably employs a combination of the above two chlorides, due to the fact that the combination is effective in breaking the oxide film of aluminum during ball milling. In the present invention, the chloride is preferably analytically pure or more pure.
In the invention, hydroxide and chloride can prevent the agglomeration of aluminum powder in the ball milling process and damage the oxide film of the aluminum powder; the added chloride can provide chloride ions which promote aluminum corrosion during hydrolysis; the addition of hydroxides and chlorides (such as calcium hydroxide and aluminum chloride) can provide an alkaline environment during hydrolysis that promotes aluminum corrosion; the addition of hydroxides and chlorides (such as stannous chloride, bismuth hydroxide) can generate elemental metals in situ during the ball milling process, and these elemental metals form a miniature galvanic cell with aluminum during the hydrolysis process, wherein the aluminum (negative electrode) is corroded.
The aluminum, hydroxide and chloride are mixed and then ball-milled in a protective atmosphere to obtain the aluminum-based composite material. In the present invention, the protective atmosphere is preferably a nitrogen atmosphere or an inert gas atmosphere. The ball milling is carried out under the protective atmosphere, so that the aluminum powder is prevented from being oxidized in the ball milling process. In the invention, the ball-to-material ratio of the ball milling is preferably 10-30: 1, and more preferably 15-25: 1; the ball milling time is preferably 3-20 h, and more preferably 5-15 h; the rotation speed of the ball milling is preferably 300-550 r/min, and more preferably 350-500 r/min. In the present invention, the material of the ball milling pot and the material of the grinding ball are preferably corundum.
The invention also provides the aluminum matrix composite material prepared by the method of the technical scheme. The aluminum-based composite material provided by the invention needs to be stored in vacuum, nitrogen or inert gas, so that the long-time contact with air is avoided, and the activity in the air is gradually reduced.
The invention also provides an application of the aluminum matrix composite material in the technical scheme in preparation of hydrogen, which comprises the following steps: mixing the aluminum matrix composite material with water for reaction, and collecting hydrogen. In the invention, after the aluminum matrix composite material is contacted with water, a violent reaction immediately occurs, and hydrogen is released. In the present invention, the water is preferably in excess to ensure the completion of the reaction of the aluminum matrix composite. The aluminum-based composite material provided by the invention reacts immediately after contacting with water, does not need pressurization, can be used under 90-120 kPa, and is more beneficial to reaction when the pressure is higher. In the invention, the temperature of the mixing reaction of the aluminum-based composite material and water is 0-100 ℃, preferably 10-90 ℃, more preferably 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃ or 90 ℃. The mixing reaction can be carried out at normal temperature or under heating condition, and the reaction rate is higher at high temperature. The invention has no special requirement on water reacting with the aluminum matrix composite material, and can be used for tap water, sewage, river water and seawater. The method for collecting hydrogen in the present invention is not particularly limited, and a method known to those skilled in the art may be used.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
Mixing the aluminum powder and the hydroxide according to the mass ratio of 85:15, wherein the particle size of the aluminum powder is 100 meshes, and the purity is 99%; the hydroxide is a mixture of bismuth hydroxide, aluminum hydroxide and calcium hydroxide, and the mass ratio of the bismuth hydroxide to the aluminum hydroxide to the calcium hydroxide is 70:20: 10;
mixing the raw materials, putting the mixture into a corundum ball milling tank, putting the corundum ball milling tank into a glove box filled with argon, sealing, and finally carrying out ball milling on a QM-3SP2 planetary ball mill; wherein the ball-material ratio is 10:1, the ball milling time is 6h, and the ball milling rotating speed is 500r/min, so as to obtain the aluminum matrix composite.
Example 2
Mixing according to the mass ratio of aluminum to hydroxide to chloride of 80:5:15, wherein the particle size of the aluminum powder is 150 meshes, and the purity is 99%; the hydroxide is a mixture of aluminum hydroxide and bismuth hydroxide, and the mass ratio of the aluminum hydroxide to the bismuth hydroxide is 50: 50; the chloride is a mixture of bismuth chloride, sodium chloride and stannous chloride, wherein the mass ratio of the bismuth chloride to the sodium chloride to the stannous chloride is 60:30: 10;
mixing the raw materials, putting the mixture into a corundum ball milling tank, putting the corundum ball milling tank into a glove box filled with argon, sealing, and finally carrying out ball milling on a QM-3SP2 planetary ball mill; wherein the ball-material ratio is 20:1, the ball milling time is 10h, and the ball milling rotating speed is 300r/min, so as to obtain the aluminum matrix composite.
Example 3
Mixing according to the mass ratio of aluminum to hydroxide to chloride of 80:10:10, wherein the particle size of the aluminum powder is 200 meshes, and the purity is 99%; the hydroxide is a mixture of bismuth hydroxide, aluminum hydroxide and calcium hydroxide, and the mass ratio of the bismuth hydroxide to the aluminum hydroxide to the calcium hydroxide is 80:10: 10; the chloride is a mixture of sodium chloride, aluminum chloride and stannous chloride, and the mass ratio of the sodium chloride to the aluminum chloride to the stannous chloride is 70:10: 20;
mixing the raw materials, putting the mixture into a corundum ball milling tank, putting the corundum ball milling tank into a glove box filled with argon, sealing, and finally carrying out ball milling on a QM-3SP2 planetary ball mill; wherein the ball-material ratio is 30:1, the ball milling time is 20h, and the ball milling rotating speed is 400r/min, so as to obtain the aluminum matrix composite.
The morphology of the aluminum powder before ball milling in example 3 and the morphology of the aluminum-based composite material obtained after ball milling in example 3 were respectively tested, and the results are shown in fig. 1 and fig. 2, where fig. 1 is the morphology of the aluminum powder before ball milling and fig. 2 is the aluminum-based composite material after ball milling. As can be seen from the comparison between FIG. 1 and FIG. 2, the surface of the aluminum powder is smooth and compact, while the surface of the aluminum-based composite material is rough and loose, because the hydroxide and the chloride can prevent cold welding between the aluminum powder on one hand, and on the other hand can generate some active substances capable of activating the aluminum during the ball milling process, so that the aluminum powder generates more defects during the ball milling process, thereby improving the activity of the aluminum powder.
The hydrogen production performance of the aluminum-based composite materials prepared in the embodiments 1-3 is respectively tested, and the test method comprises the following steps: at 101.325kPa, 1g of the aluminum-based composite material was put into a reaction vessel containing 300mL of tap water (30 ℃ C.), and the generated hydrogen was collected by a drainage gas-collecting method and measured. The hydrogen production of the aluminum-based composite materials of examples 1 to 3 are respectively shown in fig. 1 to 3, the hydrogen production of examples 1 to 3 is over 800 ml after 600 seconds of reaction with water, it should be noted that the aluminum-based composite material of example 1 has an induction time of 7 seconds, and the aluminum-based composite material of example 1 is contacted with water for about 7 seconds to start hydrogen production, while examples 2 and 3 with chloride added have no induction time, and the hydrogen production is improved compared with example 1. This indicates that there is a synergistic effect between the hydroxide and the chloride, which can increase the hydrogen production of the aluminum matrix composite. The hydrogen production data in FIGS. 1 to 3 are shown in Table 1:
TABLE 1 examples 1 to 3 Hydrogen production (g/mL) at different times
| Time of day | Example 1 | Example 2 | Example 3 |
| |
300 | 790 | 860 |
| 60s | 550 | 860 | 930 |
| 100s | 700 | 865 | 935 |
| 200s | 710 | 870 | 935 |
| 300s | 775 | 870 | 935 |
| 400s | 785 | 870 | 935 |
| 500s | 795 | 870 | 935 |
| |
800 | 870 | 935 |
The unit of hydrogen production in table 1 is mL/g, which refers to the volume of hydrogen that can be generated by 1g of aluminum-based composite material, and the test conditions of the hydrogen volume are as follows: 101.325KPa, 30 ℃.
In conclusion, the aluminum-based composite material provided by the invention has good hydrogen production performance, and the preparation method of the aluminum-based composite material provided by the invention is simple, easy to operate, and cheap and easily available in raw materials.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the aluminum matrix composite is characterized by comprising the following steps:
and mixing aluminum, hydroxide and chloride, and performing ball milling in a protective atmosphere to obtain the aluminum-based composite material.
2. The preparation method according to claim 1, wherein the aluminum, the hydroxide and the chloride are respectively in parts by mass:
60-95 parts of aluminum;
5-25 parts of hydroxide;
0-15 parts of chloride.
3. The method according to claim 1, wherein the aluminum is a metallic aluminum powder having a particle size of 100 to 200 mesh.
4. The method of claim 1, wherein the hydroxide comprises one or more of bismuth hydroxide, aluminum hydroxide, and calcium hydroxide.
5. The method of claim 1, wherein the chloride comprises one or more of magnesium chloride, stannous chloride, aluminum chloride, sodium chloride, and bismuth chloride.
6. The preparation method according to any one of claims 1 to 5, wherein the aluminum, the hydroxide and the chloride are in parts by mass:
60-95 parts of aluminum;
5-25 parts of hydroxide;
1-15 parts of chloride;
the hydroxide is a mixture of bismuth hydroxide, aluminum hydroxide and calcium hydroxide;
the chloride is a mixture of sodium chloride, aluminum chloride and stannous chloride.
7. The preparation method of claim 1, wherein the ball-milling ball-to-material ratio is 10-30: 1, the ball-milling time is 3-20 h, and the ball-milling rotation speed is 300-550 r/min.
8. The preparation method according to claim 7, wherein the material of the ball milling pot and the material of the grinding balls are corundum.
9. An aluminium matrix composite material obtainable by a process as claimed in any one of claims 1 to 8.
10. Use of the aluminium matrix composite material according to claim 9 for the preparation of hydrogen, comprising the steps of:
mixing the aluminum matrix composite material with water for reaction, and collecting hydrogen; the temperature of the mixing reaction is 0-100 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093605A (en) * | 2022-08-05 | 2022-09-23 | 浙江荣泰科技企业有限公司 | Preparation method and application of aluminum hydroxide-tin bismuth alloy hybrid powder material |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093605A (en) * | 2022-08-05 | 2022-09-23 | 浙江荣泰科技企业有限公司 | Preparation method and application of aluminum hydroxide-tin bismuth alloy hybrid powder material |
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