CN108751128A - A kind of method that physics ball milling metal powder produces hydrogen energy source - Google Patents
A kind of method that physics ball milling metal powder produces hydrogen energy source Download PDFInfo
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- CN108751128A CN108751128A CN201810668532.0A CN201810668532A CN108751128A CN 108751128 A CN108751128 A CN 108751128A CN 201810668532 A CN201810668532 A CN 201810668532A CN 108751128 A CN108751128 A CN 108751128A
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- metal powder
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- ball milling
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- hydrogen
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- 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
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- 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
Abstract
The present invention provides a kind of methods that physics ball milling metal powder produces hydrogen energy source.Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, carries out wet ball grinding under hydrogen protection, is removed the hydroxide that oxide layer or reaction generate under ball action by metal powder.This method in metal powder hydrogen manufacturing by applying auxiliary agent and physics ball milling, so that the oxide/hydroxide film generated in hydrolytic hydrogen production reaction is removed with metal powder, it can effectively ensure that hydrogen manufacturing yield and reaction rate, and whole process is easy to operate, reaction process is neutrality, low for equipment requirements, production cost is low.
Description
Technical field
The present invention relates to hydrogen preparation fields, more particularly to a kind of method that physics ball milling metal powder produces hydrogen energy source.
Background technology
Hydrogen Energy is just obtaining the extensive concern of country as a kind of green, the energy of sustainable development, and Hydrogen Energy is also ecological text
One of the importance of bright construction.On a large scale, inexpensively production hydrogen is one of the important link for developing and utilizing Hydrogen Energy, hydrogen one
The reproducible secondary energy sources of kind, calorific value is high, and reaction speed is fast, can be made by a variety of reaction paths.Hydrogen is after releasing energy
By-product be water, it is environmentally friendly.Although current Hydrogen Energy is used widely not yet, with the fossil energy increasingly decayed
The problems such as source and energy crisis getting worse, is but of great significance to the research and development of Hydrogen Energy.
For the source of Hydrogen Energy, mainly there is the following aspects：Photoelectrocatalysis hydrolytic hydrogen production, biomass hydrogen preparation, hydroboration
Object hydrolytic hydrogen production, water electrolysis hydrogen production, catalytically reforming hydrogen producing technology, metal and material hydrolytic hydrogen production etc..At present both at home and abroad research compared with
Hot is the hydrolytic hydrogen production technology of metal_based material.Metal_based material hydrogen manufacturing is mainly lived using metal chemistries such as aluminium, magnesium
Sprinkle, can occur self-corrosion evolving hydrogen reaction under room temperature in the solution, this alloy hydrolysis hydrogen manufacturing be a kind of very promising energy storage and
Energy converslon materials.
Chinese invention patent application number 201710017327.3 discloses a kind of preparation method of magnesium alloy hydrogen manufacturing material；
Magnesium alloy hydrogen manufacturing material is using magnesium, aluminum metal powder or magnesium-aluminum metal alloyed powder as presoma, mechanical mixture salt of weak acid, briquetting, height
Temperature processing, obtains magnesium alloy hydrogen manufacturing material；The molar ratio of magnesium and aluminium is 0.1 ~ 1, and salt of weak acid is magnesium alloy quality
0.01 ~ 20wt%；The cation of salt of weak acid is one kind of sodium, potassium, calcium, barium and strontium；Weak acid salt anionic is bismuthic acid root, stannic acid
One kind of root, ferrous acid root, germanic acid root, meta-aluminic acid root and inclined zincic acid root.
Chinese invention patent application number 201310287296.5 discloses a kind of fast hydrogen making agent, by aluminium, magnesium, calcium oxide,
Low-melting-point metal, rubbing agent, adhesive and antioxidant form by a certain percentage.Aluminium is the major function material of hydrogen production agent,
A large amount of activation point is formed on its surface under the collective effect of magnesium and low-melting-point metal, then after chance water produced by calcium oxide
Alkaline environment in occur hydrolysis generate hydrogen.Rubbing agent can prevent the reunion of metallic aluminium in mechanical milling process；Adhesive
The shape of transport easy to package can will be processed into after ball milling in powdered hydrogen production agent；Antioxidant can prevent the oxidation of hydrogen production agent,
Convenient for long time stored.
Chinese invention patent application number 201010290898.2 discloses a kind of neutral and water at normal temperature solution hydrogen manufacturing aluminium base
Compound and preparation method thereof, the aluminum-based composites by elemental metals pure aluminium powder and prevent aluminium powder is generated in mechanical milling process glue
Knot, and in water generate dense oxidation film and rise catalytic action amorphous or nanometer crystal alloy strip composition, metal pure aluminium powder with
The ratio of amorphous or nanometer crystal alloy strip is that (Y=0.1 ~ 20) 100: Y, the particle size range of metal pure aluminium powder exist in mass ratio
0.01~10um.The preparation method of the invention hydrolytic hydrogen production aluminum-based composites is after mixing above-mentioned material, to be obtained through high-energy ball milling
To aluminum-based composites.
Chinese invention patent application number 201710039768.3 disclose a kind of Al-LiH- metal oxides hydrogen manufacturing material and
Preparation method, the material are formed by aluminium powder and additive ball milling, and additive is LiH and metal oxide；The quality hundred of aluminium powder
Divide than being 50 ~ 95%, the mass percent of additive is 5 ~ 50%.Preparation method includes：（1）Aluminium is weighed by certain mass ratio
Powder, LiH and metal oxide, are added together with abrading-ball in ball grinder, sealing；（2）Ball milling obtains hydrogen manufacturing material；（3）It takes out
Hydrogen manufacturing material.
According to above-mentioned, in the reaction process of the metal_based material hydrogen manufacturing in existing scheme, the hydroxide and oxygen that easily generate
Change film and be simultaneously attached to metal surface, inhibit hydrolysis, and the mode of traditional destruction oxidation film or hydroxide film be mainly alkali,
Hydride, butter and alloy are blended, and manufacturing cost is higher, and metal price used in its alloying is relatively
Height, reaction residue is difficult to be recycled, therefore overall cost is higher.In consideration of it, the present invention proposes a kind of physics ball milling gold
The method for belonging to powder extraction hydrogen energy source, can effectively solve above-mentioned technical problem.
Invention content
For in the wider metal_based material hydrogen manufacturing of current application, in Surface Creation hydroxide and oxidation film, inhibit
Hydrolytic hydrogen production reaction efficiency, and the mode manufacturing cost of traditional destruction skin covering of the surface is high, to equipment requirement height, while alloy material
Material manufacturing cost itself is high, and the present invention proposes a kind of method that physics ball milling metal powder produces hydrogen energy source, to effectively improve
Hydrogen production efficiency, and it is simple for process, and manufacturing cost is low, and hydrogen purity is high.
Specific technical solution of the present invention is as follows：
A kind of method that physics ball milling metal powder produces hydrogen energy source, the method that the physics ball milling metal powder produces hydrogen energy source
Process be：Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, in hydrogen shield
Lower carry out wet ball grinding is removed the hydroxide that oxide layer or reaction generate under ball action by metal powder, exposure
Go out more active sites, to improve hydrogen manufacturing yield and reaction rate.
Preferably, the metal powder is one or both of aluminium powder, magnesium powder.
Preferably, the metal chloride is one or both of aluminium chloride, magnesium chloride.
Preferably, the mass concentration of the metal chloride aqueous solution is 30 ~ 40%.
Preferably, the auxiliary agent be iron, copper, tin, zinc, magnesium sulfate, calcium chloride, barium sulfate, calcium sulfate, in strontium carbonate extremely
Few one kind.
Preferably, the vacuum degree of the vacuum ball mill is 0.001 ~ 0.1Pa.
Preferably, the sphere of the vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.
Preferably, the rotating speed of the ball milling is 250 ~ 350r/min, and Ball-milling Time is 60 ~ 90min.
Preferably, in the wet ball grinding system, 72 ~ 82 parts by weight of metal powder, 15 ~ 20 weight of metal chloride aqueous solution
Measure part, 3 ~ 8 parts by weight of auxiliary agent.
Since aluminium, magnesium chemical property are active, self-corrosion evolving hydrogen reaction, alloy hydrolysis can occur under room temperature in the solution
Hydrogen manufacturing is a kind of very promising energy storage and energy converslon materials.But the hydroxide that aluminium, magnesium metal generate during the reaction
It can be attached to metal surface with oxidation film, to inhibit its hydrolysis.Traditional mode for destroying oxidation film or hydroxide film
Predominantly alkali, hydride, butter and alloy are blended, and manufacturing cost is higher, and such as Sn of metal used in alloying,
The prices such as In, Bi, Sr are relatively high, and reaction residue improves overall cost without being recycled.The innovation of the present invention
Point is to make the oxide/hydroxide of magnesium/aluminum metal powder face be detached from metal powder by ball milling, to promote hydrogen manufacturing
The precipitation of reaction and hydrogen.The metal salt assitant being added simultaneously has facilitation, by-product with metal chloride to evolving hydrogen reaction
Required ceramic based sizing can be obtained by adjusting each component content, improve the utility value of by-product.
The Hydrogen Energy preparation method of above-mentioned assistant metal powder provided by the invention, will under ball action by metal powder
The hydroxide stripping that oxide layer or reaction generate, exposes more active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal chloride can improve surface-active with auxiliary agent, simultaneously participate in subsequent reactions and form corresponding ceramic slurry.Meanwhile passing through
Ball milling makes the oxide/hydroxide of magnesium/aluminum metal powder face be detached from metal powder, to promote hydrogen production reaction and hydrogen
Precipitation.Metal salt assitant has facilitation, by-product can be by adjusting each group evolving hydrogen reaction with metal chloride simultaneously
Divide content to obtain required ceramic based sizing, improves the utility value of by-product.
The present invention provides a kind of methods that physics ball milling metal powder produces hydrogen energy source, compared with prior art, dash forward
The characteristics of going out and excellent effect are：
1, propose that auxiliary agent is added in vacuum ball mill carries out the method that assistant metal powder Hydrogen Energy is produced.
2, by applying ball milling in metal powder hydrogen manufacturing so that the oxide/hydroxide generated in hydrolytic hydrogen production reaction
Object film is removed with metal powder, can effectively ensure that hydrogen manufacturing yield and reaction rate.
3, the hydrogen purity that method used in the present invention obtains is high, easy to operate, and reaction process is neutrality, is wanted to equipment
It asks relatively low, existing ball-grinding machine transformation can be used directly, the later stage reaction source realization can be added simultaneously continuously by detaching slurry
Metaplasia is produced, and large-scale industrial production is suitable for.
4, the preparation of hydrogen of the present invention can carry out during preparing aluminium base or magnesium-based ceramic material, be helped by adjusting
Agent content forms corresponding ceramic slurry, so as to effectively reduce production cost.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is aluminium chloride.The mass concentration of metal chloride aqueous solution is 30%.It helps
Agent is copper.The vacuum degree of vacuum ball mill is 0.001Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling
Rotating speed is 250r/min, Ball-milling Time 90min.In wet ball grinding system, 72 parts by weight of metal powder, metal chloride are water-soluble
20 parts by weight of liquid, 8 parts by weight of auxiliary agent.
Embodiment 2
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is magnesium chloride.The mass concentration of metal chloride aqueous solution is 40%.It helps
Agent is strontium carbonate.The vacuum degree of vacuum ball mill is 0.1Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling
Rotating speed be 250r/min, Ball-milling Time 60min.In wet ball grinding system, 82 parts by weight of metal powder, metal chloride water
15 parts by weight of solution, 3 parts by weight of auxiliary agent.
Embodiment 3
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is magnesium chloride.The mass concentration of metal chloride aqueous solution is 32%.It helps
Agent is calcium sulfate.The vacuum degree of vacuum ball mill is 0.01Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling
Rotating speed be 280r/min, Ball-milling Time 80min.In wet ball grinding system, 77 parts by weight of metal powder, metal chloride water
15 parts by weight of solution, 8 parts by weight of auxiliary agent.
Embodiment 4
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is aluminium chloride.The mass concentration of metal chloride aqueous solution is 38%.It helps
Agent is copper.The vacuum degree of vacuum ball mill is 0.1Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling turns
Speed is 320r/min, Ball-milling Time 70min.In wet ball grinding system, 80 parts by weight of metal powder, metal chloride aqueous solution
15 parts by weight, 5 parts by weight of auxiliary agent.
Embodiment 5
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is magnesium chloride.The mass concentration of metal chloride aqueous solution is 40%.It helps
Agent is zinc.The vacuum degree of vacuum ball mill is 0.05Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling turns
Speed is 300r/min, Ball-milling Time 75min.In wet ball grinding system, 75 parts by weight of metal powder, metal chloride aqueous solution
20 parts by weight, 5 parts by weight of auxiliary agent.
Embodiment 6
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution and auxiliary agent is added, under hydrogen protection into
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, is exposed more by row wet ball grinding
More active sites, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is magnesium chloride.The mass concentration of metal chloride aqueous solution is 35%.It helps
Agent is barium sulfate.The vacuum degree of vacuum ball mill is 0.1Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.Ball milling
Rotating speed be 250r/min, Ball-milling Time 90min.In wet ball grinding system, 82 parts by weight of metal powder, metal chloride water
15 parts by weight of solution, 3 parts by weight of auxiliary agent.
Test method is：
Weigh aluminium powder（Purity is 99%, and average grain diameter is 40 μm）1g, input are equipped in the round-bottomed flask of 200mL distilled water, are utilized
Scale is accurate to the 100mL graduated cylinders of 0.1mL, and the hydrogen that reaction generates is collected using drainage；React the volume of the hydrogen generated
For V, reaction time t, aluminium powder quality is m, hydrogen-producing speed V/（t·m）, the hydrogen total volume after the completion of reacting is VAlways, production
Hydrogen amount is VAlways/m。
Pass through the assistant metal powder for the embodiment 6 that the above method measures（Aluminium powder）Hydrogen-producing speed, the hydrogen of the method for hydrogen manufacturing
Yield and hydrogen manufacturing cost are as shown in table 1.
Comparative example 1
Metal powder is placed in vacuum ball mill, auxiliary agent is added, carries out wet ball grinding under hydrogen protection, passes through metal powder
The hydroxide that oxide layer or reaction generate is removed under ball action, more active sites are exposed, to improve hydrogen manufacturing
Yield and reaction rate.
Metal powder is aluminium powder.Auxiliary agent is barium sulfate.The vacuum degree of vacuum ball mill is 0.1Pa.The ball of vacuum ball mill
Body is zirconium ball, ratio of grinding media to material 2:1.The rotating speed of ball milling is 250r/min, Ball-milling Time 90min.In wet ball grinding system, metal
97 parts by weight of powder, 3 parts by weight of auxiliary agent.
Chloride is not added for comparative example 1.
Comparative example 2
Metal powder is placed in vacuum ball mill, a small amount of metal chloride aqueous solution is added, carries out wet method under hydrogen protection
The hydroxide that oxide layer or reaction generate is removed by metal powder under ball action, exposes more activity by ball milling
Site, to improve hydrogen manufacturing yield and reaction rate.
Metal powder is aluminium powder.Metal chloride is magnesium chloride.The mass concentration of metal chloride aqueous solution is 35%.Very
The vacuum degree of empty ball mill is 0.1Pa.The sphere of vacuum ball mill is zirconium ball, ratio of grinding media to material 2:1.The rotating speed of ball milling is 250r/
Min, Ball-milling Time 90min.In wet ball grinding system, 85 parts by weight of metal powder, 15 parts by weight of metal chloride aqueous solution.
Auxiliary agent is not added for comparative example 2.
Test method is：
Hydrogen producing rate and hydrogen output, and account cost are tested, as shown in table 1.
Table 1：
Claims (9)
1. a kind of method that physics ball milling metal powder produces hydrogen energy source, which is characterized in that the physics ball milling metal powder system
The process of the method for hydrogen energy source is taken to be：Metal powder is placed in vacuum ball mill, be added a small amount of metal chloride aqueous solution and
Auxiliary agent carries out wet ball grinding under hydrogen protection, the hydrogen for being generated oxide layer or reaction under ball action by metal powder
Oxide is removed, and more active sites are exposed, and hydrogen is precipitated.
2. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：The gold
Category powder is one or both of aluminium powder, magnesium powder.
3. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：The gold
Category chloride is one or both of aluminium chloride, magnesium chloride.
4. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：The gold
The mass concentration for belonging to aqueous chloride solution is 30 ~ 40%.
5. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：It is described to help
Agent is at least one of iron, copper, tin, zinc, magnesium sulfate, calcium chloride, barium sulfate, calcium sulfate, strontium carbonate.
6. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：It is described true
The vacuum degree of empty ball mill is 0.001 ~ 0.1Pa.
7. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：It is described true
The sphere of empty ball mill is zirconium ball, ratio of grinding media to material 2:1.
8. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：The ball
The rotating speed of mill is 250 ~ 350r/min, and Ball-milling Time is 60 ~ 90min.
9. a kind of method that physics ball milling metal powder produces hydrogen energy source according to claim 1, it is characterised in that：It is described wet
In method ball milling system, 72 ~ 82 parts by weight of metal powder, 15 ~ 20 parts by weight of metal chloride aqueous solution, 3 ~ 8 parts by weight of auxiliary agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498803A (en) * | 2020-05-22 | 2020-08-07 | 苏州思美特表面材料科技有限公司 | Hydrogen production method |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498803A (en) * | 2020-05-22 | 2020-08-07 | 苏州思美特表面材料科技有限公司 | Hydrogen production method |
| CN111498803B (en) * | 2020-05-22 | 2022-04-29 | 苏州思美特表面材料科技有限公司 | Hydrogen production method |
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Application publication date: 20181106 |