CN110102280A - A kind of activating agent and preparation method thereof for hydrogen storage material - Google Patents

A kind of activating agent and preparation method thereof for hydrogen storage material Download PDF

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Publication number
CN110102280A
CN110102280A CN201910357474.4A CN201910357474A CN110102280A CN 110102280 A CN110102280 A CN 110102280A CN 201910357474 A CN201910357474 A CN 201910357474A CN 110102280 A CN110102280 A CN 110102280A
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activating agent
preparation
hydrogen
annealing
inert gas
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李志林
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Zhuzhou Platinum Land New Energy Technology Co ltd
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Beijing Platinum Land Hydrogen Energy Technology Development Co Ltd
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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    • 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
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
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Abstract

This application discloses a kind of activating agents and its manufacturing method for hydrogen storage material, wherein the chemical general formula of the activating agent are as follows: MxNyWherein, x and y respectively indicates the atomicity of M and N, 0 x≤90 <, 0 y≤80 <, one or more of x+y=100, M Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru, one or more of N Li, Pd, Nb, La, Ce, Nd, Sm and Y.Activating agent of the invention, which can shorten, to be filled and (adds) hydrogen, puts (de-) hydrogen response time, and then improves hydrogen-storing device responding ability.

Description

A kind of activating agent and preparation method thereof for hydrogen storage material
Technical field
This application involves Hydrogen Technology fields, more particularly to a kind of for the activating agent of hydrogen storage material and its preparation side Method.
Background technique
Hydrogen (H) is located at first in the periodic table of elements, is widely present in nature.Hydrogen Energy refers to hydrogen and oxygen The chemical energy that reaction releases is learned, is a kind of clean secondary energy sources, with energy density is big, combustion heat value is high, source is wide, can Storage, it is renewable, can the flammable, no pollution of electricity, zero carbon row the advantages that, help to solve energy crisis and environmental pollution etc. to ask Topic, is known as " ultimate energy " of 21 century.
Currently, as the energy and environmental crisis are on the rise, Hydrogen Energy industry development, hydrogen manufacturing, hydrogen storage, use are accelerated both at home and abroad Technology fast development is realized in the fields such as hydrogen (fuel cell), hydrogenation stations, and a large amount of innovation achievements and application product explosion type emerge in large numbers, It is widely applied in fields such as automobile, rail traffic, ship, space flight, logistics system, mine car, fork truck, energy storage, industry health hair Exhibition, it is contemplated that " Hydrogen Energy society " will be formed soon.
Therefore, urgent problem to be solved is to develop when one kind is reacted with hydrogen and hydrogen-containing compound to have larger promotion at present The activating agent of effect, and price is human-oriented, is able to ascend technology while reducing cost.
Therefore, the defect to solve current technology, it is necessary to propose a kind of activating agent for hydrogen storage material.
Summary of the invention
Aiming to overcome that the above problem or at least being partially solved or extenuate for the application solves the above problems.
According to the one aspect of the application, a kind of activating agent for hydrogen storage material, the chemistry of the activating agent are proposed General formula are as follows: MxNy, wherein x and y respectively indicates the atomicity of M and N, 0 < x≤90,0 < y≤80, x+y=100, M Al, One or more of Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru, N Li, Pd, Nb, La, Ce, Nd, Sm And one or more of Y.
Preferably, the activating agent are as follows: Al20La80、Al75Fe5Li20、Sn70Pt20Nd10、Fe15Co15Y70、 Ni75Ru10Y15、Sn75Mg10Nd10Sm5、Ti22Fe22Nb56、(FeV80)60Ce40、Ag25Pd75And Ti22Cr40Mn4Nb34In one Kind is several.
According to the one aspect of the application, a kind of preparation method of activating agent for hydrogen storage material, the system are proposed Preparation Method includes:
It S1 is) M according to chemical general formulaxNyConfiguring the raw material of activating agent, wherein x and y respectively indicates the atomicity of M and N, and 0 One in < x≤90,0 < y≤80, x+y=100, M Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru Kind or several, one or more of N Li, Pd, Nb, La, Ce, Nd, Sm and Y；
S2) under vacuum or inert gas environment, activating agent described in melting is to be made as cast condition activating agent；
S3) under vacuum or inert gas environment, the as cast condition activating agent is made annealing treatment to obtain annealing activity Agent；
S4 the quick-fried broken processing of hydrogen) is carried out to the annealing activating agent, the activating agent is made.
Preferably, in step S2), the vacuum degree of vacuum environment is 5 × 10-3Inertia in Pa or inert gas environment Gas pressure is 0.05-0.08MPa；And
Method of smelting is electric arc melting, and fusion process turns over the raw material melting 3-5 times；Or method of smelting is induction Melting, selected crucible is three high graphite crucibles or zirconia ceramic crucible in fusion process.
Preferably, in step S3), the vacuum degree of vacuum environment is 5 × 10-3Inertia in Pa or inert gas environment The pressure of gas is 0.05-0.08MPa；And
To the as cast condition activating agent in 500 DEG C of -1500 DEG C of annealing 3h-12h.
Preferably, in step S4), the quick-fried broken processing of hydrogen is carried out to the annealing activating agent in the case where Hydrogen Vapor Pressure is 4MPa,
Preferably, after carrying out the quick-fried broken processing of hydrogen to the annealing activating agent, to the annealing activating agent in 100-400 DEG C It carries out vacuumizing 30-120 minutes under environment and handle.
Preferably, to pulverization process is carried out after the annealing activating agent vacuumize process, to obtain the work of powdered form Property agent.
Preferably, the granularity of the activating agent is 19 μm or less.
Preferably, further include step S5), wherein step S5) are as follows: packing processes, manner of packing are carried out to the activating agent Using vacuumizing or filling with inert gas is to the activating agent protection packaging.
Of the invention has the advantage that:
1. hydrogen storage material and its catalyst activating agent of the invention, hydrogenation activity with higher, room temperature low pressure (20 DEG C, 0.5MPa) environment activated the incubation time less than 3 seconds, used in hydrogen storage material and its catalyst as activating agent, can Shortening fills and (adds) hydrogen, puts (de-) hydrogen response time, and then improves hydrogen-storing device responding ability.
2. inert element and active element are arranged in pairs or groups, were both reduced by hydrogen storage material and its catalyst activating agent of the invention The use cost of high active material, and improve activating agent property stable in the air, it is convenient for safety in transportation and storage.
3. hydrogen storage material and its catalyst of the invention activating agent are in powder structure, female in hydrogen storage material and its catalyst Easy to use, the far super base material of Acceptable life is added in material.
According to the accompanying drawings to the detailed description of the specific embodiment of the application, those skilled in the art will be more Above-mentioned and other purposes, the advantages and features of the application are illustrated.
Detailed description of the invention
Some specific embodiments of the application are described in detail by way of example and not limitation with reference to the accompanying drawings hereinafter. Identical appended drawing reference denotes same or similar part or part in attached drawing.It should be appreciated by those skilled in the art that these What attached drawing was not necessarily drawn to scale.In attached drawing:
Fig. 1 is the process flow diagram for preparing the activating agent for hydrogen storage material according to an embodiment of the present application；
Fig. 2 is the process flow diagram that the activating agent of hydrogen storage material is used for according to the preparation of another embodiment of the application；
Fig. 3 is the Ti for hydrogen storage material of the invention22Fe22Nb56The metallograph of activating agent；
Fig. 4 is the Ti for hydrogen storage material of the invention22Fe22Nb56The distribution of particle sizes test result of activating agent；And
Fig. 5 is that hydrogenation activity function of the present invention preparation for the embodiment 11-15 of the activating agent of hydrogen storage material is surveyed Test result.
Code name meaning in figure: A-TiFe phase region；B-richness Nb phase region.
Specific embodiment
In being described below, for illustration and not for limitation, propose such as based on the medium-term and long-term of user's energy characteristic The detail of load forecasting method, technology etc, to understand thoroughly the embodiment of the present invention.However, those skilled in the art Member in the other embodiments without these details it should be clear that also may be implemented the present invention.In other situations, it omits To well-known based on user's detailed description of the Mid-long term load forecasting method of energy characteristic, in case unnecessary details hampers Hinder description of the invention.
In addition, to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment and phase Technical solution of the present invention is clearly and completely described in the attached drawing answered.Obviously, described embodiment is only the present invention one Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
In order to illustrate technical solutions according to the invention, the following is a description of specific embodiments.
The embodiment provides a kind of activating agent for hydrogen storage material, the chemical general formulas of the activating agent are as follows: MxNy, wherein x and y respectively indicates the atomicity of M and N, 0 < x≤90,0 < y≤80, x+y=100, M Al, Ti, V, Cr, One or more of Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru, in N Li, Pd, Nb, La, Ce, Nd, Sm and Y It is one or more of.
Embodiment 1 to 10 as follows is the specific embodiment of the activating agent for hydrogen storage material of the invention, is implemented The content of example 1 to 10 is shown in Table 1.Table 1 is activating agent (wherein, the activating agent of the invention for hydrogen storage material of the invention For for hydrogen storage material and its catalyst, thus the activating agent for hydrogen storage material of the invention be alternatively referred to as hydrogen storage material and its Catalyst activating agent) representative formulations component.
Table 1
The embodiment of the present invention also proposed a kind of preparation method for manufacturing the above-mentioned activating agent for hydrogen storage material, described Preparation method includes:
It S1 is) M according to chemical general formulaxNyConfiguring the raw material of activating agent, wherein x and y respectively indicates the atomicity of M and N, and 0 One in < x≤90,0 < y≤80, x+y=100, M Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru Kind or several, one or more of N Li, Pd, Nb, La, Ce, Nd, Sm and Y；
S2) under vacuum or inert gas environment, activating agent described in melting is to be made as cast condition activating agent；
S3) under vacuum or inert gas environment, the as cast condition activating agent is made annealing treatment to obtain annealing activity Agent；And
S4 the quick-fried broken processing of hydrogen) is carried out to the annealing activating agent, the activating agent is made.
Further, in step sl, raw material disposal is carried out first, specifically, materials statement surface treatment, removal oxidation Layer.In the activating agent MxNyIn, the surface oxide layer of raw material M is removed and is dried using olefin(e) acid cleaning, material N Surface oxide layer uses and is mechanical grinding to display metallic luster.Then according to stoichiometric ratio ingredient between activating agent element.It is excellent Selection of land, in this step, purity >=95% of selected alloy raw material.
Further, in step s 2, under vacuum or inert gas shielding environment, as cast condition is prepared using melting Activating agent, method of smelting include: the melting of resistance stove heating, induction melting, smelting in suspension, electric arc melting method.Preferably, at this In step, smelting preparation method is electric arc melting, and to guarantee alloy microstructure uniformity, fusion process turns over melting to alloy 3-5 times；Alternatively, the smelting preparation method in the step is induction melting, selected crucible is three high graphite crucibles or zirconium oxide pottery Porcelain crucible.
Further, in step s3, as cast condition activating agent is under vacuum or inert gas shielding environment, in 500-1500 DEG C (such as 600 DEG C, 750 DEG C, 800 DEG C) anneal 3-12 hour, cool to room temperature with the furnace and obtain activating agent of annealing.Studies have shown that adopting Facilitate the activity of activating agent after being made annealing treatment with the temperature and annealing time to as cast condition activating agent.
Preferably, in step S2 and S3, vacuum environment vacuum degree reaches 5 × 10-3Pa or inert gas shielding environment Pressure is 0.05-0.08MPa.
Further, in above-mentioned steps S4, to annealing activating agent carry out the quick-fried broken processing of hydrogen, Hydrogen Vapor Pressure 4MPa, with 100-400 DEG C of environment vacuumizes 30-120 minutes afterwards, further using being mechanically pulverized, obtains Agent Powder, granularity is 19 μ M is hereinafter, specifically, carry out 800 mesh sub-sieves to Agent Powder, acquisition partial size is in 19 μm of Agent Powders below.Preferably, Mechanical crushing method in this step is mechanical spheroidal graphite under air-flow crushing or inert atmosphere protection.
Further, in above-mentioned steps S5, packing processes are carried out to Agent Powder, manner of packing is used and vacuumized Or filling with inert gas protection packaging, to obtain final activating agent.
Preparation method of the invention is described in detail referring now to embodiment 11-15.
Embodiment 11
The hydrogen storage material and its catalyst activating agent of embodiment 1, the preparation method of use are as follows in a kind of above-mentioned table 1 (example 1, example 2, example 3,4 activating agent fusing point of example are below 1000 DEG C in above-mentioned table 1, and preparation method is similar to this):
Aluminum feedstock use purity for 99% commercial-purity aluminium, polishing removal surface scale, lithium raw material use purity for 99% battery grade lithium stick.It is that 20:80 weighs aluminium, lithium raw material, and broken mixing is placed in height according to Al and La atomic ratio In pure zirconia crucible, it is put into resistance furnace together.Burner hearth is vacuumized 15 minutes, and is filled with high-purity argon gas, to burner hearth air After cyclic permutation 5 times, it is filled with 0.8MPa argon gas, in the case where argon atmosphere protects environment, resistance furnace is warming up to 700 DEG C.It is complete to aluminium, lithium It is primary every stirring in 5 minutes after full-fusing, heating device of electric resistance furnace is closed after 6 stirrings, to Al20La80Alloy is with furnace It is cooled to room temperature, cast alloy is taken out in blow-on.By Al20La80It is further broken using airflow milling after cast alloy cutting and crushing, By 800 mesh sub-sieves, obtains partial size and reused in 19 μm of Agent Powders below not by the active agent particle of sub-sieve Airflow milling is broken.It is vacuumized with aluminium foil bag and packs Al20La80Activating agent.
Embodiment 12
The hydrogen storage material and its catalyst activating agent of embodiment 5 in a kind of above-mentioned table 1, use the preparation method is as follows:
Nickel raw material uses purity for 99% technical pure metal nickel powder, and ruthenium raw material uses purity for 99% pure metal ruthenium powder, Yttrium raw material use purity for 97% micron order yttrium powder, according to Ni, Ru, Y atomic ratio be 75:10:15 weigh nickel powder, ruthenium powder, Yttrium powder, three kinds of raw materials are poured into after mixing in the three high graphite crucibles of oil surface BN, and are put into medium frequency induction melting furnace. To induction melting furnace pumping high vacuum to 5 × 10-3Pa, induction heating is to 1250 DEG C, after raw material melt completely, every 5 minutes electricity Magnetic stirring is primary, and heating is closed in melting after twenty minutes, and melting charge is poured onto rotary water-cooled copper dish, to alloy remaining in crucible After being cooled to room temperature with the cast alloy in water cooled copper plate, Ni is taken out in blow-on75Ru10Y15Alloy.It will be in water cooled copper plate Ni75Ru10Y15It is further broken using airflow milling after cast alloy percussion is broken, by 800 mesh sub-sieves, partial size is obtained at 19 μm It is broken to reuse airflow milling not by the active agent particle of sub-sieve for Agent Powder below.It is vacuumized and is packed with aluminium foil bag Ni75Ru10Y15Activating agent.
Embodiment 13
The hydrogen storage material and its catalyst activating agent of embodiment 6 in a kind of above-mentioned table 1, use the preparation method is as follows:
Tin raw material uses purity for 99% technical pure metal block tin, and magnesium raw material uses purity for 99% pure metal MAG block, Neodymium raw material uses purity for 99% pure metal neodymium block, and samarium raw material uses purity for 99% pure metal samarium block, and mechanical grinding removes table After surface oxidized skin, block tin, MAG block, neodymium block, samarium block are weighed according to Sn, Mg, Nd, Sm atomic ratio 75:10:10:5.By four kinds of originals Expect in the water-cooled red copper crucible for dividing valve being put into Cold Crucible Induction Levitation Melting furnace, pumping high vacuum to 3 × 10-3Pa is filled with height For pure argon to 0.7MPa, induction heating closes heating after melting completely to 1000 DEG C, raw material, turns over after alloy cooling and solidifying Turn alloy cast ingot, again melting, repeatedly melting 5 times, by the Sn of molten condition after last time melting75Mg10Nd10Sm5It closes Gold is poured onto rotary water-cooled copper dish, after the cast alloy on alloy remaining in crucible and water cooled copper plate is cooled to room temperature, opens Furnace takes out Sn75Mg10Nd10Sm5Alloy.By the Sn in water cooled copper plate75Mg10Nd10Sm5After cast alloy percussion is broken, further adopt It is broken with airflow milling, by 800 mesh sub-sieves, partial size is obtained in 19 μm of Agent Powders below, does not pass through the activating agent of sub-sieve It is broken to reuse airflow milling for particle.It is vacuumized with aluminium foil bag and packs Sn75Mg10Nd10Sm5Activating agent.
Embodiment 14
The hydrogen storage material and its catalyst activating agent of embodiment 7 in a kind of above-mentioned table 1, use the preparation method is as follows:
Titanium material uses purity for 98% industrial titanium sponge, through mild acid wash and is dried, and iron material uses purity For 99% pure metal iron staff, grinder buffing removes surface scale, and niobium raw material uses purity for 99% pure metal niobium stick, according to Ti, Fe, Nb atomic ratio 22:22:56 are weighed, and are placed in the crucible of arc-melting furnace after shredding mixing, pumping high vacuum to 5 ×10-3Pa, is filled with high-purity argon gas to 0.8MPa, and the alloy raw material in electric arc melting crucible closes electric arc after melting completely, wait close Alloy cast ingot is overturn after gold cooling and solidifying, melt back 5 times, after the alloy cast ingot in crucible is cooled to room temperature, blow-on is taken out Ti22Fe22Nb56Alloy cast ingot (ingot casting metallograph is as shown in Figure 2).By Ti22Fe22Nb56Alloy cast ingot is put into hydrogenation reaction cauldron In, it is filled with high-purity hydrogen and discharges hydrogen after hydrogen equilibrium pressure to 4MPa, reaction kettle is warming up to 100 DEG C and vacuumizes 30 points Clock, is then cooled to room temperature, take out hydrogen it is quick-fried it is broken after Ti22Fe22Nb56Powder, it is further 60 minutes broken using high energy spheroidal graphite. By 800 mesh sub-sieves, partial size is obtained in 19 μm of Agent Powders (particle size test result is as shown in Figure 3) below, is not passed through It is broken to reuse high energy spheroidal graphite for the active agent particle of sub-sieve.It is vacuumized with aluminium foil bag and packs Ti22Fe22Nb56Activating agent.
Embodiment 15
The hydrogen storage material and its catalyst activating agent of embodiment 8 in a kind of above-mentioned table 1, use the preparation method is as follows:
Iron and vanadium raw materials select 80 (FeV of ferrovanadium80) intermediate alloy block, cerium raw material use purity for 99% industrial pure metal Cerium ingot, two kinds of raw materials remove surface scale with grinder buffing.According to FeV80It is that 60:40 weighs ferrovanadium with Ce atomic ratio 80 intermediate alloy blocks, cerium ingot, and broken mixing is placed in the crucible of arc-melting furnace, pumping high vacuum to 3 × 10-3Pa is filled with High-purity argon gas is to 0.8MPa, and alloy raw material in electric arc melting crucible closes electric arc after melting completely, after alloy cooling and solidifying Alloy cast ingot is overturn, melt back 5 times, after the alloy cast ingot in crucible is cooled to room temperature, (FeV is taken out in blow-on80)60Ce40It closes Golden ingot casting.By (FeV80)60Ce40Alloy cast ingot is put into hydrogenation reaction cauldron, is filled with high-purity hydrogen to 4MPa, is put down to Hydrogen Vapor Pressure After weighing apparatus, discharge hydrogen, reaction kettle be warming up to 400 DEG C and is vacuumized 30 minutes, be then cooled to room temperature, take out hydrogen it is quick-fried it is broken after (FeV80)60Ce40Powder, it is further 90 minutes broken using high energy spheroidal graphite.By 800 mesh sub-sieves, obtain partial size 19 μm with Under Agent Powder it is broken to reuse high energy spheroidal graphite not by the active agent particle of sub-sieve.It is vacuumized and is packed with aluminium foil bag (FeV80)60Ce40Activating agent.
Hydrogen storage material made from above-described embodiment 11,12,13,14,15 and its catalyst activating agent, according to national standard GB/T 1479.1-2011 " the measurement part 1 of metal powder apparent density: funnel method " determines the apparent density of activating agent, uses Pressure-component-temperature (PCT) tester carries out hydrogenation kinetics performance test, as shown in table 2 and Fig. 5.Table 2 is to implement Activating agent performance characteristic made from example 11-15, specific performance characteristic is referring to table 2.
Table 2
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this Shen It please the ordinary meaning that is understood of one of ordinary skill in the art.
In the description of the present application, it is to be understood that term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom" "inner", "outside", " up time The orientation or positional relationship of the instructions such as needle ", " counterclockwise ", " axial direction ", " radial direction ", " circumferential direction " be orientation based on the figure or Positional relationship is merely for convenience of description the application and simplifies description, rather than the device or element of indication or suggestion meaning must There must be specific orientation, be constructed and operated in a specific orientation, therefore should not be understood as the limitation to the application.
In addition, term " first ", " second " etc. are used for description purposes only, it is not understood to indicate or imply relatively important Property or implicitly indicate the quantity of indicated technical characteristic.In the description of the present application, the meaning of " plurality " is two or more, Unless otherwise specifically defined.
In this application unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc. Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integral；It can be mechanical connect It connects, is also possible to be electrically connected；It can be directly connected, can also can be in two elements indirectly connected through an intermediary The interaction relationship of the connection in portion or two elements.It for the ordinary skill in the art, can be according to specific feelings Condition understands the concrete meaning of above-mentioned term in this application.
In this application unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists Second feature " on ", " top " and " above " but fisrt feature be directly above or diagonally above the second feature, or be merely representative of First feature horizontal height is higher than second feature.Fisrt feature can be under the second feature " below ", " below " and " below " One feature is directly under or diagonally below the second feature, or is merely representative of first feature horizontal height less than second feature.
The preferable specific embodiment of the above, only the application, but the protection scope of the application is not limited thereto, Within the technical scope of the present application, any changes or substitutions that can be easily thought of by anyone skilled in the art, Should all it cover within the scope of protection of this application.Therefore, the protection scope of the application should be with scope of protection of the claims Subject to.

Claims (10)

1. a kind of activating agent for hydrogen storage material, the chemical general formula of the activating agent are as follows: MxNy, wherein x and y respectively indicate M With the atomicity of N, 0 < x≤90,0 < y≤80, x+y=100, M Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt And one or more of one or more of Ru, N Li, Pd, Nb, La, Ce, Nd, Sm and Y.
2. being used for the activating agent of hydrogen storage material as described in claim 1, which is characterized in that the activating agent are as follows: Al20La80、 Al75Fe5Li20、Sn70Pt20Nd10、Fe15Co15Y70、Ni75Ru10Y15、Sn75Mg10Nd10Sm5、Ti22Fe22Nb56、(FeV80)60Ce40、Ag25Pd75And Ti22Cr40Mn4Nb34One or more of.
3. a kind of preparation method of the activating agent for hydrogen storage material, the preparation method include:
It S1 is) M according to chemical general formulaxNyConfiguring the raw material of activating agent, wherein x and y respectively indicates the atomicity of M and N, 0 < x≤ One of 90,0 < y≤80, x+y=100, M Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ag, Sn, Mg, Pt and Ru or several Kind, one or more of N Li, Pd, Nb, La, Ce, Nd, Sm and Y；
S2) under vacuum or inert gas environment, activating agent described in melting is to be made as cast condition activating agent；
S3) under vacuum or inert gas environment, the as cast condition activating agent is made annealing treatment to obtain annealing activating agent；
S4 the quick-fried broken processing of hydrogen) is carried out to the annealing activating agent, the activating agent is made.
4. the preparation method of activating agent as claimed in claim 3, which is characterized in that in step S2), the vacuum of vacuum environment Degree is 5 × 10-3The pressure of inert gas is 0.05-0.08MPa in Pa or inert gas environment；And
Method of smelting is electric arc melting, and fusion process turns over the raw material melting 3-5 times；Or method of smelting is that induction is molten It refines, selected crucible is three high graphite crucibles or zirconia ceramic crucible in fusion process.
5. the preparation method of activating agent as claimed in claim 3, which is characterized in that in step S3), the vacuum of vacuum environment Degree is 5 × 10-3Inert gas pressure is 0.05-0.08MPa in Pa or inert gas environment；And
To the as cast condition activating agent in 500 DEG C of -1500 DEG C of annealing 3h-12h.
6. the preparation method of activating agent as claimed in claim 3, which is characterized in that in step S4), be in Hydrogen Vapor Pressure The quick-fried broken processing of hydrogen is carried out to the annealing activating agent under 4MPa.
7. the preparation method of activating agent as claimed in claim 6, which is characterized in that it is quick-fried broken to carry out hydrogen to the annealing activating agent After processing, the annealing activating agent is carried out to vacuumize processing in 30-120 minutes under 100-400 DEG C of environment.
8. the preparation method of activating agent as claimed in claim 7, which is characterized in that the annealing activating agent vacuumize process After carry out pulverization process, to obtain the activating agent of powdered form.
9. the preparation method of activating agent as claimed in claim 8, which is characterized in that the granularity of the activating agent be 19 μm with Under.
10. the preparation method of the activating agent as described in any one of claim 3 to 9, which is characterized in that further include step S5), Wherein, step S5) are as follows: packing processes are carried out to the activating agent, manner of packing use vacuumizes or filling with inert gas is to described Activating agent protection packaging.
CN201910357474.4A 2019-04-29 2019-04-29 A kind of activating agent and preparation method thereof for hydrogen storage material Pending CN110102280A (en)

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CN113546623A (en) * 2021-07-28 2021-10-26 苏州金宏气体股份有限公司 Rare earth composite organic hydrogen storage hydrogen-carrying catalytic active substance, load and application

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CN101642703A (en) * 2009-09-03 2010-02-10 浙江大学 Catalyst of sodium aluminum hydride coordination oxide and preparation method thereof
CN105695775A (en) * 2016-02-26 2016-06-22 华南理工大学 Preparation method and application for yttrium-iron-based alloy material

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CN101642703A (en) * 2009-09-03 2010-02-10 浙江大学 Catalyst of sodium aluminum hydride coordination oxide and preparation method thereof
CN105695775A (en) * 2016-02-26 2016-06-22 华南理工大学 Preparation method and application for yttrium-iron-based alloy material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113546623A (en) * 2021-07-28 2021-10-26 苏州金宏气体股份有限公司 Rare earth composite organic hydrogen storage hydrogen-carrying catalytic active substance, load and application
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