CN116101974A - Aluminum hydride hydrogen storage material doped with polymer and preparation method thereof - Google Patents

Aluminum hydride hydrogen storage material doped with polymer and preparation method thereof Download PDF

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Publication number
CN116101974A
CN116101974A CN202310211385.5A CN202310211385A CN116101974A CN 116101974 A CN116101974 A CN 116101974A CN 202310211385 A CN202310211385 A CN 202310211385A CN 116101974 A CN116101974 A CN 116101974A
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hydrogen storage
storage material
polymer
pmma
aluminum hydride
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陈淑花
张恒
李泳佳
李垚呈
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Henan Hydrogen Source Technology Co ltd
Dalian University
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Henan Hydrogen Source Technology Co ltd
Dalian University
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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
    • C01B3/0005—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
    • C01B3/001—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 characterised by the uptaking medium; Treatment thereof
    • C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • 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
    • Y02E60/32—Hydrogen storage

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)

Abstract

The invention relates to the technical field of hydrogen storage materials, and discloses an aluminum hydride hydrogen storage material doped with polymer and a preparation method thereof, comprising a composite hydrogen storage material, wherein the composite hydrogen storage material consists of light metal hydride and polymer, and the light metal hydride comprises LiH and MgH 2 Or AlH 3 At least one of the polymers comprises at least one of PMMA, ABS or PVP, and the mass ratio of the light metal hydride to the polymer is 1:0.1 to 100 percent, the composite hydrogen storage material is prepared from AlH 3 And PMMA, wherein the composition expression of the composite hydrogen storage material is AlH 3 +x wt.% PMMA, wherein x represents the mass fraction of PMMA in the composite hydrogen storage material, and 1<x<100. Therefore, the preparation method of the aluminum hydride hydrogen storage material of the doped polymer has the advantages of simple process, easy control, good controllability, lower additive cost, and high-pressure pressing of the ball-milled materialThe space utilization rate can be effectively increased by forming the material into a wafer shape.

Description

Aluminum hydride hydrogen storage material doped with polymer and preparation method thereof
Technical Field
The invention relates to the technical field of hydrogen storage materials, in particular to an aluminum hydride hydrogen storage material doped with a polymer and a preparation method thereof.
Background
The hydrogen energy is a novel clean energy which is rapidly developed in twenty-first century, and is widely focused in countries around the world, is a secondary energy which is clean and environment-friendly, has large energy density and flexible and various in utilization form, and can be used as an effective carrier of large-scale renewable energy. However, the large-scale utilization of hydrogen energy is still subject to a plurality of restrictions, wherein the high-density safe storage of hydrogen is one of bottleneck technologies for restricting the utilization of hydrogen energy. The prior hydrogen storage technology has three mature modes, namely high-pressure gaseous hydrogen storage, low-temperature liquid hydrogen storage and solid hydrogen storage, and the hydrogen storage material has the advantages of large volume hydrogen storage density, high safety, convenient transportation, easy operation and the like, and is a hydrogen storage mode with great application prospect in the future. Currently, solid hydrogen storage materials of relatively wide application include LiBH 4 、LiAlH 4 、LiNH 2 、AlH 3 And hydride hydrogen storage materials, liquid materials comprise inorganic ammonia, organic hydrazine, hydrocarbon, carboxylic acid or alcohols, etc.
AlH 3 Is a potential high-performance hydrogen storage material, and brings importance to scientific researchers in the field of hydrogen storage. AlH (AlH) 3 The thermal decomposition temperature of (C) is 150-200 ℃, and the modified hydrogen release temperature can be further reduced. In recent years, with the rise of the research fields of hydrogen energy and fuel cells, aluminum hydride has also received more and more attention. AlH (AlH) 3 Has high weight and volume hydrogen density of 10.1wt.% and 0.148kg H respectively 2 L is twice the liquid hydrogen density.
PMMA has good performance in improving the air stability of the hydrogen storage material. At present, researches show that a composite material formed by ball milling and mixing PMMA and metal hydride has good air stability, and in the aspect of hydrogen release, the initial hydrogen release temperature of the hydrogen storage composite material is obviously reduced, and the hydrogen release rate is obviously increased, so that AlH 3 PMMA composite material at initial hydrogen release temperature, hydrogen release rate andthere is some improvement in air stability.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides the aluminum hydride hydrogen storage material of the doped polymer and the preparation method thereof.
(II) technical scheme
In order to achieve the purpose of the aluminum hydride hydrogen storage material doped with the polymer, the invention provides the following technical scheme: the invention provides an aluminum hydride hydrogen storage material doped with polymer, which comprises a composite hydrogen storage material, wherein the composite hydrogen storage material consists of light metal hydride and polymer, and the light metal hydride comprises LiH and MgH 2 Or AlH 3 At least one of the polymers comprises at least one of PMMA, ABS or PVP.
Preferably, the mass ratio of the light metal hydride to the polymer is 1:0.1 to 100.
Preferably, the composite hydrogen storage material is made of AlH 3 And PMMA, wherein the composition expression of the composite hydrogen storage material is AlH 3 +x wt.% PMMA, wherein x represents the mass fraction of PMMA in the composite hydrogen storage material, and 1<x<100。
Preferably, the value of x is 7.5.
Preferably, the preparation method comprises the following steps:
s1, under the atmosphere of inert gas, placing metal hydride and polymer into a ball mill according to a certain proportion for mechanical ball milling, and obtaining a powdery composite material after ball milling;
s2, performing high-pressure curing treatment on the ball-milled composite material powder.
Preferably, the rotation speed of the ball mill is 100-500 rpm.
Preferably, the ball milling time is 0.1 to 100 hours.
Preferably, the inert gas comprises one or more of nitrogen, argon, hydrogen or helium.
Preferably, the ball-to-material ratio in the ball milling process is 10-100: 1.
preferably, the curing pressure of the high-pressure curing treatment is 1-100 MPa, and the diameter of the pressed sheet of the high-pressure curing treatment is 1-100 mm.
(III) beneficial effects
Compared with the prior art, the invention provides the rare earth oxide doped aluminum hydride hydrogen storage material and the preparation method thereof, and the aluminum hydride hydrogen storage material has the following beneficial effects:
since the hydrogen storage material is in AlH 3 Middle doped polymer PMMA which can be coated on AlH 3 Around the particle, H-O bond of PMMA and AlH 3 The H of the polymer is formed into a chemical effect, so that the aluminum hydride hydrogen storage material modified by the method has a unique catalytic effect, the initial hydrogen release temperature is obviously reduced, the temperature can be reduced to 110 ℃ from 140 ℃, the air stability is obviously enhanced, meanwhile, the adopted polymer PMMA is low in cost and easy to obtain, the additive is added by adopting a mechanical ball milling method, so that the additive is simple in adding process and suitable for industrial mass production, in addition, the material is pressed into a round plate shape by using the ball-milled material through high pressure, and the space utilization rate can be effectively increased.
Drawings
FIG. 1 is an X-ray diffraction diagram of a sample before releasing hydrogen of a composite hydrogen storage material prepared according to an embodiment of the present invention;
FIG. 2 shows the prepared composite hydrogen storage material and the original AlH 3 A graph of hydrogen release amount versus time measured by constant temperature hydrogen release test at 100 ℃ of the sample;
FIG. 3 is a graph of hydrogen evolution versus time measured at a constant temperature of 140℃for the prepared pellet composite.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention firstly provides an aluminum hydride hydrogen storage material doped with polymer, which comprises a composite hydrogen storage material, wherein the composite hydrogen storage material consists of light metal hydride and polymer, and the light metal hydride comprises LiH and MgH 2 Or AlH 3 At least one of the polymers comprises at least one of PMMA, ABS or PVP.
Further, the mass ratio of the light metal hydride to the polymer is 1:0.1 to 100.
Further, the composite hydrogen storage material is made of AlH 3 And PMMA, wherein the composition expression of the composite hydrogen storage material is AlH 3 +x wt.％PMMA。
Further, the mass ratio of the light metal hydride to the polymer is 1:0.1-100, wherein x represents the mass percentage of PMMA in the composite hydrogen storage material and is 1< x <100, the value range of x is 1-80, and the value of x is 7.5.
Further, the preparation method comprises the following steps:
s1, under the atmosphere of inert gas, placing metal hydride and polymer into a ball mill according to a certain proportion for mechanical ball milling, and obtaining a powdery composite material after ball milling;
s2, performing high-pressure curing treatment on the ball-milled composite material powder.
And under inert gas atmosphere, placing the metal hydride and the polymer into a ball mill according to a certain proportion for mechanical ball milling, obtaining the PMMA-doped aluminum hydride composite hydrogen storage material after ball milling, performing high-pressure curing treatment on the obtained composite hydrogen storage material, and pressing the obtained material into a round plate shape under high pressure.
Further, the rotational speed of the mechanical ball mill is preferably 100 to 500rpm, more preferably 200 to 400rpm.
Further, the time of the mechanical ball milling is preferably 0.1 to 100 hours, more preferably 1 to 3 hours.
Further, the inert gas in the mechanical ball milling is preferably one or more of argon, hydrogen, nitrogen or helium, and the inert gas is used for ensuring AlH 3 The (aluminum hydride) and PMMA (polymethyl methacrylate) are subjected to an inert atmosphere during the ball milling, and the kind of the inert gas is not limited herein.
Further, the ball-to-material ratio of the mechanical ball mill is preferably 10-100: 1, more preferably 40-60:1, it should be noted that the person skilled in the art can set the ball milling speed, the ball milling time and the ball milling ball material ratio according to the actual requirements, and the invention is not limited herein.
Further, the pressure required for the high-pressure cured material is preferably 1 to 100MPa, more preferably 1 to 10MPa, and the diameter of the pressed sheet of the high-pressure cured material is preferably 1 to 100mm.
Hereinafter, an aluminum hydride hydrogen storage material doped with a polymer and a method for preparing the same according to the present invention will be described in detail by way of specific examples.
Embodiment one: alH is treated in nitrogen atmosphere 3 AlH with PMMA according to the formula 3 And (2) weighing 9.75g and 0.25g of PMMA (polymethyl methacrylate) in a proportion of +2.5wt.% respectively, uniformly mixing in a nitrogen atmosphere, wherein the total mass is 10g, loading a uniformly mixed sample into a ball mill, adding steel balls (300 g of total mass) into the ball mill according to a ball-to-material ratio of 30:1, loading the ball mill into a 100mL ball mill, setting a ball milling rotating speed of 350rpm, performing mechanical ball milling for 2 hours, taking out the ball mill after the ball milling process is finished, opening a tank in the nitrogen atmosphere, and collecting a composite hydrogen storage material product.
Embodiment two: alH is treated in nitrogen atmosphere 3 AlH with PMMA according to formula 3 The mixture ratio of +5wt.% PMMA is respectively weighed 9.50g and 0g50g, uniformly mixing in a nitrogen atmosphere, wherein the total mass is 10g, loading a uniformly mixed sample into a ball mill, adding steel balls (total mass is 300 g) into the ball mill according to the ratio of ball-to-material ratio of 30:1, then loading the ball mill into a 100mL ball mill, setting the ball milling rotation speed to 350rpm, performing mechanical ball milling for 2 hours, taking out the ball mill after the ball milling process is finished, opening a tank in the nitrogen atmosphere, and collecting a composite hydrogen storage material product.
Embodiment III: alH is treated in nitrogen atmosphere 3 AlH with PMMA according to formula 3 And (2) respectively weighing 9.25g and 0.75g of PMMA (polymethyl methacrylate) in a proportion of +7.5wt.%, uniformly mixing in a nitrogen atmosphere, wherein the total mass is 10g, loading a uniformly mixed sample into a ball mill, adding steel balls (300 g) into the ball mill according to a ball-to-material ratio of 30:1, loading the ball mill into a 100mL ball mill, setting a ball milling rotating speed of 350rpm, performing mechanical ball milling for 2 hours, taking out the ball mill after the ball milling process is finished, opening a tank in the nitrogen atmosphere, and collecting a composite hydrogen storage material product.
Experimental example four: alH is treated in nitrogen atmosphere 3 AlH with PMMA according to formula 3 And (2) respectively weighing 9.0g and 1.0g of PMMA (polymethyl methacrylate) in a proportion of +10wt.%, uniformly mixing in a nitrogen atmosphere, wherein the total mass is 10g, loading a uniformly mixed sample into a ball mill, adding steel balls (300 g) into the ball mill according to a ball-to-material ratio of 30:1, loading the ball mill into a 100mL ball mill, setting the ball mill rotation speed to 350rpm, performing mechanical ball milling for 2 hours, taking out the ball mill after the ball milling process is finished, opening a tank in the nitrogen atmosphere, and collecting a composite hydrogen storage material product.
Judgment standard: in order to evaluate the hydrogen storage performance of the prepared composite hydrogen storage material, the ball-milled product is subjected to constant temperature hydrogen release test at 100 ℃ and the corresponding hydrogen release amount is calibrated, the constant temperature hydrogen release test result at 100 ℃ is shown in figure 2, and the result shows that PMMA (polymethyl methacrylate) remarkably improves alpha-AlH 3 In addition, the modified composite material shows faster kinetics with increasing dehydrogenation temperature, the total hydrogen evolved from the composite material at 100 ℃ for 30min is 3.5%, the total hydrogen evolved at 100min is 5%, and untreated AlH 3 100 as receivedmin hydrogen release is 0.5%, XRD image measured before hydrogen release is shown in figure 1, generation of alumina in the material can be effectively reduced by increasing mass proportion of polymer PMMA, on the one hand, hydrogen release efficiency of the composite material is improved, and positive peach shape in figure 1 represents AlH 3 Is inverted peach-shaped to represent Al 2 O 3 Is a curve of (2).
It can be found from fig. 1 that adding 10% PMMA can effectively prevent the composite material from being oxidized or hydrolyzed by oxygen and water vapor in the air, and because the generation of alumina can form a firm oxide layer on the surface of aluminum hydride particles, when starting to release hydrogen, hydrogen is difficult to break through the external oxide layer, so that the generation of alumina can be avoided to effectively increase the hydrogen release efficiency of the composite material.
Composite hydrogen storage material according to fig. 2 with original AlH 3 The hydrogen desorption amount-time curve measured by the constant temperature hydrogen desorption test at 100 ℃ of the sample is shown as a diamond in FIG. 2, which shows Pure alpha-AlH 3 Is a circle representing As-filled alpha-AlH 3 The curve is shown in the figure, the inverted triangle shows the curve of 2.5% by mass of PMMA, the heart-shaped curve shows the curve of 5% by mass of PMMA, the pentagram shows the curve of 7.5% by mass of PMMA, the regular triangle shows the curve of 10% by mass of PMMA, and AlH with the best hydrogen release performance is obtained 3 And (3) carrying out high-pressure curing treatment on +7.5wt.% PMMA component, weighing 9.6g of composite material and 0.4g of Al powder in a nitrogen atmosphere, mixing in a ball mill, adding steel balls (total mass 300 g) into the ball mill according to the ratio of 30:1, sealing the ball mill in the nitrogen atmosphere, placing the sealed ball mill in a planetary ball mill for mechanical ball milling, wherein the rotating speed of the ball mill is 350rpm, the ball milling time is 2h, taking out the ball mill after the ball milling process is finished, opening a tank in the nitrogen atmosphere, carrying out compression molding by adopting the pressure of 4MPa, and waiting for a hydrogen discharge test.
In order to evaluate the hydrogen release capacity of the prepared tabletting materials, the constant temperature hydrogen release condition of the tabletting materials at 140 ℃ is tested, as shown in fig. 3, the diamond shape in fig. 3 shows a curve when no Al is added, the circle shows a curve when 2% of Al is added, the inverted triangle shows a curve when 4% of Al is added, the pentagram shows a curve when 6% of Al is added, the regular triangle shows a curve when 8% of Al is added, the tabletting hydrogen release test is carried out by adding each proportion of Al in the graph, compared with the material without adding Al powder, the non-light hydrogen release amount of the tabletting materials with the added Al powder is increased, the hydrogen release rate is also increased, and the hydrogen release amount of the tabletting materials with the added Al powder can be increased by 2.1%, so that the hydrogen release amount of the tabletting materials can be obviously improved by adding the Al powder with different proportions, meanwhile, the PMMA material can be effectively slowed down by the speed of air oxidation and hydrolysis, and the formed tabletting hydrogen release amount of the Al powder can be increased in the prepared material.
The beneficial effects of the invention are as follows:
since the hydrogen storage material is in AlH 3 Middle doped polymer PMMA which can be coated on AlH 3 Around the particle, H-O bond of PMMA and AlH 3 The H of the aluminum hydride hydrogen storage material modified by the method has a unique effect in catalysis, the initial hydrogen release temperature of the aluminum hydride hydrogen storage material is obviously reduced, the temperature can be reduced to 110 ℃ from 140 ℃, the air stability is obviously enhanced, meanwhile, the adopted polymer PMMA is low in cost and easy to obtain, the adding process is simple by adopting a mechanical ball milling method for adding the additive, and the aluminum hydride hydrogen storage material is suitable for industrial mass production. Therefore, the preparation method of the aluminum hydride hydrogen storage material of the doped polymer has the advantages of simple process, easy control, good controllability, lower additive cost, and the material after ball milling is pressed into a round sheet shape by high pressure, so that the space utilization rate can be effectively increased.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. Hydrogenation of doped polymersThe aluminum hydrogen storage material and the preparation method thereof are characterized by comprising a composite hydrogen storage material, wherein the composite hydrogen storage material consists of light metal hydride and polymer, and the light metal hydride comprises LiH and MgH 2 Or AlH 3 At least one of the polymers comprises at least one of PMMA, ABS or PVP.
2. The aluminum hydride hydrogen storage material of doped polymer and its preparation method as claimed in claim 1, wherein the mass ratio of the light metal hydride to the polymer is 1:0.1 to 100.
3. The aluminum hydride hydrogen storage material doped with polymer and the preparation method thereof as claimed in claim 2, wherein the composite hydrogen storage material is prepared from AlH 3 And PMMA, wherein the composition expression of the composite hydrogen storage material is AlH 3 +x wt.% PMMA, wherein x represents the mass fraction of PMMA in the composite hydrogen storage material, and 1<x<100。
4. The aluminum hydride hydrogen storage material of doped polymer and method of making same as claimed in claim 3, wherein x has a value of 7.5.
5. The aluminum hydride hydrogen storage material of doped polymer and method of making same as claimed in claim 4, wherein said method of making comprises the steps of:
s1, under the atmosphere of inert gas, placing metal hydride and polymer into a ball mill according to a certain proportion for mechanical ball milling, and obtaining a powdery composite material after ball milling;
s2, performing high-pressure curing treatment on the ball-milled composite material powder.
6. The aluminum hydride hydrogen storage material doped with polymer and the preparation method thereof according to claim 5, wherein the rotation speed of the ball mill is 100-500 rpm.
7. The aluminum hydride hydrogen storage material of doped polymer and its preparation method as claimed in claim 6, wherein the ball milling time is 0.1-100 h.
8. The aluminum hydride hydrogen storage material of a doped polymer and method of making same of claim 7, wherein said inert gas comprises one or more of nitrogen, argon, hydrogen or helium.
9. The aluminum hydride hydrogen storage material doped with polymer and the preparation method thereof according to claim 8, wherein the ball-material ratio in the ball milling process is 10-100: 1.
10. the aluminum hydride hydrogen storage material of doped polymer and the preparation method thereof according to claim 9, wherein the curing pressure of the high-pressure curing treatment is 1-100 MPa, and the diameter of the pressed sheet of the high-pressure curing treatment is 1-100 mm.
CN202310211385.5A 2023-03-07 2023-03-07 Aluminum hydride hydrogen storage material doped with polymer and preparation method thereof Pending CN116101974A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117583594A (en) * 2023-11-20 2024-02-23 南京工程学院 Waste aluminum alloy modified hydrolysis hydrogen production composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117583594A (en) * 2023-11-20 2024-02-23 南京工程学院 Waste aluminum alloy modified hydrolysis hydrogen production composite material and preparation method thereof
CN117583594B (en) * 2023-11-20 2024-04-26 南京工程学院 Waste aluminum alloy modified hydrolysis hydrogen production composite material and preparation method thereof

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