CN112265958B - Composite hydrogen storage material and preparation method thereof - Google Patents
Composite hydrogen storage material and preparation method thereof Download PDFInfo
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- CN112265958B CN112265958B CN202011178204.6A CN202011178204A CN112265958B CN 112265958 B CN112265958 B CN 112265958B CN 202011178204 A CN202011178204 A CN 202011178204A CN 112265958 B CN112265958 B CN 112265958B
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- 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
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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
- Y02E60/32—Hydrogen storage
Abstract
The invention discloses a composite hydrogen storage material and a preparation method thereof, belonging to the field of hydrogen storage materials. The composite hydrogen storage material comprises magnesium amide, lithium hydride and alkali metal silicon hydride, wherein the molar ratio of the magnesium amide to the lithium hydride is 1:2, and the addition amount of the alkali metal silicon hydride is 1-15 mol%. When the composite hydrogen storage material is applied, magnesium amide, lithium hydride and alkali metal silicon hydride react under the heating condition, and alkali metal (such as K, Rb, Cs) and silicon atoms diffuse into amino compounds, so that the breakage of N-H bonds in the amino compounds is promoted, and the thermodynamic and kinetic properties of the hydrogen absorption and desorption reaction are improved. In the hydrogen absorption and desorption circulation process, the alloy formed by alkali metals (K, Rb, Cs) and silicon is continuously pulverized in the hydrogen absorption and dehydrogenation process, so that the alloy can be uniformly dispersed in a Li-Mg-N-H system, and the excellent circulation stability of the material is ensured. Therefore, the composite hydrogen storage material provided by the application has low hydrogen absorption and desorption temperature and extremely excellent low-temperature cyclic hydrogen absorption and desorption performance.
Description
Technical Field
The invention belongs to the technical field of solid hydrogen storage, and particularly relates to a composite hydrogen storage material and a preparation method thereof.
Background
Energy is the basis on which human beings rely for survival and also is important motivation support for the rapid development of modern civilization. However, with the continuous expansion of population and the continuous improvement of living standard of people, people have an increasing demand for energy, and the problem of environmental pollution caused by the massive use of traditional fossil fuels and the problem of energy exhaustion caused by non-renewability of the traditional fossil fuels compel us to find clean renewable energy. Hydrogen energy has received wide attention all over the world with its advantages of wide sources, efficient cleaning, high energy density, etc. Hydrogen storage technology is an important bottleneck in the large-scale application of hydrogen energy at present. Among various hydrogen storage modes, solid-state hydrogen storage has high safety and hydrogen charging and discharging speedFast speed, low comprehensive cost and the like. Among the solid-state hydrogen storage materials that have been developed, magnesium amide/lithium hydride (Mg (NH)2)2-2LiH) system has a reversible hydrogen storage capacity of about 5.6 wt% and relatively suitable thermodynamic properties, and is currently one of the most promising hydrogen storage materials for large-scale on-board applications. However, the magnesium amide/lithium hydride system has a high kinetic barrier, the material needs to have a good hydrogen evolution kinetic performance at a temperature above 180 ℃, and the product after hydrogen evolution can be completely hydrogenated at a temperature above 200 [ Journal of Alloys ]&Compounds,2005,398(1-2):235-239]。
Therefore, many scholars improve the kinetics and thermodynamics of hydrogen absorption and desorption reactions by various means to lower the hydrogen absorption and desorption temperature and improve the cycle stability. The hydrogen storage performance of an amino magnesium/lithium hydride system can be obviously improved by reducing the particle size, but the particles of the material have the tendency of agglomeration and growth in the hydrogen absorption and desorption process of circulation, so that the hydrogen absorption and desorption performance can be gradually weakened in the circulation process. By catalytic modification, e.g. by addition of "Li2MgN2H2Although the hydrogen storage performance of the system is improved to some extent by the seed crystals, the carbon-based material, the transition metal and the compound thereof, etc. [ Acta Physico-Chimica Sinica,2015,31(4):627-635 ]]. Adding LiBH4And KH, but the first hydrogen absorption and desorption temperature can be significantly reduced, but the hydrogen absorption and desorption amount of the material is significantly reduced in the process of circulating hydrogen absorption and desorption due to the deterioration of the particle size, the grain size, the dispersion degree of the catalyst, and the like of the material in the circulating process. However, for hydrogen storage materials of the magnesium amide/lithium hydride system for large-scale application, good cycle performance is one of the most important indicators. Therefore, the development of the composite hydrogen storage material with low hydrogen absorption and desorption temperature and good cycle stability is significant.
Disclosure of Invention
The invention provides a composite hydrogen storage material and a preparation method thereof, aiming at the defects of the existing magnesium amide/lithium hydride system hydrogen storage technology.
In order to achieve the purpose, the invention adopts a technical scheme that:
there is provided a composite hydrogen storage material comprising: magnesium amide, lithium hydride and alkali metal silicon hydride; wherein the molar ratio of the magnesium amide to the lithium hydride is 1:2, and the addition amount of the alkali metal silicon hydride is 1-15 mol%.
Wherein the alkali metal silicon hydride comprises potassium silicon hydride KSiH3Rubidium hydrosilation RbSiH3And cesium hydrosilate CsSiH3At least one of them.
In order to achieve the purpose, the invention adopts another technical scheme that:
a preparation method of a composite hydrogen storage material is provided, which comprises the following steps:
weighing magnesium amide, lithium hydride and alkali metal silicon hydride, mixing and putting into a ball milling tank, wherein the molar ratio of the magnesium amide to the lithium hydride is 1:2, and the addition amount of the alkali metal silicon hydride is 1-15 mol%;
vacuumizing the ball milling tank and filling hydrogen pressure;
and putting the ball milling tank into a ball mill for ball milling.
Wherein the alkali metal silicon hydride comprises potassium silicon hydride KSiH3Rubidium hydrosilation RbSiH3And cesium hydrosilate CsSiH3At least one of them.
Wherein the hydrogen pressure is 2-5 MPa.
Wherein, before the step of filling the ball-milling tank with hydrogen pressure after vacuumizing, the method further comprises the following steps: and adding mill materials into a ball milling tank, wherein the mass ratio of the mill materials to the mixture of the magnesium amide, the lithium hydride and the alkali metal silicon hydride is 40-120: 1.
The grinding object comprises steel balls, the diameters of the steel balls are 12mm, 10mm and 7mm, the number of the steel balls with the diameters of 12mm is 4, the number of the steel balls with the diameters of 10mm is 6, and the number of the steel balls with the diameters of 7mm is 18.
Wherein, the ball milling tank comprises a steel tank, and the volume is 180 mL.
When the ball mill performs ball milling, the ball milling rotating speed is 300-500 rpm, the ball milling time is 12-36 h, and the operation mode is clockwise and anticlockwise alternation.
Wherein, the ball mill is a planetary ball mill.
The invention has the following effective effects: in contrast to the prior art, the present invention provides a composite hydrogen storage material comprising magnesium amide, lithium hydride and alkali metal silicon hydride, that is, the present application combines alkali metal silicon hydride with magnesium amide and lithium hydride to form a multi-element reaction destabilizing system. Therefore, the invention can adopt a preset preparation method to refine the particle size of the material in the multicomponent reaction destabilizing system and increase the surface defects, thereby shortening the hydrogen diffusion distance and improving the hydrogen absorption and desorption reaction activity of the composite hydrogen storage material. Further, when the composite hydrogen storage material is applied to hydrogen absorption and desorption, magnesium amide, lithium hydride and alkali metal silicon hydride are reacted under the heating condition, wherein alkali metals (such as K, Rb, Cs) and silicon atoms are diffused into amino compounds, the breakage of N-H bonds in the amino compounds is promoted, and thus the thermodynamic and kinetic properties of the hydrogen absorption and desorption reaction are improved. In the hydrogen absorption and desorption circulation process, the alloy formed by alkali metal (such as K, Rb, Cs) and silicon is continuously pulverized in the hydrogen absorption and dehydrogenation process, so that the alloy can be uniformly dispersed in a Li-Mg-N-H system, and the excellent circulation stability of the material is ensured. Therefore, the composite hydrogen storage material provided by the application has low hydrogen absorption and desorption temperature and extremely excellent low-temperature circulating hydrogen absorption and desorption performance, and the application improves the hydrogen storage performance of the original system by utilizing the alkali metal silicon hydride, and has lower cost.
Drawings
FIG. 1 shows Mg (NH) in example 12)2-2LiH-0.05KSiH3And Mg (NH)2)2-hydrogen evolution with temperature curve of 2LiH material.
FIG. 2 shows Mg (NH) in example 12)2-2LiH-0.05KSiH3And Mg (NH)2)2-2LiH、Mg(NH2)2Graph of hydrogen storage capacity of-2 LiH-0.05KH material for 10 cycles of hydrogen absorption and desorption.
FIG. 3 shows Mg (NH) in example 22)2-2LiH-0.08RbSiH3And Mg (NH)2)2-hydrogen sorption curve with temperature of 2LiH material.
FIG. 4 shows Mg (NH) in example 32)2-2LiH-0.03CsSiH3Hydrogen evolution with temperature curve (d).
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments that can be obtained by a person skilled in the art without making any inventive step based on the embodiments in the present application belong to the protection scope of the present application.
A composite hydrogen storage material includes magnesium amide, lithium hydride, and alkali metal silicon hydride. Wherein the molar ratio of magnesium amide to lithium hydride is 1:2, and the amount of the alkali metal silicon hydride added is 1 to 15 mol%, for example, 1 mol%, 5 mol%, 10 mol%, 15 mol%, or the like. Preferably, the alkali metal silicon hydride comprises potassium silicon hydride KSiH3Rubidium hydrosilation RbSiH3And cesium hydrosilate CsSiH3At least one of them.
The composite hydrogen storage material provided by the invention comprises magnesium amide, lithium hydride and alkali metal silicon hydride, namely, the alkali metal silicon hydride, the magnesium amide and the lithium hydride are compounded to form a multi-component reaction destabilizing system. Therefore, the invention can adopt a preset preparation method to refine the particle size of the material in the multicomponent reaction destabilizing system and increase the surface defects, thereby shortening the hydrogen diffusion distance and improving the hydrogen absorption and desorption reaction activity of the composite hydrogen storage material. Further, when the composite hydrogen storage material is applied to hydrogen absorption and desorption, magnesium amide, lithium hydride and alkali metal silicon hydride are reacted under the heating condition, wherein alkali metals (such as K, Rb, Cs) and silicon atoms are diffused into amino compounds, the breakage of N-H bonds in the amino compounds is promoted, and thus the thermodynamic and kinetic properties of the hydrogen absorption and desorption reaction are improved. In the hydrogen absorption and desorption circulation process, the alloy formed by alkali metal (such as K, Rb, Cs) and silicon is continuously pulverized in the hydrogen absorption and dehydrogenation process, so that the alloy can be uniformly dispersed in a Li-Mg-N-H system, and the excellent circulation stability of the material is ensured. Therefore, the composite hydrogen storage material provided by the application has low hydrogen absorption and desorption temperature and extremely excellent low-temperature circulating hydrogen absorption and desorption performance, and the application improves the hydrogen storage performance of the original system by utilizing the alkali metal silicon hydride, and has lower cost.
In addition, the application also provides a preparation method of the composite hydrogen storage material, which comprises the following steps.
Step one, weighing magnesium amide, lithium hydride and alkali metal silicon hydride, mixing and putting into a ball milling tank. Wherein the molar ratio of magnesium amide to lithium hydride is 1:2, and the amount of the alkali metal silicon hydride added is 1 to 15 mol%, for example, 1 mol%, 4 mol%, 9 mol%, 15 mol%, or the like.
Preferably, the alkali metal silicon hydride comprises potassium silicon hydride KSiH3Rubidium hydrosilation RbSiH3And cesium hydrosilate CsSiH3At least one of them.
And step two, vacuumizing the ball milling tank and filling hydrogen pressure.
Preferably, the hydrogen pressure is 2 to 5MPa, such as 2MPa, 3MPa, 5MPa, and the like.
Wherein, before the step of filling hydrogen pressure after vacuumizing the ball-milling tank, the method also comprises the following steps:
adding the mill base into a ball milling tank, wherein the mass ratio of the mill base to the mixture of the magnesium amide, the lithium hydride and the alkali metal silicon hydride is 40-120: 1, such as 40:1, 60:1, 80:1, 100:1, 120:1 and the like.
Preferably, the mill pot comprises a steel pot having a volume of 180 mL. Of course, in other embodiments, other volumes of milling pots may be selected depending on the amounts of mill material and mixture described above.
The steel balls with different diameters are selected to be mixed as the grinding object, the diameters of the steel balls can be adjusted according to actual requirements, and the quantity of each type of steel balls can also be specifically adjusted. Preferably, the steel balls have diameters of 12mm, 10mm and 7mm, wherein the number of steel balls having a diameter of 12mm is 4, the number of steel balls having a diameter of 10mm is 6, and the number of steel balls having a diameter of 7mm is 18.
And step three, putting the ball milling tank into a ball mill for ball milling.
After the mixture of the ground material and the magnesium amide, the lithium hydride and the alkali metal silicon hydride is put into a ball milling tank, the ball milling tank is vacuumized and then filled with hydrogen pressure, the ball milling tank can be put into a ball mill for ball milling.
The parameters of the ball milling process can be adjusted according to actual requirements, preferably, the ball mill is a planetary ball mill, when the ball mill performs ball milling, the ball milling rotation speed is 300-500 rpm, such as 300rpm, 400rpm, 500rpm, and the like, the ball milling time is 12-36 h, such as 12h, 24h, 36h, and the like, and the operation mode is clockwise and counterclockwise alternating.
The preparation method of the composite hydrogen storage material is simple and safe, has wide application prospect, improves the hydrogen storage performance of the original system by utilizing the alkali metal silicon hydride, and has lower cost. Furthermore, the composite hydrogen storage material prepared by the preparation method has low hydrogen absorption and desorption temperature and extremely excellent low-temperature circulating hydrogen absorption and desorption performance.
The preparation process and performance characterization of the composite hydrogen storage material of the present application are described below with reference to specific examples.
Example 1
The samples were weighed in a glove box under argon atmosphere, and the magnesium amide (Mg (NH)2)2) And the molar ratio of lithium hydride (LiH) is 1:2, potassium hydrosilicide (KSiH)3) The amount of powder added was 5 mol%. Then putting the powder into a ball milling tank, adding milling materials (the ball-material ratio is 50: 1), vacuumizing the ball milling tank, filling hydrogen pressure of 5MPa, performing ball milling treatment by adopting a planetary ball mill (the rotating speed is 500rpm, the ball milling time is 24h, and the ball milling tank alternately runs clockwise and anticlockwise), and taking out hydrogen storage material powder in a glove box after ball milling is finished to obtain Mg (NH)2)2-2LiH-0.05KSiH3A composite hydrogen storage material. Under the same conditions, Mg (NH) can be prepared respectively2)2-2LiH and Mg (NH)2)2-2LiH-0.05KH of material as control group. For Mg (NH)2)2-2LiH-0.05KSiH3And Mg (NH)2)2Two samples of-2 LiH were subjected to a hydrogen evolution with temperature test, as can be seen from FIG. 1, Mg (NH)2)2The initial hydrogen evolution temperature of the-2 LiH material is about 130 ℃ and the hydrogen evolution is only 0.66 wt% when the temperature is raised to 170 ℃. In comparison, Mg (NH)2)2-2LiH-0.05KSiH3The initial hydrogen release temperature of the composite hydrogen storage material is reduced to about 80 ℃, the hydrogen release amount reaches 4 wt% when the temperature is increased to 170 ℃, and the final total hydrogen release amount is as much as 5.1 wt%. Apparently, Mg (NH)2)2-2LiH-0.05KSiH3Hydrogen desorption performance ratio Mg (NH) of composite hydrogen storage material2)2-2LiH is much better.
FIG. 2 shows Mg (NH)2)2-2LiH-0.05KSiH3And Mg (NH)2)2-2LiH、Mg(NH2)2A hydrogen storage capacity chart of hydrogen absorption and desorption of three materials of-2 LiH-0.05KH for 10 times of circulation (the circulation condition is that hydrogen is desorbed at 170 ℃ and hydrogen is absorbed at 150 ℃, and the temperature is kept for 2 h). From the figure, Mg (NH) is known2)2The capacity of the 2LiH is greatly reduced from the second hydrogen discharge, and the capacity retention rate of 10 cycles is only 57.7%; mg (NH) for better performance reported before2)2The capacity retention of the-2 LiH-0.05KH material after 10 cycles is only 77.7%. And for Mg (NH) in the present invention2)2-2LiH-0.05KSiH3The first hydrogen discharge capacity of the composite hydrogen storage material is 4.79 wt%, the tenth hydrogen discharge capacity is 4.7 wt%, and the capacity retention rate of 10 cycles is as high as 98.1%. Thus, Mg (NH)2)2-2LiH-0.05KSiH3The composite hydrogen storage material has extremely good circulation stability at a lower temperature.
Example 2
The samples were weighed in a glove box under argon atmosphere, and the magnesium amide (Mg (NH)2)2) And the molar ratio of lithium hydride (LiH) is 1:2, rubidium hydrosilation (RbSiH)3) The amount of powder added was 8 mol%. Then putting the powder into a ball milling tank, simultaneously adding milling materials (the ball material ratio is 60: 1), vacuumizing the ball milling tank, then filling hydrogen pressure of 4MPa, and performing ball milling treatment by a line type star ball mill (the rotating speed is 400rpm, the ball milling time is 12h, clockwise and reversely rotatingHour hand alternate operation), after ball milling is finished, taking out hydrogen storage material powder in a glove box to obtain Mg (NH)2)2-2LiH-0.08RbSiH3A hydrogen storage material; under the same conditions, Mg (NH) can be prepared2)2-2LiH material was used as control group. As can be seen in FIG. 3, Mg (NH)2)2The-2 LiH material starts to absorb hydrogen at about 100 ℃, and can completely absorb hydrogen only during the heat preservation period at 200 ℃. And Mg (NH)2)2-2LiH-0.08RbSiH3The initial hydrogen absorption temperature of the composite hydrogen storage material is only 60 ℃, the hydrogen absorption is basically complete at 150 ℃, and the composite hydrogen storage material shows good hydrogen absorption performance.
Example 3
The samples were weighed in a glove box under argon atmosphere, and the magnesium amide (Mg (NH)2)2) And the molar ratio of lithium hydride (LiH) is 1:2, cesium hydrosilicide (CsSiH)3) The amount of powder added was 3 mol%. Then putting the powder into a ball milling tank, simultaneously adding milling materials (the ball-material ratio is 80: 1), vacuumizing the ball milling tank, then filling hydrogen pressure of 3MPa, performing ball milling treatment by adopting a planetary ball mill (the rotating speed is 300rpm, the ball milling time is 36h, and the ball milling alternately runs clockwise and anticlockwise), and after the ball milling is finished, taking out hydrogen storage material powder in a glove box to obtain Mg (NH)2)2-2LiH-0.03CsSiH3A hydrogen storage material. As can be seen from FIG. 4, Mg (NH)2)2-2LiH-0.03CsSiH3The composite hydrogen storage material begins to release hydrogen at about 80 ℃, the hydrogen release amount at 170 ℃ reaches 3.6 wt%, the total hydrogen release amount is 4.9 wt%, and the hydrogen release performance is excellent.
Examples 4 to 16
Aminomagnesium (Mg (NH) was prepared in the same manner as in examples 1, 2 and 32)2) And the molar ratio of lithium hydride (LiH) is 1:2, only changing the addition of alkali metal silicon hydride and the ball milling preparation condition, the corresponding composite hydrogen storage material can be prepared. Table 1 lists the initial hydrogen desorption temperature, hydrogen storage capacity and capacity retention rate after ten hydrogen absorption and desorption cycles of each corresponding composite hydrogen storage material, wherein the conditions of the hydrogen absorption and desorption cycles are that the temperature is kept at 170 ℃ for 2h for hydrogen desorption and the temperature is kept at 150 ℃ for 2h for hydrogen absorption.
As can be seen from Table 1, magnesium amide (Mg (NH)2)2And lithium hydride (LiH) in a molar ratio of 1:2, adding different molar amounts of potassium hydrosilicide (KSiH)3) Rubidium hydrosilation (RbSiH)3) Cesium hydrosilicide (CsSiH)3) The composite hydrogen storage material prepared under different ball milling conditions has lower hydrogen releasing temperature, higher hydrogen releasing amount and excellent circulation stability.
The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.
Claims (8)
1. A composite hydrogen storage material, comprising:
magnesium amide, lithium hydride and alkali metal silicon hydride;
wherein the molar ratio of the magnesium amide to the lithium hydride is 1:2, and the addition amount of the alkali metal silicon hydride is 1-15 mol%;
the preparation method of the composite hydrogen storage material comprises the following steps: weighing magnesium amide, lithium hydride and alkali metal silicon hydride, mixing, putting into a ball milling tank, vacuumizing the ball milling tank, filling hydrogen pressure, and putting the ball milling tank into a ball mill for ball milling.
2. The composite hydrogen storage material of claim 1, wherein the alkali metal silicon hydride comprises potassium silicon hydride KSiH3Rubidium hydrosilation RbSiH3And cesium hydrosilate CsSiH3At least one of them.
3. The composite hydrogen storage material according to claim 1, wherein the hydrogen pressure is 2 to 5 MPa.
4. The composite hydrogen storage material of claim 1, wherein before the step of evacuating the ball mill tank and charging hydrogen pressure, the method further comprises:
and adding an abrasive into a ball milling tank, wherein the mass ratio of the abrasive to the mixture of the magnesium amide, the lithium hydride and the alkali metal silicon hydride is 40-120: 1.
5. The composite hydrogen storage material of claim 4, wherein the abrasive comprises steel balls having diameters of 12mm, 10mm and 7mm, respectively, wherein the number of steel balls having a diameter of 12mm is 4, the number of steel balls having a diameter of 10mm is 6, and the number of steel balls having a diameter of 12mm is 18.
6. The composite hydrogen storage material of claim 4, wherein the ball mill tank comprises a steel tank having a volume of 180 mL.
7. The composite hydrogen storage material of claim 1, wherein the ball mill is operated in a ball milling mode with a rotation speed of 300-500 rpm for 12-36 h and a clockwise and counterclockwise alternation.
8. The composite hydrogen storage material of claim 1, wherein the ball mill is a planetary ball mill.
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