CN113336188A - Composite hydrogen storage material NaBH4@ NiCo-NC and preparation method thereof - Google Patents
Composite hydrogen storage material NaBH4@ NiCo-NC and preparation method thereof Download PDFInfo
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- 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 belongs to the technical field of hydrogen storage materials, and particularly relates to a composite hydrogen storage material NaBH4@ NiCo-NC and a preparation method thereof. The method comprises the following steps: preparing NiCo-MOFs nano-sheets; preparing a sheet-shaped carrier NiCo-NC porous carbon material; NaBH4Preparation of @ NiCo-NC. Wherein the synthesis of the flake NiCo-NC template material is controlled by controlling the temperature rise process; nano NaBH4The load of the NiCo-NC is 20-60%, and the mass fraction of the NiCo-NC is 80-40%. NaBH4The hydrogen storage material has poor dynamic performance and poor cycle reversibility, and the NaBH in the composite material is prepared by the method of the invention4Complete reversibility is realized at 400 ℃, and the hydrogen evolution kinetic performance is obviously improved. Therefore, the material prepared by the invention has excellent hydrogen storage performance. The method has the advantages of simple process, easy operation, convenient synthesis and easy realization.
Description
Technical Field
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a composite hydrogen storage material NaBH4@ NiCo-NC and a preparation method thereof.
Background
Hydrogen energy is an ideal alternative energy source of the traditional fossil fuel, and the development of a safe, efficient and economic hydrogen storage means is a key step of the practical application of the hydrogen storage material. Solid-state hydrogen storage has advantages of good safety, high hydrogen storage capacity, and the like, compared to high-pressure gaseous hydrogen storage and liquid hydrogen storage, and thus, more and more researches have been made on development and improvement of performance of solid-state hydrogen storage material systems [1 ].
In recent years, metal complex hydrides have received much attention from researchers because of their higher mass and volume hydrogen storage density relative to metal hydrides [2]. In which NaBH is present4Having a mass hydrogen storage density of 10.8 wt% and a density of 115 kg-m-3The volume hydrogen storage density of (3) is a very potential metal coordination hydride hydrogen storage material]. However, NaBH4Of high thermodynamic stability, pure NaBH4The hydrogen evolution is started above 500 ℃ and NaBH is added4The hydrogen release kinetics and the cycle performance of the hydrogen storage material are poor, and the characteristics restrict the application of the hydrogen storage material. Researchers have adopted methods of nanocrystallization, addition of catalysts and combination of both to improve NaBH4Hydrogen storage performance of (1). Peter Ngene et al found that NaBH4Confinement in a nanoporous carbon template, NaBH4The initial hydrogen releasing temperature is reduced by 220 ℃, and the hydrogen releasing capacity is only 43 percent after hydrogen is absorbed under the hydrogen pressure of 325 ℃ and 60 bar [4 ]]. Another study has prepared NaBH by a solution method4Nano particles and in-situ reduction of metal coating layer on the surface thereof, and prepared metal-coated NaBH4The hydrogen storage performance of the nano-particles is obviously improved [5 ]](ii) a Meganne et al NaBH prepared by this method4The @ Ni composite material combines the catalytic action of nano confinement and Ni, and realizes the hydrogen storage capacity of a recyclable system of 2.5 wt% at 350 ℃ [6 ]]. NaBH prepared by Chong et al graphene coating method4@ G nanomaterial, the initial hydrogen evolution temperature of the material drops to only 40 ℃, the composite material can release 7.0 wt% of hydrogen during the process of heating to 460 ℃ in steps, and the partial hydrogen storage capacity is completely reversible, but the hydrogen evolution temperature is still relatively high in practical application [ 7%]. Based on these studies, we utilized a sheet-like porous carbon material template loaded with NiCo catalyst to deposit NaBH4The nano confinement and in-situ catalytic combination are combined, and the reversible capacity of the composite material with the weight percent of 4.5 percent is realized at the temperature of 400 ℃.
1] Yu X, Tang Z, Sun D, et al. Recent advances and remaining challenges of nanostructured materials for hydrogen storage applications[J]. Progress in Materials Science, 2017, 88: 1-48.
[2] He T, Cao H, Chen P. Complex hydrides for energy storage, conversion, and utilization[J]. Advanced Materials, 2019, 31(50): 1902757.
[3] Humphries T D, Kalantzopoulos G N, Llamas-Jansa I, et al. Reversible hydrogenation studies of NaBH4 milled with Ni-containing additives[J]. The Journal of Physical Chemistry C, 2013, 117(12): 6060-6065.
[4] Ngene P, van den Berg R, Verkuijlen M H W, et al. Reversibility of the hydrogen desorption from NaBH4 by confinement in nanoporous carbon[J]. Energy & Environmental Science, 2011, 4(10): 4108-4115.
[5] Christian M, Aguey-Zinsou K F. Synthesis of core–shell NaBH4@M (M= Co, Cu, Fe, Ni, Sn) nanoparticles leading to various morphologies and hydrogen storage properties[J]. Chemical Communications, 2013, 49(60): 6794-6796.
[6] Christian M L, Aguey-Zinsou K F. Core–shell strategy leading to high reversible hydrogen storage capacity for NaBH4[J]. ACS nano, 2012, 6(9): 7739-7751.
[7] Chong L, Zeng X, Ding W, et al. NaBH4 in “graphene wrapper:” significantly enhanced hydrogen storage capacity and regenerability through nanoencapsulation[J]. Advanced Materials, 2015, 27(34): 5070-5074。
Disclosure of Invention
The invention aims to provide a composite hydrogen storage material with high hydrogen storage capacity, low hydrogen release temperature and good cycle performance and a preparation method thereof.
The composite hydrogen storage material provided by the invention is a sheet-shaped porous carbon composite material loaded with sodium borohydride and attached with a nickel-cobalt catalyst, and is recorded as NaBH4@NiCo-NC。
Hair brushThe composite hydrogen storage material NaBH4The preparation method of @ NiCo-NC comprises the steps of preparing NiCo-MOFs nano-sheets, and calcining the NiCo-MOFs nano-sheets under inert gas to obtain a NiCo-NC porous carbon material; reacting NaBH4Dissolving in organic solvent, loading the solution and pumping to obtain NaBH4@ NiCo-NC; the method comprises the following specific steps:
(1) preparation of NiCo-MOFs nano-sheet:
reacting for 3-8 hours under continuous ultrasound by taking N, N-dimethylformamide as a solvent, Co salt and Ni salt as a Co source and a Ni source and terephthalic acid and triethylamine as ligands to obtain a NiCo-MOFs sheet material;
the method comprises the following specific operations: dissolving Ni salt, Co salt and terephthalic acid in a mixed solution of ethanol, water and N, N-dimethylformamide at room temperature (such as 25-30 ℃); stirring the obtained mixed solution, continuously performing ultrasonic treatment in an ultrasonic machine for 3-8 hours, centrifugally cleaning with ethanol, ultrasonically dispersing in distilled water, and freeze-drying to obtain a nanosheet material, which is marked as NiCo-MOFs;
(2) preparing a NiCo-NC sheet nano porous carbon template:
transferring the NiCo-MOFs nano-sheets into a tube furnace, heating to 600-fold-of-organic-carbon (I) temperature at the speed of 1-3 ℃/min under the protection of inert gas, preserving heat for 1-3 h, carbonizing, and cooling to obtain a sheet-shaped nano porous carbon template, which is marked as NiCo-NC; the NiCo particles in the NiCo-NC are uniform in size and have the particle size of 20-50 nm;
(3) solution method of NaBH4Loading to NiCo-NC:
reacting NaBH4Dissolving in organic solvent (such as diethylene glycol dimethyl ether, tetrahydrofuran, etc.), stirring to obtain colorless clear solution; adding NiCo-NC into the mixture, and performing ultrasonic dispersion uniformly; removing the solvent, NaBH, by extracting the solvent4Nucleation and growth on NiCo-NC to obtain NaBH4Supported nickel-cobalt-containing sheet-like porous carbon material, noted NaBH4@ NiCo-NC; loaded NaBH4The particle size of the nano-particles is uniform, and the particle size is 30-70 nm.
In the step (1) of the invention, Ni (NO) is adopted as the Ni salt3)2·6H2O, the CThe o salt is Co (NO)3)2·6H2O; the molar ratio of the Ni salt to the Co salt is in the range of 1:2 to 2: 1.
In step (3) of the present invention, NaBH is adjusted4And the addition amount of NiCo-NC, and controlling the contents of the two components: NaBH4The mass percent of the NiCo-NC is 20-60%, and the mass percent of the NiCo-NC is 80-40%.
In step (3) of the present invention, the organic solvent is preferably diethylene glycol dimethyl ether or tetrahydrofuran.
NaBH prepared by the invention4The @ NiCo-NC is a high-efficiency composite hydrogen storage material and has excellent hydrogen storage performance. The hydrogen can be released by heating to 315 ℃, and the hydrogen can be completely released by heating to 550 ℃. NaBH at 400 ℃ C4The @ NiCo-NC may achieve a system cycle hydrogen storage capacity of 4.5 wt%.
The invention has the following advantages:
(1) NaBH for use in the invention4The material as hydrogen source is cheap.
(2) The loading method used by the invention has low requirements on equipment and is easy to realize.
(3) Simple process and convenient synthesis.
(4) The hydrogen release temperature is relatively low, and the system reversible hydrogen storage capacity of 4.5 wt% is realized at 400 ℃.
Drawings
FIG. 1 is SEM and TEM images of different stage products. Wherein, (a) SEM picture of NiCo-MOFs nano-sheet, (b) SEM picture of NiCo-NC, (c) NaBH4SEM pictures of @ NiCo-NC, (d) TEM pictures of NiCo-NC, (e) NaBH4TEM image of @ NiCo-NC, (f) NaBH4HRTEM image of @ NiCo-NC.
Figure 2 is an XRD spectrum of the different stage product.
Figure 3 is a graph of the TPD hydrogen evolution for different samples. Wherein, the curve with dots is commercialized NaBH4The solution method with a pentagram curve is used for preparing porous carbon loaded NaBH after NiCo etching according to the mass ratio of 1:14The curve with a square is NaBH ball-milled according to the mass ratio of 1:14And NiCo-NC with triangular curve in mass ratioNaBH prepared for 1:1 solution process4@NiCo-NC。
FIG. 4 shows NaBH at different temperatures4Constant temperature hydrogen discharge curve of @ NiCo-NC and ball milling NaBH4Comparative plot at 400 ℃.
FIG. 5 shows NaBH at 400 deg.C 45 cycles of dehydrogenation curve @ NiCo-NC.
FIG. 6 shows NaBH loadings of 60% and 67% at 400 deg.C4Constant temperature Hydrogen desorption Curve of @ NiCo-NC.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1:
(1) preparation of flaky NiCo-MOFs
0.75 mmol of Ni (NO) at room temperature (25 ℃ C.)3)2·6H2O、0.75 mmol Co(NO3)2·6H2O and 1.5 mmol of terephthalic acid were dissolved in a mixed solution composed of 4 mL of ethanol, 4 mL of water and 64 mL of N, N-dimethylformamide. 1.6 mL of triethylamine was added rapidly and stirred for 5 minutes. The product was placed in an ultrasonic machine and sonicated for 8 h. After three centrifugation washes with ethanol, the product was dispersed in water and sonicated for 30 minutes. And (4) freeze-drying the dispersed product for 72 h to finally obtain the NiCo-MOFs nanosheet material.
(2) Preparation of NiCo-NC porous nanosheet
And (3) placing the NiCo-MOFs after freeze drying in a tube furnace, heating to 900 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 1h, and cooling to obtain a product, namely NiCo-NC.
(3) 50% load of NaBH4Preparation of @ NiCo-NC
In an argon glove box, 50 mg NaBH4Added into 25 mL of diethylene glycol dimethyl ether and stirred for 1h to obtain a transparent clear solution. Adding 50 mg NiCo-NC, continuously carrying out ultrasonic treatment in an ultrasonic machine for 0.5 h, transferring the ultrasonic product into a reaction tube, drying the solvent at 80 ℃ and continuously carrying out vacuum treatment for 12 h to obtain the product, namely NaBH with the load of 50 percent4@NiCo-NC。
Prepared NaBH with 50% loading capacity4The @ NiCo-NC starts to release hydrogen slowly at about 150 ℃, the hydrogen release rate is obviously increased at 310 ℃, and complete hydrogen release can be realized at 550 ℃, as shown in figure 3.
Example 2:
NiCo-NC porous nanosheets were prepared in the same manner as in step (1) and step (2) of example 1, and 30 mg of NaBH was placed in an argon glove box4Added into 15 mL of diethylene glycol dimethyl ether and stirred for 1h to obtain a transparent clear solution. Adding 20 mg NiCo-NC, continuously carrying out ultrasonic treatment in an ultrasonic machine for 0.5 h, transferring the ultrasonic product into a reaction tube, drying the solvent at 80 ℃ and continuously carrying out vacuum treatment for 12 h to obtain the product which is 60% loaded NaBH4@ NiCo-NC. At 400 ℃, NaBH with 60 percent of prepared load capacity4@ NiCo-NC may evolve 7.4 wt.% (relative to NaBH) within 6h4Mass of) much higher than commercial NaBH4The hydrogen evolution (1.3 wt%) was 6h at 440 ℃.
Example 3:
NiCo-NC porous nanosheets were prepared in the same manner as in step (1) and step (2) of example 1, and 40 mg of NaBH was placed in an argon glove box4Added into 20 mL of diethylene glycol dimethyl ether and stirred for 1h to obtain a transparent clear solution. Adding 20 mg NiCo-NC, continuously carrying out ultrasonic treatment in an ultrasonic machine for 0.5 h, transferring the ultrasonic product into a reaction tube, drying the solvent at 80 ℃ and continuously carrying out vacuum treatment for 12 h to obtain the product of NaBH with 67% loading4@ NiCo-NC. At 400 ℃, 67% load of NaBH is prepared4@ NiCo-NC may evolve 7.5 wt.% (relative to NaBH) within 6h4Mass of) much higher than commercial NaBH4Hydrogen evolution at 440 ℃ for 6 h.
Claims (5)
1. The preparation method of the composite hydrogen storage material is characterized by comprising the following specific steps of:
(1) preparation of NiCo-MOFs nano-sheet:
reacting for 3-8 hours under continuous ultrasound by taking N, N-dimethylformamide as a solvent, Co salt and Ni salt as a Co source and a Ni source and terephthalic acid and triethylamine as ligands to obtain a nanosheet material, which is marked as NiCo-MOFs;
(2) preparing a NiCo-NC sheet nano porous carbon template:
transferring the NiCo-MOFs nano-sheets into a tube furnace, heating to 600-fold-of-organic-carbon (I) temperature at the speed of 1-3 ℃/min under the protection of inert gas, preserving heat for 1-3 h, carbonizing, and cooling to obtain a sheet-shaped nano porous carbon template, which is marked as NiCo-NC; the NiCo particles in the NiCo-NC are uniform in size and have the particle size of 20-50 nm;
(3) solution method of NaBH4Loading to NiCo-NC:
reacting NaBH4Dissolving in organic solvent, stirring and dissolving to obtain colorless clear solution; adding NiCo-NC into the mixture, and performing ultrasonic dispersion uniformly; removing the solvent, NaBH, by extracting the solvent4Nucleation and growth on NiCo-NC to obtain NaBH4Supported nickel-cobalt-containing sheet-like porous carbon material, noted NaBH4@ NiCo-NC; loaded NaBH4The particle size of the nano-particles is uniform, and the particle size is 30-70 nm.
2. The method according to claim 1, wherein in the step (1), Ni (NO) is used as the Ni salt3)2·6H2O, the Co salt adopts Co (NO)3)2·6H2O; the molar ratio of the Ni salt to the Co salt is in the range of 1:2 to 2: 1.
3. The method according to claim 1, wherein in step (3), NaBH is adjusted4And the addition amount of NiCo-NC, and controlling the contents of the two components: NaBH4The mass percent of the NiCo-NC is 20-60%, and the mass percent of the NiCo-NC is 80-40%.
4. The method according to claim 1, wherein the organic solvent in the step (3) is diethylene glycol dimethyl ether or tetrahydrofuran.
5. A process for the preparation of a compound of the formula I as claimed in any of claims 1 to 4The composite hydrogen storage material obtained by the method is a sheet-shaped porous carbon composite material loaded with sodium borohydride and attached with a nickel-cobalt catalyst, and is marked as NaBH4@NiCo-NC。
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| CN113979407A (en) * | 2021-11-10 | 2022-01-28 | 复旦大学 | Composite hydrogen storage material NaBH4@ NiB-CNC and preparation method thereof |
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