CN108658038B - Based on LiAlH4Hydrogen storage material and method for producing the same - Google Patents

Based on LiAlH4Hydrogen storage material and method for producing the same Download PDF

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CN108658038B
CN108658038B CN201810689813.4A CN201810689813A CN108658038B CN 108658038 B CN108658038 B CN 108658038B CN 201810689813 A CN201810689813 A CN 201810689813A CN 108658038 B CN108658038 B CN 108658038B
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lialh
hydrogen
additive
hydrogen storage
storage material
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CN108658038A (en
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孙立贤
陈沛荣
徐芬
王飞飞
印世璐
程日光
曹黎志
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Guilin University of Electronic Technology
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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
    • 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

Abstract

The invention discloses a method based on LiAlH4Of LiAlH4And metal nanoparticle loaded carbon material additive (Ni-Co/C). The preparation method comprises the following steps: 1) preparing a precursor of the Ni-Co/C additive; 2) preparing Ni-Co/C additive; 3) based on LiAlH4And (4) preparing the hydrogen storage material. Greatly reduce LiAlH4When the doping amount of the catalyst is 2wt%, the hydrogen releasing temperature of the system is reduced to 70 ℃, and the hydrogen releasing amount reaches 7.2 wt%; when the doping amount of the catalyst is 10wt%, the hydrogen releasing temperature of the system is reduced to 50 ℃, and the hydrogen releasing amount reaches 6.4 wt%. The catalyst Ni-Co/C prepared by the invention has the advantages that the metal particles reach the nano scale and have high dispersibility; the LiAlH thus obtained4The composite hydrogen storage material can show good hydrogen release performance at a lower temperature.

Description

Based on LiAlH4Hydrogen storage material and method for producing the same
Technical Field
The invention relates to a hydrogen storage material of a new energy material, in particular to a LiAlH-based hydrogen storage material4The hydrogen storage material and the preparation method thereof.
Background
The depletion of energy has become a common problem facing human beings, the search of green, efficient and renewable new energy for replacing fossil energy becomes a development target of all countries in the world, and a great deal of research in the academic world is obtained at present. The hydrogen energy is one of the most potential alternative energy sources due to the advantages of high heat value, environmental protection, no pollution, renewability and the like. At present, the development and utilization of hydrogen energy mainly face three key problems of production, storage and transportation. Among them, how to safely and efficiently use hydrogen energy as vehicle-mounted storage is the research subject with the most challenging and commercial value at present. The traditional high-pressure liquid and gaseous hydrogen storage has low efficiency and low safety, which become important factors restricting large-scale commercialization of vehicle-mounted hydrogen storage, and solid hydrogen storage has great research potential as a hydrogen storage mode with large hydrogen storage amount, and is the most popular hydrogen storage direction currently researched.
LiAlH4It is considered as the most potential solid hydrogen storage material because of its high hydrogen storage capacity (10.6 wt%), but it cannot be practically used because of its high hydrogen discharge temperature, poor reversibility and other disadvantages.
In recent years, most research has focused on catalytic modification of the catalyst, and reports have been made of Ti, Fe, TiF3，SrFe12O19，CoFe2O4，NiFe3O4，Li2TiO3Can effectively reduce LiAlH4The hydrogen discharge temperature and the hydrogen discharge rate are improved; meanwhile, with the extensive research of carbon materials in recent years, the carbon materials have good dispersibility and thermal conductivity, so that the carbon materials are found to be capable of effectively improving LiAlH to a certain extent4Hydrogen evolution performance of.
Researches show that the metal-loaded carbon material can effectively improve LiAlH4The carbon material enables the catalyst to have higher dispersity in the hydrogen storage material, the high activity of the nano metal particles has strong catalytic capability, and the synergistic effect of the two can greatly improve the LiAlH4Hydrogen evolution performance of.
The MWCNTs loaded with Co and Ni were prepared by chemical reduction method using Wen-Ta Tsai et al, and it was found that LiAlH can be converted to a mixture of 20wt% MWCNT/Co4The hydrogen release temperature is about 103 ℃ ahead of time; when 20wt% MWCNT/Ni was added, the hydrogen evolution temperature was lowered to 77 ℃. (Tan, C. -Y.; Tsai, W. -T., Effects of Ni and Co-purified MWCNTs addition on the hydrogenation catalyst and stability of LiAlH.; and4. International Journal of Hydrogen Energy 2015, 40, 14064-14071.）。
YIjing Wang et al prepared a Co-supported carbon material as a catalyst and found that the amount of Co/C, LiAlH added was 10wt%4The initial hydrogen release temperature is reduced to 100 ℃, and the hydrogen release amount can reach 7.05 wt%.
Both of the above materials have the following problems: (1) the initial hydrogen release temperature is higher; (2) the large amount of catalyst added results in a decrease in the amount of hydrogen released. (Li, L.; Wang, Y.; Jiano, L.; Yuan, H., Enhanced catalytic efficiencies of Co @ C additive on dehydrogenation properties of LiAlH 4. Journal of Alloys and Compounds 2015, 645, S468-S471.) therefore, how to reduce the hydrogen evolution temperature is the key to the study of this type of catalyst, and further improvement can be achieved by nanosized metal particles while increasing their degree of dispersion on the carbon substrate surface.
Based on the consideration, the method adopts a Ni and Co bimetal loading mode, uses cheaper glucose as a carbon substrate to synthesize the metal nanoparticle loaded carbon material catalyst, and can be used for observing that metal particles reach the nanometer scale under a scanning electron microscope and are uniformly dispersed on the surface of the carbon substrate. The hydrogen discharge performance test shows that the LiAlH is greatly improved by the catalyst4The dehydrogenation performance of (c).
Disclosure of Invention
The invention aims to provide a hydrogen storage material catalyst, which is used for synthesizing a metal nanoparticle loaded carbon material (Ni-Co/C), and takes Ni-Co/C as a catalyst and LiAlH4Compounding to effectively improve LiAlH4The method has simple process and low cost, and is suitable for large-scale production.
In order to achieve the aim, the specific technical scheme for achieving the aim of the invention is as follows:
the preparation method of the Ni-Co/C comprises the following specific preparation processes:
mixing Ni (NO)3)2·6H2O、Co(NO3)2·6H2O, glucose and hexamethylenetetramine are respectively used as a nickel source, a cobalt source, a carbon source and a complexing agent according to a certain proportion (1-2): (1-2): 1: dissolving 1 in deionized water, stirring, carrying out hydrothermal reaction at 180-200 ℃ for 12-24 h, carrying out suction filtration washing, carrying out vacuum drying at 60-80 ℃ for 12-24 h, heating to 600-800 ℃ at a heating rate of 3-5 ℃/min in a nitrogen atmosphere, keeping for 2-5 h, and naturally cooling to room temperature.
Mixing LiAlH4Compounding with Ni-Co/C material, and hydrogen releasing from the composite materialAnd (3) testing the performance, wherein the specific operation process is as follows:
(1) in an argon atmosphere glove box, LiAlH4And weighing a sample according to a certain ratio (100-10): 1, wherein the total mass of the sample is 0.5g, putting the sample into a stainless steel ball milling tank, the ball-material ratio is (60-40): 1, packaging the ball milling tank and taking the ball milling tank out of the glove box.
(2) The ball milling pot is arranged on a planetary ball mill, the ball milling time is set to be 0.5-3 h, and the rotating speed is set to be 300-600 r/min.
(3) And (4) after the ball milling is finished, putting the ball milling tank into a glove box, and taking out the ball-milled sample for later use.
(4) Weighing a proper amount of sample (600-800 mg), and heating to 300 ℃ at a heating rate of 3 ℃/min to test the hydrogen release performance of the hydrogen storage material.
The invention has the following advantages:
the method adopts glucose and hexamethylenetetramine as a carbon source and a complexing agent respectively, and has simple and easy operation process and low cost;
secondly, the carbon material has good thermal conductivity and dispersibility, and the agglomeration phenomenon of the hydrogen storage material is effectively reduced;
thirdly, synthesizing metal particles with nanometer scale, and highly and uniformly dispersing the metal particles on the surface of the carbon substrate;
fourthly, effectively improves LiAlH4When the doping amount of the catalyst is 2wt%, the hydrogen releasing temperature of the system is reduced to 75 ℃, and the hydrogen releasing amount reaches 7.2 wt%; when the doping amount of the catalyst is 10wt%, the hydrogen releasing temperature of the system is reduced to 55 ℃, the hydrogen releasing amount reaches 6.4wt%, and the hydrogen releasing performance is greatly improved.
Description of the drawings:
fig. 1 is an XRD pattern of carbon-supported nano-metal particles of specific example 1 of the present invention;
fig. 2 is an SEM image of carbon-supported nano-metal particles of embodiment 1 of the present invention;
FIG. 3 is a dehydrogenation curve of LiAlH4 doped with 0wt% Ni-Co/C according to specific example 2 of the present invention;
FIG. 4 is a dehydrogenation curve of LiAlH4 doped with 2wt% Ni-Co/C according to specific example 3 of the present invention;
FIG. 5 is a dehydrogenation curve of LiAlH4 doped with 5wt% Ni-Co/C according to specific example 4 of the present invention;
FIG. 6 is a dehydrogenation curve of LiAlH4 doped with 10wt% Ni-Co/C according to specific example 5 of the present invention.
Detailed Description
The invention is further described in detail by the embodiments and the accompanying drawings, but the invention is not limited thereto.
Example 1
Step 1) weighing 0.7g of glucose and 0.7g of hexamethylenetetramine, dissolving in 40ml of deionized water, and continuously stirring; 2.5mmol Co (NO) were weighed out separately3)2·6H2O、Ni(NO3)2·6H2Dissolving O in 15ml of deionized water respectively, stirring fully and continuously, pouring the solution, and continuously stirring for 30 min;
step 2) pouring the solution into a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven for hydrothermal reaction for 24 hours at 180 ℃, and then cooling to room temperature;
step 3), after the hydrothermal reaction is finished, performing suction filtration and washing on the product for 3 times by using alcohol and deionized water respectively, and drying the washed product in a vacuum drying oven at 60 ℃ for 12 hours;
and 4) placing the product in a tubular furnace, adopting nitrogen as protective gas, raising the temperature to 700 ℃ at the heating rate of 5 ℃/min at the airflow flow rate of 60ml/min, keeping the temperature for 3h, and then cooling to room temperature to obtain the target product Ni-Co/C.
Example 2
Step 1) weighing 0.5g of LiAlH in an argon atmosphere glove box4And (3) putting the mixture into a stainless steel ball milling tank with a ball-to-material ratio of 40:1, packaging the ball milling tank and taking the ball milling tank out of the glove box.
And 2) canning the ball mill on a planetary ball mill, setting the ball milling time to be 0.5h and the rotating speed to be 450 r/min.
And 3) after the ball milling is finished, putting the ball milling tank into a glove box, and taking out the ball-milled sample for later use.
And 4) weighing a proper amount of sample (600-800 mg), and heating to 300 ℃ at a heating rate of 3 ℃/min to test the hydrogen release performance of the hydrogen storage material.
Example 3
Step 1) 0.01g of Ni-Co/C and 0.49g of LiAlH are respectively weighed in an argon atmosphere glove box4And (3) putting the mixture into a stainless steel ball milling tank with a ball-to-material ratio of 40:1, packaging the ball milling tank and taking the ball milling tank out of the glove box.
And 2) canning the ball mill on a planetary ball mill, setting the ball milling time to be 0.5h and the rotating speed to be 450 r/min.
And 3) after the ball milling is finished, putting the ball milling tank into a glove box, and taking out the ball-milled sample for later use.
And 4) weighing a proper amount of sample (600-800 mg), and heating to 300 ℃ at a heating rate of 3 ℃/min to test the hydrogen release performance of the hydrogen storage material.
Example 4
Step 1) respectively weighing 0.025g of Ni-Co/C and 0.475g of LiAlH in an argon atmosphere glove box4And (3) putting the mixture into a stainless steel ball milling tank with a ball-to-material ratio of 40:1, packaging the ball milling tank and taking the ball milling tank out of the glove box.
And 2) canning the ball mill on a planetary ball mill, setting the ball milling time to be 0.5h and the rotating speed to be 450 r/min.
And 3) after the ball milling is finished, putting the ball milling tank into a glove box, and taking out the ball-milled sample for later use.
And 4) weighing a proper amount of sample (600-800 mg), and heating to 300 ℃ at a heating rate of 3 ℃/min to test the hydrogen release performance of the hydrogen storage material.
Example 5
Step 1) respectively weighing 0.05g of Ni-Co/C and 0.45g of LiAlH in an argon atmosphere glove box4And (3) putting the mixture into a stainless steel ball milling tank with a ball-to-material ratio of 40:1, packaging the ball milling tank and taking the ball milling tank out of the glove box.
And 2) canning the ball mill on a planetary ball mill, setting the ball milling time to be 0.5h and the rotating speed to be 450 r/min.
And 3) after the ball milling is finished, putting the ball milling tank into a glove box, and taking out the ball-milled sample for later use.
And 4) weighing a proper amount of sample (600-800 mg), and heating to 300 ℃ at a heating rate of 3 ℃/min to test the hydrogen release performance of the hydrogen storage material.
The hydrogen storage material prepared in example 2 was subjected to a hydrogen desorption performance test, and the result is shown in fig. 2, which shows that the initial hydrogen desorption temperature was 190 ℃, and the hydrogen desorption amount was 7.3wt% when the temperature was raised to 300 ℃.
The hydrogen storage material prepared in example 3 was subjected to a hydrogen desorption performance test, and the result is shown in fig. 3, which shows that the initial hydrogen desorption temperature was 75 ℃, and the hydrogen desorption amount was 7.2wt% when the temperature was raised to 300 ℃.
The hydrogen storage material prepared in example 4 was subjected to a hydrogen desorption performance test, and the result is shown in fig. 4, which shows that the initial hydrogen desorption temperature was 63 ℃ and the hydrogen desorption amount was 6.6wt% when the temperature was raised to 300 ℃.
The hydrogen storage material prepared in example 5 was subjected to a hydrogen desorption performance test, and the result is shown in fig. 5, which shows that the initial hydrogen desorption temperature was 55 ℃, and the hydrogen desorption amount was 6.4wt% when the temperature was raised to 300 ℃.

Claims (3)

1. Based on LiAlH4The hydrogen storage material of (2), characterized in that: from LiAlH4And metal nano particle loaded carbon material additive Ni-Co/C;
the Ni-Co/C additive is prepared by loading Ni and Co on carbon simultaneously by a hydrothermal method by using a nickel source, a cobalt source, a carbon source and a complexing agent according to a certain substance quantity ratio;
the nickel source is Ni (NO)3)2·6H2The O and cobalt source is Co (NO)3)2·6H2O, a carbon source of glucose and a complexing agent of hexamethylenetetramine, wherein the mass ratio of Co to Ni is 1: 1;
the LiAlH4And the Ni-Co/C additive is (100-10) in percentage by mass: 1.
2. LiAlH-based according to claim 14The method for preparing the hydrogen storage material is characterized by comprising the following steps:
step 1) preparing a precursor of the Ni-Co/C additive, namely dissolving a nickel source, a cobalt source, a carbon source and a complexing agent in a solvent according to a certain mass ratio, performing hydrothermal reaction under a certain condition, performing suction filtration and washing, and drying in a vacuum drying oven to obtain the precursor of the Ni-Co/C additive;
the mass ratio of the nickel source, the cobalt source, the carbon source and the complexing agent in the step 1) is (1-2): (1-2): 1:1, the hydrothermal reaction in the step 1) is carried out under the conditions that the hydrothermal temperature is 180-200 ℃ and the hydrothermal time is 12-24 hours;
step 2) preparation of Ni-Co/C additives, namely calcining the precursor obtained in the step 1 under certain conditions to obtain a product Ni-Co/C additives;
the calcining condition in the step 2) is that nitrogen is used as protective atmosphere, the calcining temperature is 600-800 ℃, and the calcining time is 2-5 h;
step 3) based on LiAlH4Preparing a hydrogen storage material by mixing the LiAlH obtained in the step 2 according to a certain mass ratio4And additives, and ball milling under certain conditions to obtain the LiAlH-based material4The hydrogen storage material of (a);
the step 3) LiAlH4And the additive in a mass ratio of (100-10): 1, the ball milling conditions are that argon is used as protective atmosphere, and the ball-to-material ratio is (60-40): 1, ball milling time is 0.5-3 h, and rotating speed is 300-600 r/min.
3. LiAlH-based according to claim 14The hydrogen storage material is applied to the field of hydrogen storage, and is characterized in that: when the doping amount of the catalyst is 2wt%, the hydrogen releasing temperature of the system is reduced to 70 ℃, and the hydrogen releasing amount reaches 7.2 wt%; when the doping amount of the catalyst is 10wt%, the hydrogen releasing temperature of the system is reduced to 50 ℃, and the hydrogen releasing amount reaches 6.4 wt%.
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CN111439723A (en) * 2020-04-16 2020-07-24 安泰科技股份有限公司 Doped Mg (BH)4)2Hydrogen-based storage material and preparation method thereof
CN112408317A (en) * 2020-12-01 2021-02-26 桂林电子科技大学 Carbon-loaded titanium dioxide-doped lithium aluminum hydride hydrogen storage material and preparation method thereof
CN113336188B (en) * 2021-06-02 2022-09-16 复旦大学 Composite hydrogen storage material NaBH 4 @ NiCo-NC and preparation method thereof
CN113769750B (en) * 2021-09-15 2024-02-27 江苏科技大学 Simple preparation method of NiO@C nano powder and application of NiO@C nano powder in hydrogen storage material

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Effects of Ni and Co-decorated MWCNTs addition on the dehydrogenation behavior and stability of LiAlH4;Chia-Yen Tan et.al;《hydrogen energy》;20150330;第40卷;第14064-14065页、第14068页 *
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