CN117983242A - A Ag-Co3O4 metal nanocomposite material and its preparation method and application - Google Patents
A Ag-Co3O4 metal nanocomposite material and its preparation method and application Download PDFInfo
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- CN117983242A CN117983242A CN202310696788.3A CN202310696788A CN117983242A CN 117983242 A CN117983242 A CN 117983242A CN 202310696788 A CN202310696788 A CN 202310696788A CN 117983242 A CN117983242 A CN 117983242A
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Abstract
本发明公开了一种Ag‑Co3O4金属纳米复合材料及其制备方法和应用，涉及金属复合材料技术领域，将Co(NO3)2·6H2O和AgNO3置于容器中，再向其中倒入无水乙醇，在常温下搅拌均匀后，对搅拌均匀的溶液边搅拌边加热，直至剩余少量液体时停止加热，继续搅拌至出现粉红色粉末时停止，冷却至室温；将所述红色粉末置于加热装置中加热至高温并在该温度下煅烧，得到最终黑色粉末状固体样品。本发明制备方法操作简单，安全可控，产率高；在常温环境条件下的对氨硼烷络合物水解产氢具有高效的催化活性，针对银元素而言，其TOF值达到了265.4min‑1；且制备成本低，能够有效利用银等稀缺资源，该催化剂中银元素的质量含量为2.002％。
The invention discloses a Ag-Co 3 O 4 metal nanocomposite material and a preparation method and application thereof, and relates to the technical field of metal composite materials. Co(NO 3 ) 2 ·6H 2 O and AgNO 3 are placed in a container, and then anhydrous ethanol is poured therein, and after being stirred evenly at room temperature, the stirred solution is heated while stirring until a small amount of liquid is left, and the heating is stopped, and the stirring is continued until a pink powder appears, and the mixture is cooled to room temperature; the red powder is placed in a heating device and heated to a high temperature and calcined at the temperature to obtain a final black powder solid sample. The preparation method of the invention is simple to operate, safe and controllable, and has a high yield; the hydrolysis of ammonia borane complex to produce hydrogen under normal temperature environmental conditions has efficient catalytic activity, and for silver, its TOF value reaches 265.4min ‑1 ; and the preparation cost is low, and scarce resources such as silver can be effectively utilized, and the mass content of silver in the catalyst is 2.002%.
Description
Technical Field
The invention relates to the technical field of metal composite materials, in particular to an Ag-Co 3O4 metal nano composite material, a preparation method and application thereof.
Background
The current hydrogen energy is also widely applied, the application method is diversified, the heat energy can be directly generated by combustion, the fuel cell can be prepared by using the fuel as fuel, and the fuel cell has good application prospect in the fields of energy, traffic, industry and the like. The borane ammonia complex has the characteristics of higher hydrogen storage amount, safety, stability, no pollution and the like, and is an ideal solid hydrogen storage material.
Compared with other hydrogen storage methods, the solid hydrogen storage method has the advantages that a small space stores hydrogen with large volume density, the solid hydrogen storage method is easy to dissolve in solvents such as water, ethanol and sodium hydroxide, hydrogen production by hydrolysis of ammonia borane complex is one of hydrogen production paths, noble metals such as Pt, pd and Ru have special electronic structures, excellent catalytic activity is shown in the ammonia borane hydrolysis hydrogen production, but the noble metals have high cost and scarce resources, so that the solid hydrogen storage method is difficult to obtain large-scale application, and the catalytic activity of the noble metal catalyst in the ammonia borane hydrolysis hydrogen production is poor. Thus, the preparation of efficient low-cost catalysts has become a hot spot of research.
SaimThe nickel nanocluster and the cobalt nanocluster catalysts were synthesized by et al (Water soluble nickel(0)and cobalt(0)nanoclusters stabilized by poly(4-styrenesulfonic acid-co-maleic acid):Highly active,durable and cost effective catalysts in hydrogen generation from the hydrolysis of ammonia borane,International Journal of Hydrogen Energy,2011,36,1424-1432), respectively, and in the ammonia borane hydrolysis hydrogen production reaction, the conversion frequencies (TOF) of the two catalysts were 10.1min -1 (nickel cluster) and 25.7min -1 (cobalt cluster); yangbin Ren et Al (Ni-Mo2C Nanocomposites as Highly Efficient Catalysts for Hydrogen Generation from Hydrolysis of Ammonia Borane,Energy&Fuels,2021,35,19,16222-16231) synthesized a gamma-Al 2O3 supported Ni-Mo x C catalyst using an impregnation method, wherein 10Ni30Mo xC/γ-Al2O3 had the highest TOF value (75.1 min -1) in the hydroborazine hydrolysis hydrogen production reaction in the series of catalysts; ahmet Bulut et al (Carbon dispersed copper-cobalt alloy nanoparticles:Acost-effective heterogeneous catalyst with exceptional performance in the hydrolytic dehydrogenation of ammonia-borane,Applied Catalysis B:Environmental,2016,180,121-129) prepared a novel catalyst, bimetallic copper-cobalt alloy nanoparticles (CuCo/C) supported on activated carbon, with a TOF value of 2700h -1 in the hydrolysis hydrogen production reaction of ammonia borane.
However, the catalysts obtained by the above preparation methods all have the following disadvantages: the high-efficiency catalyst has high manufacturing cost, complex operation and harsh reaction conditions; and the catalytic activity of the catalyst on the ammonia borane complex hydrolysis hydrogen production is not high under the normal temperature environment condition.
Disclosure of Invention
The invention aims to provide an Ag-Co 3O4 metal nano composite material, a preparation method and application thereof, and solves the problems existing in the background technology.
The invention realizes the above purpose through the following technical scheme:
The invention provides a preparation method of an Ag-Co 3O4 metal nanocomposite, which comprises the following steps:
(1) Placing Co (NO 3)2·6H2 O and AgNO 3) in a container, pouring absolute ethyl alcohol into the container, stirring uniformly at normal temperature, heating the uniformly stirred solution while stirring until a small amount of liquid is remained, stopping heating, continuing stirring until pink powder appears, and cooling to the room temperature;
(2) And (3) placing the red powder into a heating device, heating to 500 ℃ at a certain heating rate, and calcining for 1h at the temperature to obtain a final black powdery solid sample, namely the Ag-Co 3O4 metal nanocomposite.
A further improvement is that the mass ratio of Co (NO 3)2·6H2 O to AgNO 3) is (90-100): 1.
A further improvement is that the temperature of heating in step (1) is 70-80 ℃ and the reactants turn black beyond 80 ℃.
The further improvement is that the temperature rising rate in the step (2) is 10-15 ℃/min.
The invention provides an Ag-Co 3O4 metal nano composite material which is prepared by the preparation method.
The Ag-Co 3O4 metal nano composite material is further improved in that the Ag-Co 3O4 metal nano composite material is in the shape of nano flower-like particles with the size of about 4.0 mu m, and silver atoms are uniformly distributed on the surfaces of the particles.
The invention provides an application of the Ag-Co 3O4 metal nano composite material in catalyzing ammonia borane complex hydrolysis to produce hydrogen.
The method for catalyzing ammonia borane complex hydrolysis to produce hydrogen comprises the following steps:
(1) The Ag-Co 3O4 metal nano composite material is taken as a catalyst, added into 1 mol.L -1 NaOH aqueous solution, and fully dispersed by ultrasonic treatment for 5 min;
(2) And (3) adding ammonia borane complex into the solution dispersed in the step (1), and collecting hydrogen by a drainage method while stirring.
The invention has the beneficial effects that:
1. the preparation method is simple to operate, safe and controllable, and high in yield;
2. the ammonia borane complex has high catalytic activity on hydrogen production by hydrolysis under the normal temperature environment, and for silver element, the TOF value reaches 347.85min -1;
3. The preparation cost is low, and scarce resources such as silver can be effectively utilized (the mass content of silver element in the catalyst is 2.002%).
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image and Energy Dispersive Spectroscopy (EDS) element map of an Ag-Co 3O4 metal nanocomposite;
FIG. 2 is an X-ray diffraction pattern of an Ag-Co 3O4 metal nanocomposite;
FIG. 3 is a graph showing the performance of an Ag-Co 3O4 catalyst in catalyzing the hydrolysis of ammonia borane to produce hydrogen;
FIG. 4 is a diagram showing a preparation process of Ag-Co 3O4 metal nanocomposite; a, preparing; b, before calcination; c, calcining.
FIG. 5 is a graph showing the performance test of the catalyst of Ag-Co 3O4 metal nano composite material prepared by adding different silver nitrate to catalyze ammonia borane to hydrolyze to produce hydrogen.
Detailed Description
The present application will be described in further detail with reference to the accompanying drawings, wherein it is to be understood that the following detailed description is for the purpose of further illustrating the application only and is not to be construed as limiting the scope of the application, as various insubstantial modifications and adaptations of the application to those skilled in the art can be made in light of the foregoing disclosure.
1. Material
The methods used in this example are conventional methods known to those skilled in the art unless otherwise indicated, and the materials such as reagents used are commercially available products unless otherwise indicated.
2. Method of
2.1 Preparation of Ag-Co 3O4
Weighing 1.8g of Co (NO 3)2·6H2 O) into a beaker, weighing 0.02g of AgNO 3 into the beaker containing Co (NO 3)2·6H2 O), pouring 5mL of absolute ethyl alcohol into the beaker, fully stirring the mixture at normal temperature to uniformly mix the mixture, pouring the uniformly stirred solution into an evaporation dish (shown in fig. 4 a), heating the mixture on an electric heating jacket while stirring, controlling the temperature of the solution to be about 80 ℃, slowly stirring to prevent the solution from splashing out, observing the condition of the solution while stirring, turning off a heating device when a small amount of liquid remains in the evaporation dish, and continuing stirring until the mixture becomes pink powder (shown in fig. 4 b).
After cooling to room temperature, the medicine in the evaporation pan is transferred and the medicine attached to the evaporation pan is scraped off with a clean medicine spoon and weighed. The drug product was then placed in a clean crucible and heated to 500 ℃ in a muffle furnace at a heating rate of 10 ℃/min, respectively, and calcined at that temperature for one hour to give a final black powdered solid sample (as shown in fig. 4 c).
Material shape and structure: the Ag-Co 3O4 metal nano composite material is nano flower-shaped particles with the size of 4.0-4.0 mu m, and silver atoms are uniformly distributed on the surfaces of the nano particles (see figure 1). By performing X-ray diffraction analysis (fig. 2) on the sample, the nanomaterial showed diffraction peaks at peak positions of 31.2 °, 36.8 °, 44.7 °, 55.5 °, 59.2 °, 65.1 ° corresponding to (220), (311), (400), (422), (511), (440) crystal planes of Co 3O4 crystals (PDF card: 078-1969). Since Ag is highly dispersed in Co 3O4, which results in low loading, no characteristic diffraction peak of Ag is observed in the figure.
2.2 Hydrogen production
10Mg of the Ag-Co 3O4 metal nanocomposite prepared by 2.1 is added as a catalyst sample into a 1 mol.L -1 NaOH aqueous solution, and the solution is fully dispersed in a solvent by ultrasonic treatment for 5 min. After that, 30.8mg (1 mmol) of ammonia borane complex was added. The hydrogen was collected with stirring by drainage. The test result shows that in the reaction of catalyzing the ammonia borane complex to hydrolyze to produce hydrogen by using the Ag-Co 3O4 catalyst, hydrogen is produced from 15s, 60mL of hydrogen is produced when the reaction time is 281s, and the final yield reaches 83%. FIG. 3 is a graph showing performance tests of an Ag-Co 3O4 catalyst for catalyzing hydrolysis of ammonia borane to produce hydrogen. This can be obtained using the following TOF calculation formula: the TOF value of the Ag-Co 3O4 catalyst was 347.85mol H2·mol-1Ag·min-1. The AB hydrolysis hydrogen production TOF (min -1) value was calculated using the following formula:
Wherein Deltan-corresponds to the difference in H 2 mass over time,
The time for t 50—H2 to reach 50mL,
The time for t 10—H2 to reach 10mL,
N M -amount of Ag material in the catalyst.
In addition, we synthesized Ni-Co 3O4 and AuCu-Co 3O4 catalyst. The method comprises the following specific steps: preparation of Ni-Co 3O4 catalyst: 20mg of Ni 6(SC2H4Ph)12 (preparation method is referred to as the following document ：Xiaoqi Chai,Tao Li,Mingyang Chen,Rongchao Jin,Weiping Ding,Yan Zhu,Suppressing the active site-blocking impact of ligands of Ni6(SR)12clusters with the assistance of NH3 on catalytic hydrogenation of nitriles,Nanoscale,2018,10,19375) to be dissolved in 1mL of dichloromethane, the solution is added dropwise to a uniformly dispersed ethanol solution containing 300mg of ZIF-67MOF material, the solution is stirred for 8 hours, the solution is centrifuged to obtain purple solid, the purple solid is dried at 60 ℃, and then the purple solid is placed in a calciner to be calcined at 500 ℃ for 1 hour, and finally the Ni-Co 3O4 catalyst is obtained.
The result shows that in the hydrolysis and hydrogen production reaction of ammonia borane complex by using Ni-Co 3O4 catalyst, hydrogen is produced only after 77s, the reaction time is 361s, 60mL of hydrogen is produced, and the final yield is 83%. Similarly, auCu-Co 3O4 catalyst preparation methods such as Ni-Co 3O4 preparation methods, auCu precursors from [Au4Cu5(Dppm)2(C6H11S)6]+[BPh4]-( preparation methods are referenced below ：Manman Zhou,Shan Jin,Xiao Wei,Qianqin Yuan,Shuxin Wang,Yuanxin Du,and Manzhou Zhu,Reversible Cu-S motif transformation and Au4 distortion via thiol ligand exchange engineering,The journal of physical chemistry C,2020,124,13,7531-7538). whereas AuCu-Co 3O4 catalysts do not exhibit catalytic activity in the hydrolysis of ammonia borane complexes to hydrogen.
In addition, the influence of the addition of different silver nitrate on the reaction activity of the Ag-Co 3O4 catalyst for catalyzing the hydrolysis of ammonia borane complex to produce hydrogen is compared. The preparation method is as follows, 2.1 and Ag-Co 3O4 preparation methods are adopted, but 0.02g of AgNO 3 in the reaction is respectively replaced by 0.01g of AgNO 3,0.04g AgNO3,0.06gAgNO3. In the hydrogen production experiment under the same conditions, namely 10mg of catalyst is taken and put into reaction, and other conditions are unchanged. As shown in FIG. 5, the test results show that the TOF value of the Ag-Co 3O4 catalyst prepared by adding 20mg of silver nitrate is optimal on the premise of being based on the silver standard. Other Ag-Co 3O4 catalysts prepared from 0.01gAgNO 3 were 280.22mol H2·mol-1 Ag·min-1 (the mass content of silver element in the catalyst was 0.8785%), 0.04g Ag-Co 3O4 catalyst prepared from AgNO 3 was 213.90mol H2·mol-1 Ag·min-1 (the mass content of silver element in the catalyst was 4.625%), and 0.06g Ag-Co 3O4 catalyst prepared from AgNO 3 was 113.24mol H2·mol-1 Ag·min-1 (the mass content of silver element in the catalyst was 6.316%).
The foregoing examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
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