A preparing method of a Pt@SiO2 catalyst having a yolk-eggshell-type structure

A catalyst and eggshell technology, which is applied in the field of preparation of PtSiO2 catalyst with egg yolk-eggshell structure, can solve the problems that the size of metal particles is difficult to control to the nanometer level with catalytic activity, and the reduction process is not easy to control, so as to achieve excellent hydrogenation Activity, good recycling performance, good dispersion effect

Inactive Publication Date: 2016-05-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

At present, it has been reported that egg yolk-eggshell materials are used as carriers to carry nanoparticles. The commonly used method in the literature is to impregnate and adsorb metal salt precursors with the synthesized egg yolk-eggshell materials, and then redu

Method used

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  • A preparing method of a Pt@SiO2 catalyst having a yolk-eggshell-type structure
  • A preparing method of a Pt@SiO2 catalyst having a yolk-eggshell-type structure
  • A preparing method of a Pt@SiO2 catalyst having a yolk-eggshell-type structure

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Embodiment 1

[0038] The preparation method of mesoporous silica: under stirring at 70°C, dissolve 0.1g CTAB in 45mL deionized water, add 0.35mL NaOH (2M), and stir for 0.5h. Add 0.3mL of trimethylbenzene, sonicate for 1h to form a white emulsion. Under stirring, add 0.5mLTEOS, add 0.4mL ethyl acetate after precipitation, and stir for 1-2h. The mixture was transferred to a crystallization kettle and crystallized at 100°C for 24h. After cooling, the product was filtered with suction, washed with water and ethanol, and after drying, it was stirred with an absolute ethanol solution containing ammonium nitrate at 60°C for 0.5h, filtered with suction, washed with alcohol, and dried to obtain a white light powder (hydrophilic Materials, the ratio of benzene to water is 0.3, Chemical Communication, 2014, volume 50, page 10830).

[0039] 80mg of the above-mentioned mesoporous silica material is dispersed in 4mL of Pt nanoparticle aqueous solution, and ultrasonically adsorbed for 1-3h. Electron m...

Embodiment 2

[0041] The preparation process of Example 1 is adopted, and the difference is that the amount of adding the nanoparticle aqueous solution is 20 mL, without dilution. Electron microscope pictures show that the nanoparticles are evenly distributed on the inner core ( Figure 5 ). ICP characterizes that the metal content is 5% (mass fraction).

Embodiment 3

[0043] The preparation method of mesoporous silica: adopt the preparation process of Example 1, the difference is that, add 0.5mLTEOS, 0.4mL ethyl acetate, add 0.33mL propyltrichlorosilane after 5-10 minutes, and get the inner core as propyl (Propyl) modified mesoporous silica spheres. (hydrophobic material, benzene-to-water ratio is 1.8, Chemical Communication, 2014, volume 50, page 10830).

[0044] The preparation method of the egg yolk eggshell structure catalyst is the same as in Example 1. Electron microscope pictures show that the obtained product is a silica pellet with egg yolk-eggshell type. Pt nanoparticles are distributed in the inner core and cavity, with good dispersion and uniform particle size, with a size of about 2.3nm ( Figure 6 ). Its catalytic hydrogenation reaction activity is shown in Figure 8 .

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Abstract

The invention relates to a Pt@SiO2 catalyst and a preparing method thereof, particularly a Pt@SiO2 nanosphere having a yolk-eggshell-type structure and having a core containing Pt nano particles and organic functional groups. A silica nanosphere having a core-shell structure is prepared by adopting a mesoporous silica sphere as an inner core and by adsorbing the Pt nano particles, adding an organosilane coupling agent under alkaline conditions, stirring, filtering and drying. The microenvironment in the nanosphere can be hydrophilic, hydrophobic and super-hydrophobic. The loading amount of the Pt nano particles is adjustable in a range of 0.1-5%. Distribution of the Pt nano particles can be controlled on the inner core or a cavity. The method is characterized by simple steps, short time, and easily adjustable loading amounts and composition of the nano particles. The prepared nanosphere is high in specific surface area and pore volume, uniform in particle size and good in dispersity. The prepared catalyst shows good catalytic activity in cyclohexene hydrogenation and can be recycled.

Description

technical field [0001] The invention relates to a PtSiO with egg yolk-eggshell structure 2 Catalyst and method for its preparation. Specifically, it is a nanosphere catalyst with an egg yolk eggshell structure, an adjustable internal microenvironment of the catalyst, and loaded with Pt nanoparticles and a preparation method thereof. Background technique [0002] When the particle size of the metal particles is as small as the nanometer size, due to the quantum effect, the quasi-continuous energy level of the original bulk metal will be discrete, which will affect the coordination field environment of the surface atoms of the nanoparticles, resulting in changes in the properties of the nanoparticles. The most famous example is gold nanoparticle catalysis, bulk gold has long been considered chemically inert, but Japanese scholar Haruta (Journal of Catalysis, 1993, volume 144, page 175) found that when the particle size is reduced to 2~ When it is 5nm, it shows very excellent...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J35/10C07C5/03C07C13/18
CPCY02P20/55
Inventor 杨启华彭娟
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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