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A pt@sio with yolk‑eggshell structure 2 Catalyst preparation method

A catalyst and eggshell technology, which is applied in the field of preparation of Pt@SiO2 catalysts 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, achieving excellent Hydrogenation activity, good cycle performance, short time-consuming effect

Inactive Publication Date: 2018-01-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, it has been reported that egg yolk-eggshell materials are used as carriers to support 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 reduce them into nanoparticles (Advanced Functional Materials , 2012, Volume 22, Page 591), although this method is simple, the reduction process is not easy to control, and the size of metal particles is difficult to control to the nanometer level with catalytic activity.

Method used

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  • A pt@sio with yolk‑eggshell structure <sub>2</sub> Catalyst preparation method
  • A pt@sio with yolk‑eggshell structure <sub>2</sub> Catalyst preparation method
  • A pt@sio with yolk‑eggshell structure <sub>2</sub> Catalyst preparation method

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Embodiment 1

[0038] The preparation method of mesoporous silica: Dissolve 0.1g CTAB in 45mL deionized water under stirring at 70°C, 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 was 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 ( Image 6 ). Its catalytic hydrogenation reaction activity is shown in Figure 8 .

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Abstract

The present invention relates to Pt@SiO 2 Catalyst and method for its preparation. Specifically, it is a Pt@SiO with a yolk-eggshell structure and a core containing Pt nanoparticles and organic functional groups. 2 nanospheres. Using mesoporous silica spheres as the core, adsorb Pt nanoparticles, add organosilane coupling agent under alkaline conditions, stir, filter, and dry to obtain silica nanospheres with a core-shell structure. The microenvironment inside the nanosphere can be hydrophilic, hydrophobic, superhydrophobic; the loading of Pt nanoparticles is adjustable in the range of 0.1%-5%; the distribution of Pt nanoparticles can be controlled on the inner core or in the cavity. The method is simple in steps, short in time, easy to adjust the loading capacity and composition of nanoparticles, and the prepared nanospheres have large specific surface area and pore volume; the particle size is uniform and the dispersion is good; the obtained material has excellent performance in the hydrogenation of cyclohexene It has good catalytic activity and can be recycled.

Description

technical field [0001] The invention relates to a Pt@SiO 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 the catalysis of gold nanoparticles, bulk gold has long been considered to be chemically inert, but the Japanese scholar Haruta (Journal of Catalysis, 1993, volume 144, page 175) found that when the particle size is reduced to 2 ~ 5nm, it shows very ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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