Preparation and application of hierarchical pore catalyst for in-situ encapsulation of nano noble metal
A precious metal, multi-level pore technology, applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, preparation of amino compounds, etc., can solve the problem of low stability, difficult to control the size of metal nanoparticles, easy to block problems such as pores, to achieve the effects of good adsorption performance, simple preparation method and improved efficiency
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Embodiment 1
[0029] Embodiment 1 A kind of preparation method of the hierarchical porous catalyst of in-situ encapsulation nano noble metal palladium
[0030] The specific steps of the preparation method are as follows:
[0031] (1) Dissolve 0.15g of cetyltrimethylammonium bromide in 30mL of distilled water, then add 4mL of o-dichlorobenzene and 15mL of isopropanol, and use ammonia water to adjust the pH of the mixture to 10;
[0032] (2) Add 0.5mL tetraethoxysilane and 2mL sodium chloropalladate tetrahydrate solution with a concentration of 10mM to the above mixed solution, and stir (stirring speed is 1000rpm) for 3 hours;
[0033] (3) Centrifuge and dry the mixed solution after stirring, place the product in the air at 550°C for 3 hours, and then calcinate it in hydrogen at 200°C for 1 hour to obtain a hierarchical porous catalyst that encapsulates nano-noble palladium in situ , that is, in situ encapsulation of Pd@hierarchical porous catalysts.
[0034] Scanning electron microscope (S...
Embodiment 2
[0035] Example 2 A preparation method of a hierarchically porous catalyst that encapsulates nanoscale precious metal platinum in situ
[0036] The specific steps of the preparation method are as follows:
[0037] (1) Dissolve 0.15g of cetyltrimethylammonium bromide in 30mL of distilled water, then add 4mL of o-dichlorobenzene and 15mL of isopropanol, and use ammonia water to adjust the pH of the mixture to 10;
[0038] (2) Add 0.5mL tetraethoxysilane and 1mL chloroplatinic acid hexahydrate solution with a concentration of 10mM to the above mixed solution, and stir (stirring speed is 1000rpm) for 3 hours;
[0039] (3) Centrifuge and dry the stirred mixed solution, place the product in 550°C air for 3 hours, and then calcine in 200°C hydrogen for 1 hour to obtain a hierarchically porous catalyst for in-situ encapsulation of nano-noble metal platinum , that is, in situ encapsulation of Pt@hierarchical porous catalysts.
[0040] The results of scanning electron microscopy and tr...
experiment example 1
[0053] Experimental example 1 Hierarchical porous catalyst of the present invention is to the hydrogenation catalytic reaction of nitrobenzene
[0054] Take 20 mg of catalyst (the hierarchical porous catalyst in Examples 1 and 2 and Comparative Examples 1 and 2) and disperse it in 10 mL of water, then add 0.3 mmol of nitrobenzene, 10 μL of dodecane, and 10 mg of sodium borohydride, and centrifuge after 1 h. The organic phase solution was taken to detect the product by gas chromatography. As can be seen from Table 1, the metal hierarchical porous catalyst (embodiment 1, 2) prepared by in-situ encapsulation has a hydrogenation conversion rate of nitrobenzene greater than 99%, and simultaneously has 100% selectivity to the ideal product aniline, However, the metal hierarchical porous catalysts prepared by the impregnation method (Comparative Examples 1 and 2) have significantly lower conversion rates for the hydrogenation of nitrobenzene, and are more likely to produce by-product...
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