A kind of titanium/palladium composite catalyst, preparation method and its application in acetone hydrogenation reaction
A composite catalyst, titanium dioxide technology, applied in the direction of physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, carbon-based compound preparation, etc., can solve the problem that the activity and selectivity cannot meet the requirements of industrialization
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Embodiment 1
[0056] Step (1): Fluorine modification of mesoporous silica
[0057] Immerse 5.0 g of 40-60 mesh commercial mesoporous silica in 224 mL of 0.5 mol / L hydrofluoric acid aqueous solution, sonicate for 0.5 h, and dry overnight at 110°C to obtain fluorine-modified mesoporous silica. Elemental analysis indicated 1.6 wt% fluorine doping; labeled as SiO 2 (B-F1.6).
[0058] Step (2):
[0059] Step (2-a): supporting titanium dioxide on fluorine-modified mesoporous silica (preparation of supported titanium dioxide component)
[0060] At room temperature, mix 10mL of tetra-n-butyl titanate and 35mL of absolute ethanol in a closed flat-bottomed three-neck flask, stir vigorously for 30min, then take 20mL of glacial acetic acid, 1mL of absolute ethanol, and 0.2mL of distilled water to mix evenly, and add to the above mixture solution, stirred vigorously for 1 h. At this point, a clear transparent golden yellow solution was obtained, and 5 g of fluorine-modified mesoporous silica (SiO 2...
Embodiment 2
[0082] Step (1): Fluorine modification of mesoporous silica
[0083] Immerse 5.0 g of 40-60 mesh commercial mesoporous silica in 224 mL of 0.25 mol / L hydrofluoric acid aqueous solution, sonicate for 0.5 h, and dry at 110°C overnight. Fluorine-modified silica was obtained, elemental analysis showed that the fluorine doping amount was 0.65wt%, marked as SiO 2 (B-F-0.65).
[0084] Step (2):
[0085] Step (2-a): supporting titanium dioxide on fluorine-modified mesoporous silica (preparation of supported titanium dioxide component)
[0086] At room temperature, mix 10mL of tetra-n-butyl titanate and 35mL of absolute ethanol in a closed flat-bottomed three-neck flask, stir vigorously for 30min, then take 20mL of glacial acetic acid, 1mL of absolute ethanol, and 0.2mL of distilled water, mix well, and add to the above mixture solution, stirred vigorously for 1 h. At this point, a clear transparent golden yellow solution was obtained, and 5 g of fluorine-modified mesoporous silica...
Embodiment 3
[0093] Compared with Example 2, the difference is that in step (1), the concentration of the hydrofluoric acid aqueous solution used is 1.5mol / L, and the fluorine doping amount of the fluorine-modified silica after the step (1) is completed 2.2wt%, marked as SiO 2 (B-F-2.2).
[0094] The TiO obtained by fluorine-modified silica through step (2-a) 2 product, labeled TiO 2 / SiO 2 (B-F2.2); TiO 2 The loading was 2.24 wt%. After the step (3), the mixed catalyst of supported titanium dioxide and supported palladium is marked as TiO 2 / SiO 2 (B-F2.2) & Pd / Cor, TiO 2 The mass ratio to Pd is 36. TiO 2 / SiO 2 (B-F2.2) & Pd / Cor acetone catalytic activity results are shown in Table 2.
[0095] Embodiment 1, embodiment 2, embodiment 3 and comparative example 4 probed into the fluorine doping amount, palladium particle size on the influence of catalyst in acetone hydrogenation synthesis MIBK catalytic performance, the catalytic acetone hydrogenation of each embodiment and compar...
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