Abstract
Bi(NO3)3·5H2O and (NH4)6Mo7O24·4H2O were used as precursors to synthesize flaky γ-Bi2MoO6 samples by a hydrothermal method, and Pt/γ-Bi2MoO6 samples with different mass fractions were prepared by an NaBH4 reduction method. Alpha alkylation of benzyl alcohol and acetophenone with photocatalysts under visible light irradiation was performed, and the activity of 4 wt % Pt/γ-Bi2MoO6 (γ-Bi2MoO6 was prepared by a nitric acid method, pH = 9, and reaction temperature 180 °C) was the best. The photocatalytic reaction conditions were optimized by changing various kinds of variables, such as the type of catalyst, solvent, and base, and the amount of base, catalyst, and reactant. The optimal conditions for the organic reaction were 75 mg 4 wt % Pt/γ-Bi2MoO6, 6 mL n-heptane, 1.2 mmol NaOH, 1 mmol acetophenone, and 3 mmol benzyl alcohol. Under the optimal reaction conditions, the effects of different light wavelengths and light intensities on the reaction were measured, and the cycling ability of the photocatalyst was tested. After five cycles, the photochemical properties of the catalyst were relatively stable. Finally, the active substances were identified (such as electrons (e−), holes (h+), hydroxyl radicals (•OH), and superoxide radicals (•O2−).
Highlights
Dehydration of an alpha alkylation reaction is one of the most important methods to build C=C bonds
Benzyl alcohol was used as an alkylating agent, and an alkyl group was introduced onto acetophenone to construct C=C bonds and to synthesize 1,3-diphenyl-2-propen-1-one
Among the different preparation methods, γ-Bi2MoO6 prepared by the nitric acid method was more conducive to the α-alkylation of benzyl alcohol and acetophenone (Table 2, No 1–3)
Summary
Dehydration of an alpha alkylation reaction is one of the most important methods to build C=C bonds It is significant in organic synthesis and industrial production. Traditional alkylation [1] is the reaction of organic compounds with halo-hydrocarbons and their derivatives This method has a high yield, the required temperature is high, and there are many byproducts. Each crystal form has its own structure and property, with γ-Bi2MoO6 demonstrating a strong photoelectric effect and a wide range of visible light absorption [11]. Bi2MoO6 has good application prospects under visible light irradiation, it has many shortcomings, such as low photogenerated electron mobility and high photoelectron and hole recombination ability. A hydrothermal method to synthesize flaky γ-Bi2MoO6 and to load precious metals on its surface is applied to improve photocatalytic activities. When the loading of Pt is too high, electrons and holes will be recombined rapidly [28], which is not conducive to the α-alkylation reaction
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