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Preparation method and application of a chiral nano-gold photocatalyst
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A catalyst and nano-cerium oxide technology, applied in the field of photocatalysis, can solve the problems of low yield and the like, and achieve the effects of simple preparation method, good catalytic effect and high selectivity
Active Publication Date: 2020-11-06
HUNAN NORMAL UNIVERSITY
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It has been reported in China that lysine was used as a protective agent, cerium oxide was used as a carrier, and sodium borohydride was reduced to obtain relatively small-sized gold nanoparticles, which were applied to the reduction of acetophenone, but the yield was low
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Embodiment 1
[0027] After adding 10mL of distilled water to a 50mL round bottom flask, add 83μL of 97mmol / L chloroauric acid aqueous solution dropwise, and weigh 160mg of CeO 2 , poured into aqueous chloroauric acid solution, adjusted pH = 7 with 0.1M KOH solution, heated and stirred at 90°C for 2 hours, cooled, added dropwise sodium borohydride aqueous solution (0.08mmol sodium borohydride) for reduction, continued stirring for 1 hour, and centrifuged to obtain Purple-brown solid, washed three times with distilled water, dried under vacuum at 65°C for 12h to obtain Au@CeO 2 . Add 10 mL of anhydrous toluene to a 50 mL round bottom flask, add 0.5 mg of (1R,2R)-(-)-1,2-diphenylethylenediamine, and then add 50 mg of Au@CeO 2 , the mixture was stirred at 50 °C for 2 h, centrifuged, washed three times with toluene, and then vacuum-dried at 50 °C for 12 h to obtain purple-brown chiral Au@CeO 2 catalyst of light.
Embodiment 2
[0029] After adding 10mL of distilled water to a 50mL round bottom flask, add 166μL of 97mmol / L chloroauric acid aqueous solution dropwise, and weigh 160mg of CeO 2 , poured into aqueous chloroauric acid solution, adjusted pH = 7 with 0.1M KOH solution, heated and stirred at 90°C for 2 hours, cooled, added dropwise sodium borohydride aqueous solution (0.16 mmol sodium borohydride) for reduction, continued stirring for 1 hour, and centrifuged to obtain Purple-brown solid, washed three times with distilled water, dried under vacuum at 65°C for 12h to obtain Au@CeO 2 . Add 10 mL of anhydrous toluene to a 50 mL round bottom flask, add 1.0 mg of (1R,2R)-(-)-1,2-diphenylethylenediamine, and then add 50 mg of Au@CeO 2 , the mixture was stirred at 50 °C for 2 h, centrifuged, washed three times with toluene, and then vacuum-dried at 50 °C for 12 h to obtain purple-brown chiral Au@CeO 2 catalyst of light.
Embodiment 3
[0031] After adding 10mL of distilled water to a 50mL round bottom flask, add dropwise 250μL of 97mmol / L chloroauric acid aqueous solution, and weigh 160mg of CeO 2, poured into aqueous chloroauric acid solution, adjusted pH = 7 with 0.1M KOH solution, heated and stirred at 90°C for 2 hours, cooled, added dropwise sodium borohydride aqueous solution (0.24 mmol sodium borohydride) for reduction, continued stirring for 1 hour, and centrifuged to obtain Purple-brown solid, washed three times with distilled water, dried under vacuum at 65°C for 12h to obtain Au@CeO 2 . Add 10 mL of anhydrous toluene to a 50 mL round bottom flask, add 1.5 mg of (1R,2R)-(-)-1,2-diphenylethylenediamine, and then add 50 mg of Au@CeO 2 , the mixture was stirred at 50 °C for 2 h, centrifuged, washed three times with toluene, and then vacuum-dried at 50 °C for 12 h to obtain purple-brown chiral Au@CeO 2 catalyst of light.
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Abstract
The invention belongs to the technical field of photocatalysis, and relates to a preparation method of a chiral nanogold photocatalyst and application thereof. The preparation method comprises the following steps: (1), preparing Au@CeO2: adding a fixed amount of nanometer cerium oxide into a predetermined amount of aqueous chloroauric acid solution, adjusting the solution to neutrality, then heating, stirring for a predetermined time, then cooling, and then adding an aqueous sodium borohydride solution for reduction, centrifuging after completion of a reaction to obtain a solid product, washing and drying to obtain the Au@CeO2; (2), performing chiral modification: adding a (1R,2R)-(-)-1,2-diphenyldiethylamine chiral ligand and the Au@CeO2 prepared in the step (1) into methylbenzene according to a predetermined ratio, and reacting while stirring at a predetermined temperature, and centrifuging, washing and drying after completion of a reaction to obtain the chiral nanogold photocatalyst. The chiral nanogold photocatalyst prepared by the preparation method provided by the invention uses easily obtained raw materials, the preparation method is simple, and the prepared nanogold catalyst has a relatively good catalytic effect on hydrogenation reduction of acetophenone, successfully induces a reaction of the acetophenone to produce 1-phenylethanol and shows relatively high selectivity.
Description
technical field [0001] The invention belongs to the technical field of photocatalysis, and in particular relates to a preparation method and application of a chiral nano-gold photocatalyst. Background technique [0002] Nano-gold catalysts have superior catalytic effect in selective hydrogenation reaction, good catalytic activity and high product selectivity, making the preparation of highly dispersed nano-gold catalysts has attracted extensive attention of researchers. Many literature and patent studies have shown that when the nanometer size of gold nanoparticles is less than 10nm, it has higher catalytic activity, and the activity is linearly related to the size. The catalytic activity of nano-gold is limited by size, and it is easy to aggregate to form large particles during the preparation process, thereby reducing the catalytic activity. In order to inhibit the aggregation of nanoparticles, oxides and carbon materials are often used as carriers. Common methods include...
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