Alcohol oxidation aldehyde ketone production applied novel catalyst and preparation method thereof
A catalyst and alcohol oxidation technology, which is applied in the preparation of organic compounds, oxidation of carbonyl compounds, physical/chemical process catalysts, etc., can solve the problems of low utilization rate of oxidant atoms, large amount of three wastes, heavy pollution, etc., and achieve reusability Good, easy-to-separate, source-rich effects
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[0022] A preparation method for a novel catalyst for alcohol oxidation to produce aldehydes and ketones, said preparation comprising the steps of:
[0023] (1) Prepare a mixed colloidal aqueous solution of magnesium oxide, aluminum oxide and carbonate, the molar ratio of magnesium and aluminum content is 2.0-5.0, the total ion concentration of magnesium and aluminum is 2.0-5.0 mol / L; carbonate and oxide The molar amount of aluminum is the same; after stirring vigorously at room temperature for 1 to 6 hours, place it in a crystallization kettle at 60 to 120 ° C for 6 to 24 hours, then filter or centrifugally dehydrate the obtained colloid, wash with water until neutral, 60 ~100°C drying, the obtained solid sample is calcined at 200~400°C for 4~16 hours to obtain the corresponding magnesium-aluminum composite oxide; the carbonate is one of ammonium carbonate, sodium carbonate, and potassium carbonate ;
[0024] (2) Prepare the colloidal aqueous solution of 40-600 mesh magnesium...
Embodiment 1
[0029] 2 mol MgO, 1 mol Al 2 o 3 and 1 mol of sodium carbonate with deionized water to make 1.5 L of colloid; vigorously stirred at room temperature for 1.0 hour, placed in a crystallization kettle for 6 hours to crystallize at 60 °C, filtered, washed with water until neutral, and dried at 60 °C to obtain The solid sample was calcined at 200 °C for 4 hours to obtain the corresponding magnesium-aluminum composite oxide; it was ground into a 40-mesh powder and placed in water, and NH 4 The pH value was controlled by OH to be 9.0, aged under vigorous stirring at 40 °C for 12 hours, filtered, washed with water until neutral, and dried at 60 °C to obtain the carrier magnesium-aluminum hydrotalcite compound. Take 0.1 mol of ligand L1 and dissolve it in 100 mL of dichloromethane, add 100 mL of concentrated sulfuric acid and 300 mL of oleum dropwise at the same time, react at room temperature for 24 hours, add 500 g of ice-water mixture, and use 6 mol / L neutralized NaOH solution to ...
Embodiment 2
[0031] 6 mol MgO, 1.2 mol Al 2 o 3 and 1.2 mol of sodium carbonate with deionized water to prepare 1.5 L of colloid; vigorously stirred at room temperature for 6.0 hours, placed in a crystallization kettle for 24 hours at 120°C to crystallize, filtered, washed with water until neutral, and dried at 100°C to obtain The solid sample was calcined at 400 °C for 16 hours to obtain the corresponding magnesium-aluminum composite oxide; it was ground into a 600-mesh powder and placed in water, the pH value was adjusted to 11.0 with sodium hydroxide, and the aging was vigorously stirred at 80 °C for 36 hours. Filter, wash with water until neutral, and dry at 100°C to obtain a carrier magnesium-aluminum hydrotalcite compound. Take 0.1 mol of ligand L2 and dissolve it in 100 mL of dichloromethane, add 100 mL of concentrated sulfuric acid and 300 mL of oleum dropwise at the same time, react at room temperature for 24 hours, add 500 g of ice-water mixture, and use 6 mol / L The NaOH soluti...
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