A kind of method for preparing diol
A technology of diol and ceria, which is applied in hydrolysis preparation, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of poor reaction selectivity and complicated preparation process, and achieve mild reaction conditions, simple preparation and high selectivity Effect
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Embodiment 1
[0016] Slowly add 7.3g ethyl orthosilicate dropwise to the solution of 12.8mL tetrapropylammonium hydroxide (20% aqueous solution) and 20mL water, stir vigorously at room temperature until clear, and dissolve 0.13g tetrabutyl titanate in After 6mL of isopropanol, under the protection of nitrogen, it was slowly added dropwise to the aforementioned sol, and stirred for about 1 hour. Add the above mixture into the synthesis kettle, seal it, and place it in an oven at 180°C for 6 hours; after the crystallization is completed, it is quenched, washed with deionized water repeatedly until neutral, dried, and roasted at 550°C for 8 hours to obtain TS-1. Get its Ti:Si=1%. It was immersed in cerium nitrate solution to prepare ceria-supported TS-1 with a ceria loading of 5 wt%. Add 2 mmol of allyl chloride and 0.02 g of catalyst into the reaction flask, add 2 mL of acetone and 1 mL of water, and react at 60 ° C for 20 h. The conversion rate of allyl chloride is 78% and the selectivity o...
Embodiment 2
[0018] Slowly add 9.0g ethyl orthosilicate dropwise into a solution of 16.0mL tetrapropylammonium hydroxide (20% aqueous solution) and 30mL water, stir vigorously at room temperature until clear, and dissolve 0.28g tetrabutyl titanate in After 10mL of isopropanol, under the protection of nitrogen, it was slowly added dropwise to the aforementioned sol, and stirred for about 1 hour. Add the above mixture into the synthesis kettle, seal it, heat it with microwave assistance to 150°C, and keep it for 3 hours; after the heating is completed, it is quenched, washed with deionized water repeatedly until neutral, dried, and calcined at 500°C for 4 hours to obtain TS-1. Its Ti:Si=1.8% was measured. It was immersed in europium nitrate solution, evaporated to dryness at 100°C, and calcined at 500°C for 2 hours to prepare TS-1 loaded with europium trioxide, and the loading amount of europium trioxide was 10wt%. Add 2mmol cyclohexene and 0.02g catalyst into the reaction flask, add 2mL ac...
Embodiment 3
[0020] Slowly add 7.3g ethyl orthosilicate dropwise to the solution of 12.8mL tetrapropylammonium hydroxide (20% aqueous solution) and 20mL water, stir vigorously at room temperature until clear, and dissolve 0.13g tetrabutyl titanate in After 6mL of isopropanol, under the protection of nitrogen, it was slowly added dropwise to the aforementioned sol, and stirred for about 1 hour. Add the above mixture into the synthesis kettle, seal it, and place it in an oven at 180°C for 6 hours; after the crystallization is completed, it is quenched, washed with deionized water repeatedly until neutral, dried, and roasted at 550°C for 8 hours to obtain TS-1. Get its Ti:Si=1%. It was immersed in a lanthanum nitrate solution to prepare TS-1 loaded with dilanthanum dioxide, and the loading amount was 5wt%. Add 2mmol chloropropene and 0.02g catalyst into the reaction flask, add 2mL acetone and 1mL water, and react at 60°C for 20h. Chromatography shows that the conversion rate of chloropropene...
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