Preparation method of 3,5-dimethoxy phenylcarbinol
A technology of dimethoxybenzyl alcohol and methyl dimethoxybenzoate, which is applied in the field of preparation of 3,5-dimethoxybenzyl alcohol, can solve the problem of large amount of "three wastes" that are difficult to industrialize and operate Complicated and other issues, to achieve the effect of easy industrial production, high reactivity, and stable reaction performance
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[0037] The preparation method of 3,5-dimethoxybenzyl alcohol comprises the steps:
[0038] a. Acidify the silica sol with dilute nitric acid, and then ultrasonically treat it for 5-60 minutes to obtain a modified silica sol carrier.
[0039] b. Add the modified silica sol carrier prepared in step a to urea and copper nitrate to prepare an aqueous solution, stir for 1-10 hours, then raise the temperature to 50-98°C, stir for 10-28 hours, and filter out the solid while it is hot , washed the solid with deionized water.
[0040] c. Dry the solid obtained in step b at 90-120° C. for 6-12 hours, and then roast at 200-400° C. for 2-6 hours to obtain a grass-green solid.
[0041] d. The grass-green solid obtained in step c is subjected to on-line reduction and activation of the catalyst at a normal pressure of 150-300° C. with a hydrogen flow rate of 60-150 mL / min to obtain the copper-containing catalyst; oxidation state The catalyst does not have catalytic activity and must underg...
Embodiment 1
[0054] a. Add 60 grams of silica sol to 150 milliliters of 0.01 mol / L dilute nitric acid, and treat with ultrasonic waves for 40 minutes.
[0055] b. Add 20 grams of copper nitrate and 20 grams of urea into a 1-liter reaction bottle, then add 300 milliliters of deionized water into the bottle, stir to dissolve and clarify, and then use the modified silicon prepared in step (a) The sol was added to the prepared mixed solution of copper nitrate and urea, and after stirring at room temperature for 4 hours, the reaction bottle was heated to 90°C and stirred at this temperature for 14 hours; filtered while it was hot, and deionized with 200 ml The solid was washed with water.
[0056] c. Dry the solid obtained in step (b) at 100°C for 8 hours, and then roast it in a muffle furnace at 300°C for 3 hours to obtain a grass-green solid.
[0057] d. The grass-green solid obtained in step (c) is subjected to online reduction and activation of the catalyst under normal pressure and a hydr...
Embodiment 2
[0060] a. Add 60 grams of silica sol to 150 milliliters of 0.005 mol / L dilute nitric acid, and use ultrasonic treatment for 30 minutes.
[0061] b. Add 15 grams of copper nitrate and 15 grams of urea into a 1-liter reaction bottle, then add 250 milliliters of deionized water into the bottle, stir to dissolve and clarify, and then use the modified silicon prepared in step (a) The sol was added to the prepared mixed solution of copper nitrate and urea, and after stirring at room temperature for 4 hours, the reaction flask was heated to 70°C and stirred at this temperature for 14 hours; filtered while hot, and deionized with 200 ml The solid was washed with water.
[0062] c. Dry the solid obtained in step (b) at 110°C for 6 hours, and then roast it in a muffle furnace at 350°C for 2 hours to obtain a grass-green solid.
[0063] d. The grass-green solid obtained in step (c) is subjected to online reduction and activation of the catalyst under normal pressure and a hydrogen flow ...
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