Preparation method of dibutoxy methane
A technology of dibutoxymethane and formaldehyde is applied in the field of preparation of industrial grade dibutoxymethane, which can solve the problems of high equipment requirements, cumbersome operation, influence on product stability, etc., and achieves low equipment corrosion, easy separation, Handling easy effects
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example 1
[0024] Preparation of activated carbon-supported acid catalyst: wash 50g of activated carbon with distilled water, dry it, activate it at 120°C for 2h, weigh 15g of pretreated activated carbon and immerse it in sulfuric acid with a mass concentration of 20 times of 60% by mass, and impregnate it at 120°C under stirring After 4 hours, filter with suction, wash until neutral, dry in an oven at 120°C to constant weight, and obtain 15 g of activated carbon-immobilized acid catalyst with an acid-immobilized capacity of 15% by mass after cooling, and set aside.
example 2
[0026] Wash 50g of activated carbon with distilled water, dry it, activate it at 120°C for 2h, weigh 15g of pretreated activated carbon and immerse it in 20 times the mass concentration of 98% by mass sulfuric acid, immerse it under stirring at 120°C for 4h, filter it with suction, and wash to medium properties, dried in an oven at 120°C to constant weight, and after cooling, 15 g of activated carbon-supported acid catalyst with an acid-loaded capacity of 22% by mass was obtained for future use.
example 3
[0028] Into a 500 mL three-neck flask equipped with a thermometer, a constant speed stirrer, and a water separator (with a condenser on the top), 78.4 g of a formaldehyde solution with a concentration of 37% by mass, 187.4 g of n-butanol, and 1.3 g of HZSM-5 catalyst were respectively added. , stirred and heated up, the initial reaction temperature was 90 °C, and the reaction was continuously raised until the reaction was completed at 130 °C, and the reaction time was 3 h; during the reaction process, the raw materials and by-product water were continuously separated from the reaction system through a water separator. After the reaction was completed, the reactant was filtered to obtain 196.5 g of a colorless crude product of dibutoxymethane, the content of dibutoxymethane was 58.7% according to gas chromatography, and the content of n-butanol was 33.3%; of dibutoxymethane.
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