Ester hydrogenation catalyst and preparation method and application thereof
A catalyst, a technology for ester hydrogenation, applied in the preparation of carboxylate, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of insufficient sensitivity to nucleophilic attack, loss of carrier, slow process of gel formation, etc. The effect of high directional selectivity, improved activity and stability, and simple preparation process
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Embodiment 1
[0027] Weigh 5.7g of copper nitrate trihydrate and 0.30g of silver nitrate, add ethanol and water to make a solution, then add 7.31g of ammonia water, stir evenly, and prepare solution I for use. Mix 32g ethyl orthosilicate and 1.5g pseudo-boehmite evenly, and then add ethanol to form solution II. Slowly add solution I dropwise to solution II, stirring continuously while adding dropwise, and continue stirring for 2 h after the dropwise addition is completed. Then crystallize at 120°C for 24h, wash, dry, and finally calcinate at 450°C for 24h to obtain the target catalyst.
[0028] Press the target catalyst into tablets, crush and sieve, take 20-40 mesh catalyst and put 2g of the target catalyst into the catalyst bed, raise it from room temperature to 300°C under hydrogen atmosphere, keep it for 12h, then drop it to 240°C, and then pass through acetic acid Methyl ester undergoes ester hydrogenation reaction, and the space velocity of methyl acetate ester liquid is 1.0h -1 , t...
Embodiment 2
[0030] Weigh 9.45g of copper nitrate trihydrate and 0.542g of silver nitrate, add ethanol and water to make a solution, then add 11.52g of ammonia water, stir evenly, and prepare solution Ⅰ for use. Mix 32g ethyl orthosilicate and 3.0g pseudo-boehmite evenly, and then add ethanol to form solution II. Slowly add solution I dropwise to solution II, stirring continuously while adding dropwise, and continue stirring for 4 hours after the dropwise addition is completed. Then it was crystallized at 120°C for 24h, washed, dried, and finally calcined at 500°C for 24h to obtain the target catalyst.
[0031] The target catalyst was pressed, crushed, and sieved, and 2g of the target catalyst of 20-40 mesh was loaded into the catalyst bed. Under the conditions of 3.5MPa, liquid hourly space velocity 1.2h-1, and hydrogen-to-ester ratio of 150, dimethyl oxalate is used as raw material and methanol is used as solvent. The conversion rate of dimethyl oxalate is greater than 99.9%, and the s...
Embodiment 3
[0033]Weigh 1.89g of copper nitrate trihydrate and 1.16g of silver nitrate, add ethanol and water to make a solution, then add 1.65ml of hydrochloric acid with a concentration of 1mol / l and 3.47g of ammonia water, stir well, and prepare solution I for use. Mix 18g ethyl orthosilicate and 7.15g pseudo-boehmite evenly, then add ethanol to form solution II. Slowly add solution I dropwise to solution II, stirring continuously while adding dropwise, and continue stirring for 2 h after the dropwise addition is completed. Then it was crystallized at 120°C for 24h, washed, dried, and finally calcined at 500°C for 24h to obtain the target catalyst.
[0034] The target catalyst was pressed into tablets, crushed and sieved, and 2g of the 20-40 mesh catalyst was loaded into the catalyst bed, raised from room temperature to 260°C under a hydrogen atmosphere, kept at normal pressure for 10 hours, and then lowered to 200°C. Under the conditions of 2.5MPa, liquid hourly space velocity 1.0h-1...
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