Copper-based catalyst for preparing ethylene glycol and ethylene glycol monomethyl ether by hydrogenation of dimethyl oxalate and preparation method thereof
A technology of ethylene glycol monomethyl ether and dimethyl oxalate, which is applied to the preparation of hydroxyl compounds, dehydration of hydroxyl-containing compounds to prepare ethers, ether preparations, etc., can solve the problems of not being able to directly obtain ethylene glycol monomethyl ether, and achieve excellent Hydrogenation activity and selectivity of ethylene glycol monomethyl ether, enhanced activity and stability, effect of high specific surface area
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Embodiment 1
[0023] Zirconia preparation: Dissolve 1.80g of zirconium oxychloride in an appropriate amount of ethanol. After fully dissolving, add 1.00g of hexagonal mesoporous molecular sieve HMS. After fully grinding in an agate mortar, add 150mL of ethanol, place in a round bottom flask and heat to reflux for 24 hours. After filtration, wash, dry at 100°C, gradually raise the temperature to 650°C at 2°C / min, and bake at this temperature for 20 hours. The carrier containing the template agent obtained in the previous step was dissolved in 2M NaOH solution to remove the silicon template, and dried to obtain zirconia.
[0024] Carrier modification and metal loading: 50ml of 0.02M H 2 SO 4 Aqueous solution, add dropwise to 50ml aqueous solution containing 2g zirconia at a constant speed, stir at 20°C for 4h, raise the temperature to 90°C and continue stirring until the solvent evaporates completely, bake at 120°C for 12h, heat up to 300°C in a muffle furnace at 5°C / min Keep at ℃ for 4h...
Embodiment 2
[0027] The preparation of zirconia is the same as in Example 1.
[0028] Carrier modification and metal loading:50ml of 0.08M H 2 SO 4 Aqueous solution, add dropwise to 50ml aqueous solution containing 2g zirconia at a constant speed, stir at 40°C for 4h, raise the temperature to 90°C and continue stirring until the solvent evaporates completely, bake at 110°C for 12h, heat up to 400°C in a muffle furnace at 5°C / min Keep at ℃ for 4h to get the carrier, denoted as S-ZrO 2 -2#. 12.08gCu(NO 3 ) 2· 3H 2 O, 7.53gMn(NO 3 ) 2 4H 2 O dissolved in 100ml H 2 O is made into a metal ion solution, the pH of the suspension is adjusted to 11~12 with ammonia water, stirred and reacted in a water bath at 40°C for 5 hours, and the solution containing S-ZrO is added dropwise at a uniform speed. 2 -Aqueous solution of 2# carrier. Continue to stir for 4 hours after the dropwise addition, increase the temperature of the water bath, and continue to stir and react at 80°C until the pH ...
Embodiment 3
[0031] The preparation of zirconia is the same as in Example 1.
[0032] Carrier modification and metal loading: 50ml of 0.20M H 2 SO 4 Aqueous solution, add dropwise to 50ml aqueous solution containing 2g zirconia at a constant speed, stir at 40°C for 3h, raise the temperature to 80°C and continue stirring until the solvent evaporates completely, bake at 140°C for 14h, heat up to 500°C at 10°C / min in the muffle furnace Keep at ℃ for 4h to get the carrier, denoted as S-ZrO 2 -3#. 9.66gCu(NO 3 ) 2· 3H 2 O, 5.02gMn(NO 3 ) 2 4H 2 O dissolved in 100ml H 2 O is made into a metal ion solution, the pH of the suspension is adjusted to 10~11 with ammonia water, stirred and reacted in a water bath at 45°C for 5 hours, and the solution containing S-ZrO is added dropwise at a uniform speed. 2 -Aqueous solution of 3# carrier. Continue to stir for 6 hours after the dropwise addition, increase the temperature of the water bath, and continue to stir the reaction at 80°C until t...
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