Cu catalyst for liquid-phase selective hydrogenation of crotonaldehyde and preparation method thereof
A crotonaldehyde and selectivity technology is applied in the field of Cu catalyst for selective hydrogenation of crotonaldehyde in liquid phase to generate crotyl alcohol and the field of preparation thereof, which can solve the problem of high cost of precious metal catalysts, and achieves the improvement of electron cloud density, and the operation method is simple and good. Active and selective effects
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Embodiment 1
[0024] (1) Preparation of S-TiO using thiourea as sulfur source 2 carrier:
[0025] ① Prepare a mixed solution of 1.34g thiourea, 10ml glacial acetic acid and 20ml ethanol.
[0026] ② Dissolve 6.0 g of tetrabutyl titanate in 30 ml of ethanol, stir evenly, and add dropwise to ①. The temperature was raised to 50°C, and the solution was stirred at a constant temperature until the solution became slurry.
[0027] ③The slurry was dried at 60°C for 24h and calcined at 500°C for 3h to obtain the carrier S-TiO 2 , the S in the support accounts for S-TiO 2 3% of the total mass of the carrier.
[0028] (2) Prepare Cu(NO) with a concentration of 0.06g / ml 3 ) 2 solution. Take 3.15ml of Cu(NO 3 ) 2 Add 0.95g S-TiO to the solution 2 In the carrier, after stirring evenly, soak it at room temperature for 12 hours;
[0029] (3) The liquid was evaporated to dryness at 100°C, dried at 120°C for 8 hours, and ground into powder. After calcination at 500°C for 4h, a powder solid was obt...
Embodiment 2
[0033] (1) Preparation of S-TiO using thiourea as sulfur source 2 carrier:
[0034] ① Prepare a mixed solution of 1.34g thiourea, 10ml glacial acetic acid and 20ml ethanol.
[0035] ② Dissolve 6.0 g of tetrabutyl titanate in 30 ml of ethanol, stir evenly, and add dropwise to ①. The temperature was raised to 50°C, and the solution was stirred at a constant temperature until the solution became slurry.
[0036] ③The slurry was dried at 60°C for 24h and calcined at 500°C for 3h to obtain the carrier S-TiO 2 . S in the carrier accounts for S-TiO 2 3% of the total mass of the carrier.
[0037] (2) Prepare Cu(NO) with a concentration of 0.06g / ml 3 ) 2 solution. Take 6.3 ml of Cu(NO 3 ) 2 Add 0.9g S-TiO to the solution 2 In the carrier, after stirring evenly, soak it at room temperature for 12 hours;
[0038] (3) The liquid was evaporated to dryness at 100°C, dried at 120°C for 8 hours, and ground into powder. After calcination at 500°C for 4h, a powder solid was obtaine...
Embodiment 3
[0042] (1) Preparation of S-TiO using thiourea as sulfur source 2 carrier:
[0043] ① Prepare a mixed solution of 1.34g thiourea, 10ml glacial acetic acid and 20ml ethanol.
[0044] ② Dissolve 6.0 g of tetrabutyl titanate in 30 ml of ethanol, stir evenly, and add dropwise to ①. The temperature was raised to 50°C, and the solution was stirred at a constant temperature until the solution became slurry.
[0045] ③The slurry was dried at 60°C for 24h and calcined at 500°C for 3h to obtain the carrier S-TiO 2 . S in the carrier accounts for S-TiO 2 3% of the total mass of the carrier.
[0046] (2) Prepare Cu(NO) with a concentration of 0.06g / ml 3 ) 2 solution. Take 12.6ml of Cu(NO 3 ) 2 Add 0.8g S-TiO to the solution 2 In the carrier, after stirring evenly, soak it at room temperature for 12 hours;
[0047](3) Evaporate the liquid at 100°C, dry at 120°C for 8 hours, and grind into powder. Calcined at 500°C for 4h to obtain powder solid
[0048] (4) The obtained powder...
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