A method for preparing dimethyl 1,4-cyclohexanedicarboxylate by ruthenium-rhenium bimetallic catalyzed hydrogenation of dimethyl terephthalate
A technology of dimethyl cyclohexanedicarboxylate and dimethyl phthalate, which is applied in the preparation of carboxylate, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of catalyst preparation The process is complicated and tedious, the reaction temperature is high, and it is unfavorable for industrial application. It achieves the effects of high practicability and economy, high catalytic efficiency and high selectivity.
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Embodiment 1
[0014] Example 1: Preparation of 5% Ru / C, 5% Re / C catalysts by equal impregnation method. Weigh 0.1026gRuCl 3 , 0.0720gNH 4 ReO 4 Add 1.2ml of deionized water to dissolve, then add to 1g of activated carbon, mix evenly, soak at room temperature overnight, then dry, transfer to a blast drying oven for 4 hours at 110°C, and finally reduce under hydrogen at 460°C for 3 hours, That is, a 5% Ru / C, 5% Re / C catalyst is prepared.
Embodiment 2
[0015] Embodiment 2: Preparation of 5% Ru by equal impregnation method 0.83 Re 0.17 / C, 5% Ru 0.75 Re 0.25 / C, 5% Ru 0.5 Re 0.5 / C, 5% Ru 0.25 Re 0.75 / C, 5% Ru 0.17 Re 0.83 / C Catalyst. On the basis of the total metal loading of 5wt%, according to the Ru, Re metal molar ratio of 0.83:0.17, 0.75:0.25, 0.5:0.5, 0.25:0.75, 0.17:0.83 respectively weigh the required RuCl 3 and NH 4 ReO 4 Add 1.2ml of deionized water to dissolve, then add to 1g of activated carbon, mix well, soak overnight at room temperature, then dry, transfer to a blast drying oven for 4 hours at 110°C, and finally reduce under hydrogen at 460°C for 3 hours, that is 5% Ru 0.83 Re 0.17 / C, 5% Ru 0.75 Re 0.25 / C, 5% Ru 0.5 Re 0.5 / C, 5% Ru 0.25 Re 0.75 / C, 5% Ru 0.17 Re 0.83 / C Catalyst.
Embodiment 3
[0016] Embodiment 3: add 0.5g dimethyl terephthalate, 20g ethyl acetate, 0.125g5%Ru / C catalyst in reactor. After the reactor was sealed and ventilated, it was filled with 3MPa hydrogen and reacted at 70°C for 3 hours. After the reaction was completed, the samples were taken at room temperature, and sent to gas phase detection after centrifugal filtration and other treatments. The experimental results are shown in No. 1 in Table 1.
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