Catalyst start-up method
A catalyst, copper catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of low selectivity of ethylene glycol
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Embodiment 1
[0023] Catalyst preparation:
[0024] Take by weighing 200 grams of a silicon oxide carrier with a specific surface area of 280 square meters per gram, configure the catalyst according to the content of 35 parts of active metal copper and 10 parts of metal zinc, the steps are as follows: select copper nitrate, and zinc nitrate, according to Cu and Zn loading Prepare an impregnating solution, impregnate the silicon oxide carrier in the solution for 18 hours, and then vacuum-dry at room temperature for 10 hours to obtain a solid. The solid was then dried at 120°C for 10 hours and calcined at 450°C for 4 hours to obtain the required 30%CuO+10%ZnO / SiO 2 catalyst precursor.
[0025] Weigh the prepared 30%CuO+10%ZnO / SiO 2 The catalyst precursor is 50 grams, which is loaded into a tubular reactor with a diameter of 18 mm, and hydrogen is used as the reducing gas. At a volumetric space velocity of 2000 hours -1 , the reduction pressure is 0.5MPa, and the reduction temperature is 3...
Embodiment 2
[0027] Adopt the same catalyzer of embodiment 1, just the reduction condition of catalyzer is that the volume space velocity is 3500 hours -1 , the reduction pressure is 2.5MPa, and the reduction temperature is 200°C. After 8 hours of reduction, the temperature is lowered to 185°C in a hydrogen atmosphere. At a pressure of 2.5MPa, the weight space velocity of dimethyl oxalate is 0.8 hours. -1 , under the condition that the hydrogen ester molar ratio is 80:1, dimethyl oxalate is put into the reactor, and after being stable for 18 hours, the temperature is raised to the normal reaction temperature of the catalyst at 200°C to continue the reaction. During the whole reaction process, the conversion of dimethyl oxalate The ratios are all 100%, and the selectivity of ethylene glycol is 95.8%.
Embodiment 3
[0029] Prepare 40%CuO+8%ZnO+0.2%CeO according to the various steps and conditions of Example 1 2 / SiO 2 The catalyst precursor is loaded into the reactor with the same loading amount, and the reduction condition of the catalyst is that the volume space velocity is 1000 hours -1 , the reduction pressure is 1.5MPa, and the reduction temperature is 250°C. After reduction for 20 hours, the temperature is lowered to 170°C in a hydrogen atmosphere. At a pressure of 2.8MPa, the weight space velocity of dimethyl oxalate is 0.4 hours. -1 , under the condition that the hydrogen ester molar ratio is 120:1, dimethyl oxalate is put into the reactor, and after being stable for 40 hours, the temperature is raised to the normal reaction temperature of the catalyst at 210°C to continue the reaction. During the whole reaction process, the conversion of dimethyl oxalate The ratios are all 100%, and the selectivity of ethylene glycol is 96.5%.
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