A kind of copper-based catalyst for hydrogenation of oxalate to ethylene glycol and preparation method thereof
A technology of copper-based catalyst and oxalate ester, which is applied in the field of catalysis, can solve the problems of poor catalyst stability and achieve the effects of improving low-temperature activity, large-scale industrial application prospects, and high operation reproducibility
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Embodiment 1
[0026] A. The silica gel carrier used is the B-type silica carrier of Qingdao Ocean Chemical Co., Ltd., which is commercially available, and its specific surface area is 300m 2 / g, with an average pore size of 12nm and a particle size of 1.5-2.5cm, soak in 1mol / L ammonia water for one week, filter and dry at 120°C for 24h in a drying oven to obtain a pretreated silica carrier;
[0027] B. Dissolve 6g of copper acetate in 30mL of deionized water, stir at 60°C until the copper acetate is completely dissolved, then add 30mL of 28% concentrated ammonia water, and continue stirring for 0.5h to obtain a copper ammonia solution; put 4g of pretreated silica carrier in After drying at 160°C for 2 hours, immerse in cuproammonia solution, and after immersing at 60°C for 24 hours, filter and wash for 3-4 times to obtain the catalyst precursor;
[0028]C. Adding 7.2g of silica sol with a mass fraction of 20% in 120mL deionized water is made into a silica sol solution with a concentration o...
Embodiment 2
[0032] A. With embodiment 1.
[0033] B. Dissolve 9g of copper acetate in 30mL of deionized water, stir at 30°C until the copper acetate is completely dissolved, then add 40mL of 28% concentrated ammonia water, and continue stirring for 0.5h to obtain a copper ammonia solution; put 4g of pretreated silica carrier in After drying at 180°C for 1 hour, immerse in cuproammonia solution, and after immersing at 80°C for 12 hours, filter and wash for 3-4 times to obtain the catalyst precursor;
[0034] C. Adding 7.2g of silica sol with a mass fraction of 20% in 120mL deionized water is made into a silica sol solution with a concentration of 0.2mol / L, and stirring makes the two evenly mixed; the catalyst precursor obtained in step B is immersed in the silica sol In the solution, after stirring at 60°C for 24h, the temperature was raised to 90°C for ammonia distillation for 1h; the mixture was transferred to a hydrothermal kettle, and the temperature was raised to 200°C for hydrotherma...
Embodiment 3
[0038] A. The silica gel carrier used is the B-type silica carrier of Qingdao Ocean Chemical Co., Ltd., which is commercially available, and its specific surface area is 350m 2 / g, with an average pore diameter of 14nm and a particle size of 2-3cm, soaked in 2mol / L ammonia water for one week, filtered and dried in a drying oven at 150°C for 12h to obtain a pretreated silica carrier;
[0039] B. Dissolve 12g of copper acetate in 30mL of deionized water, stir at 40°C until the copper acetate is completely dissolved, then add 40mL of 28% concentrated ammonia water, and continue stirring for 0.5h to obtain a copper ammonia solution; put 4g of pretreated silica carrier in After drying at 150°C for 3 hours, immerse in cuproammonia solution, after immersing at 40°C for 36h, filter and wash 3-4 times to obtain the catalyst precursor;
[0040] C. Adding 14.4g of silica sol with a mass fraction of 20% in 120mL deionized water is made into a silica sol solution with a concentration of 0....
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