A kind of mixed silicon source method synthetic oxalate hydrogenation catalyst and preparation method thereof
A hydrogenation catalyst and mixed silicon source method technology, applied in the chemical industry, can solve problems such as environmental pollution in catalyst production, and achieve the effects of enhancing sintering resistance, improving the environment, and increasing hydrogenation activity and selectivity.
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Embodiment 1
[0028] The preparation method of the oxalate hydrogenation catalyst synthesized by the mixed silicon source method of the present embodiment is as follows:
[0029] Based on 100g of catalyst, according to 32%CuO, 1%B 2 o 3 , 67%SiO2 2Weigh 96.64g of copper nitrate trihydrate and 1.78g of boric acid into 1200mL of water, heat and stir until the solids are completely dissolved, add 134g of 25% silica sol (pH 1) acidified by nitric acid into the prepared solution drop by drop, and forcefully Stir for 7h, then drop an aqueous solution containing 68.12g of sodium silicate into the mixing system, wherein the ratio of silica sol and sodium silicate is 1:1 (based on SiO 2 After stirring for 2 hours, it was crystallized in a 130°C hydrothermal kettle for 12 hours. The obtained solid-liquid mixture was washed by centrifugation, washing with alcohol, and then dried at 120°C. After calcination at 450°C for 6 hours, the catalyst was prepared. use.
[0030] Catalyst evaluation: The prep...
Embodiment 2
[0032] The preparation method of the oxalate hydrogenation catalyst synthesized by the mixed silicon source method of the present embodiment is as follows:
[0033] Based on 100g catalyst, according to 20%CuO, 0.5%ZnO, 79.5%SiO 2 Take 60.4g of copper nitrate trihydrate and 1.83g of zinc nitrate hexahydrate into 2500mL of water, the concentration of copper salt is 0.1mol / L, stir until all the solids are dissolved, and acidify 212g of silica sol with a content of 25% in nitric acid (pH 2 ) was added dropwise to the prepared solution, and stirred vigorously for 1h, then the aqueous solution containing 53.89g of sodium silicate was dropped into the mixing system, wherein the ratio of silica sol and sodium silicate was 2:1 (based on SiO 2 After stirring for 2 hours, it was crystallized in a 110°C hydrothermal kettle for 20 hours, and the obtained solid-liquid mixture was washed with centrifugal water and alcohol in turn, and then dried at 100°C. After calcination at 450°C for 6 hou...
Embodiment 3
[0036] The preparation method of the oxalate hydrogenation catalyst synthesized by the mixed silicon source method of the present embodiment is as follows:
[0037] Based on 100g of catalyst, according to 20%CuO, 0.1%Al 2 o 3 , 79.9% SiO 2 Take 60.4g of copper nitrate trihydrate and 0.37g of aluminum nitrate nonahydrate into 167mL of water, the concentration of copper salt is 1.5mol / L, stir until all the solids are dissolved, and acidify 106.53g of silica sol with a content of 25% in nitric acid (pH is 2) Add dropwise to the prepared solution and stir vigorously for 6 hours, then drop the aqueous solution containing 108.3g of sodium silicate into the mixing system, wherein the ratio of silica sol and sodium silicate is 1:2 (based on SiO 2 After stirring for 4 hours, it was crystallized in a 120°C hydrothermal kettle for 15 hours. The obtained solid-liquid mixture was washed with centrifugal water and alcohol in turn, and then dried at 90°C. After calcination at 450°C for 6 h...
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