Preparation method for catalyst for synthesizing oxalic ester by gas-phase
A catalyst and oxalate technology, which is applied in the direction of catalyst activation/preparation, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc. It can solve the problems of high price, high catalyst use temperature, and influence on use, and achieve low cost Effect
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Embodiment 1
[0028] Dissolve 10 grams of ferric nitrate and 5 grams of manganese nitrate in 35 g of water, then pour it into a beaker with 100 grams of spherical α-alumina carrier with a diameter of 4 mm, dry it after impregnation, and roast it at 450 ° C for 2 hours, then roast The final carrier was put into 35 g of solution made with 0.5 gram of palladium chloride to impregnate and adsorb palladium to obtain the catalyst.
[0029] The catalyst uses H 2 The hydrogen-nitrogen mixture with a content of 90% was reduced at 250°C for 8 hours, then cooled to 105°C, and the H 2 After purging, the volume composition of the feed is 15% CH 3 ONO+30%CO+55%N 2 Air source, air speed 6000h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 1050g / L.h, and the selectivity of dimethyl oxalate is 99.75%.
Embodiment 2
[0031] 15 grams of ammonium molybdate and 10 grams of ammonium paratungstate were dissolved in 40 grams of ammonia water with a mass concentration of 17%, and then poured into a beaker with 100 grams of 3mm in diameter and 8mm in length strip-shaped α-alumina carrier, dried after immersion, and Calcined at 550° C. for 2 hours, then put the calcined carrier into 36 g solution prepared with 0.9 g palladium acetate to impregnate and adsorb palladium to obtain the catalyst.
[0032] The catalyst uses H 2 The hydrogen-nitrogen mixed gas with a content of 50% was reduced at 350°C for 8 hours, and then the temperature was lowered to 120°C, and the H 2 After purging, the volume composition of the feed is 10% CH 3 ONO+20%CO+70%N 2 Air source, air speed 4000h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 780g / L.h, and the selectivity of dimethyl oxalate is 99.85%.
Embodiment 3
[0034] Dissolve 25 grams of ferric nitrate and 12 grams of nickel nitrate in 45 grams of water, then pour it into a beaker with 100 grams of clover-shaped α-alumina carrier, dry it after impregnation, and roast it at 750 ° C for 2 hours, then put the roasted The carrier was put into 0.15 g of palladium chloride and mixed with 35 g of solution to impregnate and adsorb palladium to obtain an oxygen catalyst.
[0035] The catalyst uses H 2 The hydrogen-nitrogen mixed gas with a content of 10% was reduced at 450°C for 8 hours, and then cooled to 100°C, and the H 2 After purging, the volume composition of the feed is 15% CH 3 ONO+30%CO+55%N 2 Air source, air speed 4500h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 1050g / L.h, and the selectivity of dimethyl oxalate is 99.85%.
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