Preparation method and application of a copper phosphotungstate/attapulgite clay composite oxidation desulfurization catalyst
A technology of attapulgite clay and desulfurization catalyst, which is applied in the field of copper phosphotungstic acid oxidation desulfurization catalyst, which can solve the problems of unsuitability for large-scale industrial application, difficult control of cooling and crystallization steps, high relative proportion of pure phosphotungstic acid, etc., and achieve repeated utilization High efficiency, low safety cost, simple and clear preparation process
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[0018] 1. Preparation of copper phosphotungstate / attapulgite clay catalyst.
[0019] Measure 20mL of 0.1mol / L sodium hydroxide solution, add 10mL of 0.1mol / L copper nitrate dropwise to it, a blue flocculent precipitates, stir for 5min to make the reaction complete. Wash with deionized water several times during suction filtration, and then vacuum dry at 40°C for 1 hour to obtain copper hydroxide powder. Weigh 0.2g of copper hydroxide powder, add it to 10mL of water, and disperse it evenly by ultrasonic vibration; weigh 3.0g of phosphotungstic acid (H 3 PW 12 o 40 14H 2 (2) was dissolved in 20mL water to obtain a phosphotungstic acid solution; then, the phosphotungstic acid solution and 30mL 3g / 10mL attapulgite slurry were added dropwise to the uniform dispersion system while stirring until the blue precipitate in the system disappeared completely. The total volume of the mixed solution is 50mL~60mL, stirred at room temperature for 10min, and dried at 100°C for 2h to obtain...
Embodiment 1
[0021] Add 0.1g catalyst to 50mL simulated oil with sulfur content of 200ppm prepared by mixing 0.3g benzothiophene (BT) and 500mL n-octane, add 0.12mL H 2 o 2 and 0.1 g of cetyltrimethylammonium bromide (CTAB), magnetically stirred in a water bath at 40° C. for 1 h, the reaction mixture was cooled to room temperature, and the layers were separated. Add 25mL of N-N-dimethylformamide (DMF) and continue to stir for 5min, statically separate the layers, separate the oil phase, measure the sulfur content and calculate the desulfurization rate to be 64.84%.
[0022] The catalyst in the mixed system was recovered by suction filtration, dried at 70°C for 1 hour, washed with water several times, and reused according to the above method after drying.
[0023] In the above method, benzothiophene was replaced by dibenzothiophene (DBT), and other conditions remained unchanged, and the desulfurization rate was measured, see Table 1 for details.
Embodiment 2
[0025] Add 0.2g catalyst to 50mL simulated oil with sulfur content of 200ppm prepared by mixing 0.3g benzothiophene (BT) and 500mL n-octane, add 0.12mL H 2 o 2 and 0.1 g of cetyltrimethylammonium bromide (CTAB), magnetically stirred in a water bath at 40° C. for 1 h, the reaction mixture was cooled to room temperature, and the layers were separated. Add 25mL of N-N-dimethylformamide (DMF) and continue to stir for 5min, statically separate the layers, separate the oil phase, measure the sulfur content and calculate the desulfurization rate to be 75.26%.
[0026] The catalyst in the mixed system was recovered by suction filtration, dried at 70°C for 1 hour, washed with water several times, and reused according to the above method after drying.
[0027] In the above method, benzothiophene was replaced by dibenzothiophene, and other conditions remained unchanged, and the desulfurization rate was measured, see Table 1 for details.
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