Preparation method for Pd-V-polyoxometalate one-component three-active-center catalyst and application
An active center and multi-metal technology, which is applied in the field of preparation of palladium-vanadium-polymetallic oxygen cluster single-component three-active center catalysts, can solve the problems of low activity and large amount of noble metal catalysts, and achieve simple preparation methods and good catalysis Active, easy-to-separate effect
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specific example 1
[0034] Specific example 1: Compound Pd(dpa) 2 (VO(DMSO) 5 ) 2 [PMo 12 o 40 ] 2 Preparation of 4DMSO: In a clean beaker, add 2,2′-dipyridylamine (3 mmol), Pd(OAc) 2 (3 mmol) and 10 mL of acetonitrile, stirred vigorously at 40 °C for 20 min, cooled to room temperature, filtered, and the filtrate was evaporated slowly at room temperature. After 6 days, a pale yellow rod-shaped substance Pd(dpa)(OAc) was obtained. 2 . The yield is about 76%. H 4 PMo 11 VO 40 (0.8 mmol), Pd(dpa)(OAc) 2 (1mmol) was added to 15 mL dimethyl sulfoxide, mixed and stirred, and the resulting solution was stirred at room temperature for 40 min, then added ascorbic acid (1mmol), heated and stirred at 100°C for 3h, cooled, filtered, and the filtrate was Evaporation was slow, and after 5 days a massive single crystal was obtained. The yield is about 49%.
specific example 2
[0035] Specific example 2: Compound Pd(dpa) 2 (VO(DMSO) 5 ) 2 [PMo 12 o 40 ] 2 Preparation of 4DMSO: In a clean beaker, add 2,2′-dipyridylamine (3 mmol), Pd(OAc) 2 (3 mmol) and 10 mL of acetonitrile, stirred vigorously at 40 °C for 20 min, cooled to room temperature, filtered, and the filtrate was evaporated slowly at room temperature. After 6 days, a pale yellow rod-shaped substance Pd(dpa)(OAc) was obtained. 2 . The yield is about 76%. H 4 PMo 11 VO 40 (0.8 mmol), Pd(dpa)(OAc) 2 (1 mmol) was added to 15 mL dimethyl sulfoxide, mixed and stirred, and the resulting solution was stirred at room temperature for 40 min, then added ascorbic acid (0.8 mmol), heated and stirred at 120 degrees for 3 h, cooled, filtered, and the filtrate was Slowly evaporated under the condition of 5 days to obtain block single crystal. The yield is about 52%.
specific example 3
[0036] Specific example 3: Compound Pd(dpa) 2 (VO(DMSO) 5 ) 2 [PMo 12 o 40 ] 2 Preparation of 4DMSO: In a clean beaker, add 2,2′-dipyridylamine (3 mmol), Pd(OAc) 2 (3 mmol) and 10 mL of acetonitrile, stirred vigorously at 40 °C for 20 min, cooled to room temperature, filtered, and the filtrate was evaporated slowly at room temperature. After 6 days, a pale yellow rod-shaped substance Pd(dpa)(OAc) was obtained. 2 . The yield is about 76%. H 4 PMo 11 VO 40 (0.8 mmol), Pd(dpa)(OAc) 2 Add (1mmol) to 15 mL dimethyl sulfoxide, mix and stir, stir the resulting solution at room temperature for 40 min, then add glucose (1mmol), heat and stir at 100°C for 3h, cool, filter, and the filtrate is at room temperature Evaporation was slow, and after 5 days a massive single crystal was obtained. The yield is about 54%.
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