Preparation method of N-pyridine oxide
A technology for oxidizing pyridine and pyridine, which is applied in the field of preparation of pyridine N-oxide, can solve the problems of long stable operation period and low conversion rate of pyridine, and achieve good catalytic effect, high yield and high atom utilization
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Embodiment 1
[0014] 2.5g Na 2 WO 4 2H 2 O was dissolved in 30 mL of deionized water at 70°C, stirred and dissolved, and then 0.26 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 0.28 g mass fraction of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 24.25g of silicon dioxide and add it to the above solution, stir well and let it stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 26.07g of phosphorus-tungsten-silicon composite catalyst. Add 100g of pyridine and 26.07g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 215g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 80° C. for 120 minutes. ...
Embodiment 2
[0016] 5g Na 2 WO 4 2H 2 O was dissolved in 25 mL of deionized water at 70°C, stirred and dissolved, and then 0.64 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 0.5 g of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 20.63g of silicon dioxide and add it to the above solution, stir well and let it stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 24.27g of phosphorus-tungsten-silicon composite catalyst. Add 162g of pyridine and 24.27g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 418g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 65° C. for 50 minutes. Pour the mixture a...
Embodiment 3
[0018] 10g Na 2 WO 4 2H 2 O was dissolved in 40 mL of deionized water at 70°C, stirred and dissolved, and 1.38 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 2.0 g of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 16g of silicon dioxide and add it to the above solution, stir well and let stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 23.28g of phosphorus-tungsten-silicon composite catalyst. Add 100g of pyridine and 23.28g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 240g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 80° C. for 70 minutes. Pour the mixture after the r...
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