Preparation method and application of crystalline copper heterogeneous catalyst
A heterogeneous catalyst and crystalline phase technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve difficult separation, recovery and reuse, difficult synergistic chelation, improper disposal of environmental hazards, etc. problems, to achieve the effects of reducing errors caused by human and uncontrollable factors, improving hydrothermal stability, and reducing consumption costs
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specific Embodiment approach
[0034] Al(NO) was weighed on an analytical balance 3 ) 3 ·9H 2 O is 0.6150g, add it to the round-bottomed flask, then take 80mL of deionized water and stir until it becomes clear, adjust the pH value of the solution to 3; weigh 1g of the prepared rod-shaped SBA-15 mesoporous molecular sieve, mix it with the aluminum source solution Mix, ultrasonically shake for 10 min, and stir continuously for 4 h at room temperature; transfer the obtained mixed solution into a crystallization kettle lined with polytetrafluoroethylene, and continue to crystallize at 150 ° C for 24 hours; the crystallized mixture is washed with anhydrous ethanol Washed with deionized water, dried and then calcined at high temperature, heated to 550 °C at a heating rate of 2 °C / min, calcined for 5 h, and calcined in an air atmosphere to obtain an aluminum-modified product Al / SBA-15. Then weigh 0.2011g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in deionized water until it became clear, and 0.5 g of Al / SBA-15 was ad...
Embodiment 2
[0037] A preparation method of a crystalline phase copper catalyst Cu / Al-SBA-15(II) with high hydrothermal stability: one-step stirring for 6h, crystallization at 130°C; two-step stirring for 4h, drying at 80°C, drying 8h, the following are specific implementations:
[0038] Al(NO) was taken on an analytical balance 3 ) 3 ·9H 2 O is 0.6150g, add it to the round-bottomed flask, then take 80mL of deionized water and stir until it becomes clear, adjust the pH value of the solution to 3; weigh 1g of the prepared rod-shaped SBA-15 mesoporous molecular sieve, mix it with the aluminum source solution Mix, ultrasonically shake for 10 min, and stir continuously for 6 h at room temperature; transfer the obtained mixed solution into a crystallization kettle lined with polytetrafluoroethylene, and continue to crystallize at 130 ° C for 24 hours; the crystallized mixture is washed with absolute ethanol Washed with deionized water, dried and then calcined at high temperature, heated to 5...
Embodiment 3
[0039] Embodiment 3 (catalyst consumption 1.38mol%)
[0040] Compound 2-aminothiophenol, benzyl alcohol, potassium tert-butoxide (t-BuOK), crystalline copper catalyst Cu / Al-SBA-15(II) and solvent anhydrous toluene (toluene) were added to the round-bottomed flask. , the molar ratio of compound 2-aminothiophenol and benzyl alcohol was 1:1, and the reaction was carried out under the condition of 120°C under constant temperature stirring, refluxed, and monitored by TCL.
[0041] Compounds A and B are 0.4 mmol and 0.4 mmol for 2-aminothiophenol and benzyl alcohol respectively, the dosage of crystalline copper catalyst Cu / Al-SBA-15(II) is 1.38 mol%, and the dosage of t-BuOK is 0.8 mmol, The amount of solvent toluene was 3 mL; after 2 days of reaction, TCL monitored the complete reaction of the compound 2-aminothiophenol, the reaction ended, and the target product 2-phenylbenzo[d]thiazole was generated, which was analyzed by gas-mass spectrometry ( GC-MS) detected a yield of 67%. ...
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