Solid carried ion liquid-nanometer metal particle catalyst, and its preparing method, and application in synthesis of arylamine
A technology of nano metal particles and ionic liquids, applied in the preparation of amino compounds, preparation of organic compounds, catalysts for physical/chemical processes, etc.
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Embodiment 1
[0061] The synthesis of palladium nano-catalysts supported by two layers of ionic liquids (terminal is octyl, palladium mass percentage is 2.0%):
[0062] 1g octanized immobilized bis-imidazole (formula 2, carrier=silicon dioxide; m=1, n=0; Q=(CH 2 ) 3 , Q 1 =(CH 2 ) 4 ;L=OCH 2 CH 3 ;R=C 8 h 17 , R 1 -R 6 = H), suspended in 0.033g of palladium chloride (0.19mmol) in 10mL of acetonitrile solution, refluxed for 48h under nitrogen protection, filtered, washed with deionized water and absolute ethanol in turn, dried in vacuum at 60°C, recorded as Immobilization Catalyst Precursor A 0 .
[0063] Will be dissolved with 0.021g NaBH 4 (0.57mmol) of 3mL absolute ethanol solution was slowly added dropwise to the suspended 1.0g A 0 10mL of absolute ethanol, the color of the mixture gradually darkened and finally turned black, after the reaction was complete. Filter, wash with deionized water and absolute ethanol successively, dry under vacuum at 60°C, and suspend the obtain...
Embodiment 2-7
[0067] According to the method of embodiment 1, change terminal substituent group octyl to be other alkanes, change material type or ratio to obtain a series of catalysts as follows:
[0068] 2) 1g of octanized immobilized bis-imidazole (formula 2, carrier=silicon dioxide; m=1, n=0; Q=(CH 2 ) 3 , Q 1 =(CH 2 ) 4 ;L=OCH 2 CH 3 ;R=C 8 h 17 , R 1 -R 6 =H), 0.025g palladium chloride (0.14mmol), 0.015g NaBH 4 (0.42 mmol); Catalyst B (Pdwt% = 1.5) was obtained.
[0069] 3) 1g of octanized immobilized bis-imidazole (formula 2, carrier=silicon dioxide; m=1, n=0; Q=(CH 2 ) 3 , Q 1 =(CH 2 ) 4 ;L=OCH 2 CH 3 ;R=C 8 h 17 , R 1 -R 6 =H), 0.017g palladium chloride (0.09mmol), 0.011g NaBH 4 (0.27 mmol); Catalyst C (Pd wt% = 1.0) was obtained.
[0070] 4) 1g butylated imididazole immobilized (formula 2, carrier=silicon dioxide; m=1, n=0; Q=(CH 2 ) 3 , Q 1 =(CH 2 ) 4 ;L=OCH 2 CH 3 ;R=C 4 h 9 , R 1 -R 6 =H), 0.017g palladium chloride (0.09mmol), 0.011g NaBH 4 (0...
Embodiment 8
[0074] Embodiment 8 (comparative example)
[0075] Synthesis of silica gel directly supported palladium catalyst:
[0076] Suspend 1 g of silica gel activated according to a conventional method directly in 10 mL of deionized aqueous solution of 0.017 g of palladium chloride (0.09 mmol), stir at room temperature for 24 h, and carry out the rest of the synthesis process according to Example 1, and finally obtain a palladium with a weight loading of 1.0%. Catalyst H.
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