Method for efficiently synthesizing primary amine
A primary amine, high-efficiency technology, applied in the field of high-efficiency synthesis of primary amines, can solve the problems of lack of industrialization potential, easy to generate a large amount of waste, low selectivity, etc., to achieve easy separation and recycling, good industrial application prospects, substrates wide range of effects
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Embodiment 1-7
[0137] When the core-shell Co@CoO catalyst is prepared by the precipitation method in Examples 1-7: the cobalt source is cobalt nitrate, the precipitating agent is sodium carbonate, the calcination temperature is 450°C, and the reduction temperature is 300°C. The difference between Examples 1-7 The reason is that the volume fraction of hydrogen in the reducing gas used is different, the flow rate of the reducing gas is different, and the reduction time is different.
[0138] When cobalt-based catalysts were used to catalyze the preparation of primary amines in Examples 1-7: the reaction substrate was 0.18 g of cyclopentanone, the catalyst was 0.02 g of core-shell Co@CoO catalyst, the reaction medium was 5 ml of methanol, and the partial pressure of ammonia gas was 0.3MPa, partial pressure of hydrogen is 2MPa, reaction temperature is 90°C, reaction time is 4h, using a batch reactor to obtain the reaction product cyclopentylamine. The conversion rate of reaction substrate and th...
Embodiment 8-13
[0142] In Example 8-13, when the core-shell type Co@CoO catalyst is prepared by the precipitation method: the cobalt source is cobalt nitrate, the precipitating agent is sodium carbonate, the calcination temperature is 450°C, the volume fraction of hydrogen in the reducing gas is 10%, and the reducing gas The flow rate is 30ml / min, and the reduction time is 2h. The difference between Examples 8-13 is that the reduction temperatures used are different. Specifically, the reduction temperatures of Examples 8-13 are 225°C, 250°C, 275°C, and 300°C, respectively. , 350°C, and 400°C, the obtained core-shell Co@CoO catalysts were Co@CoO-P-225, Co@CoO-P-250, Co@CoO-P-275, Co@CoO-P-300, Co@CoO-P-350, Co@CoO-P-400.
[0143] When cobalt-based catalysts are used to catalyze the preparation of primary amines in Examples 8-13: the reaction substrate is 0.18 g of cyclopentanone, the catalyst is 0.02 g of core-shell Co@CoO catalyst, the reaction medium is 5 ml of methanol, and the partial pres...
Embodiment 14-18
[0149] In Examples 14-18, when the core-shell Co@CoO catalyst was prepared by high-temperature pyrolysis method: 5 g of cobalt nitrate was used as the cobalt source, and high-temperature calcination was carried out in a muffle furnace at 500 ° C for 5 hours to obtain the precursor Co 3 o 4 ; Embodiment 14-18 reduction precursor Co 3 o 4 The volume fraction of hydrogen in the reducing gas used was 10%, the flow rate of the reducing gas was 30ml / min, and the reduction time was 2h. The difference between Examples 14-18 was that the reduction temperatures used were different. Specifically, Examples 14-18 The reduction temperatures were 225°C, 250°C, 275°C, 300°C, 350°C, 400°C, and the obtained core-shell Co@CoO catalysts were Co@CoO-P-225, Co@CoO-P-250, Co@CoO-P-275, Co@CoO-P-300, Co@CoO-P-350, Co@CoO-P-400.
[0150] When cobalt-based catalysts were used to catalyze the preparation of primary amines in Examples 14-18: the reaction substrate was 0.18 g of cyclopentanone, the cat...
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