Preparation and activation method of Raney nickel-aluminum-x catalyst for 1,4-butynediol hydrogenation to 1,4-butanediol
A technology of butynediol and activation method, which is applied in the field of preparation and activation of Raney nickel-aluminum-X catalyst, can solve the problems affecting the purity of catalyst active products, and achieve the effects of easy pulverization, simple preparation method and improved efficiency
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Embodiment 1
[0024] Weigh 250g of Ni block, 500g of Al block and 0.75g of B respectively and place them in an intermediate frequency induction furnace, turn on the current, after Ni, Al and X are melted, after melting at 900°C for 60 minutes, pour into water to cool; The catalyst obtained after grinding to 200 mesh powder; Weigh 200g of catalyst powder and add in batches 400g of NaOH solution with a mass concentration of 25% and mix evenly, then control the temperature at 60°C for 30min, after the reaction is completed, wash with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2 hours; the activated catalyst was moved into a high-pressure reactor with 3000g35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa. The reaction temperature was 50°C and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.3%, and the selectivity of 1,4-butanediol was 90.8%.
Embodiment 2
[0026] Weigh 250g of Ni block, 500g of Al block and 0.75g of Mg and place them in the medium frequency induction furnace, turn on the current, after Ni, Al and X are melted, after melting at 900°C for 60min, pour into water to cool; The catalyst obtained after grinding to 200 mesh powder; Weigh 200g of catalyst powder and add in batches 400g of NaOH solution with a mass concentration of 25% and mix evenly, then control the temperature at 60°C for 30min, after the reaction is completed, wash with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2 hours; the activated catalyst was moved into a high-pressure reactor with 3000g35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa. The reaction temperature was 50°C and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.7%, and the selectivity of 1,4-butanediol was 92.8%.
Embodiment 3
[0028] Weigh 300g of Ni block, 500g of Al block and 1.6g of Sr respectively and put them in the medium frequency induction furnace, turn on the current, after Ni, Al and X are melted, after smelting at 1000℃ for 60min, pour into water to cool; The obtained catalyst was ground to 200-mesh powder; weighed 200g of catalyst powder and added in batches to 400g of KOH solution with a mass concentration of 25% and mixed evenly, then controlled the temperature at 60°C for 30min, after the reaction was completed, washed with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2 hours; the activated catalyst was moved into a high-pressure reactor with 3000g35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa. The reaction temperature was 50°C and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.7%, and the selectivity of 1,4-butanediol was 93.5%.
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