Method for catalyzing selective hydrogenation of 1,3-butadiene with PdAgNi/N-C catalyst
A catalyst and butadiene technology, which is applied in catalyst activation/preparation, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the problem of high catalyst cost, high butene-1 loss, and product butadiene content. Insufficient and other problems, to achieve the effect of good catalytic activity, high activity and stability
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Embodiment 1
[0021] (1) Preparation of catalyst
[0022] 0.02mmolPdCl 2 , 0.004mmolAgNO 3 and 0.002 mmol NiCl 2 Dissolve in 10mL of distilled water, stir evenly in an ice bath at 0°C, and then add 10mmol of N-C material to the above solution, wherein the N-C material is prepared by roasting melamine and glucose at 700°C for 2 hours at a mass ratio of 30:1; After stirring, dropwise add 0.1mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 80°C for 20 hours to obtain the catalyst PdAg 0.2 Ni 0.1 / N-C 500 , airtight storage.
[0023] (2) Hydrogenation reaction process
[0024] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 30 ° C, and then add 1,3-butane with a molar ratio of 1:1.2 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 1.5MPa, and the reaction space velocity is 1.0h -1 .
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Embodiment 2
[0027] (1) Preparation of catalyst
[0028] 0.02mmolPdCl 2 , 0.008mmolAgNO 3 and 0.006 mmol NiCl 2 Dissolve in 10mL of distilled water, stir evenly in an ice bath at 0°C, and then add 16mmol N-C material to the above solution, wherein, the N-C material is prepared by roasting melamine and glucose at 900°C for 6 hours at a mass ratio of 60:1; After stirring, dropwise add 0.4mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 140°C for 10 hours to obtain the catalyst PdAg 0.4 Ni 0.3 / N-C 800 , airtight storage.
[0029] (2) Hydrogenation reaction process
[0030] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 60 ° C, and then add 1,3-butane with a molar ratio of 1:2.5 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 3.2MPa, and the reaction space velocity is 4.0h -1 .
[...
Embodiment 3
[0033] (1) Preparation of catalyst
[0034] 0.02mmolPdCl 2 , 0.006mmolAgNO 3 and 0.004 mmol NiCl 2 Dissolve in 10mL distilled water, stir evenly in an ice bath at 0°C, and then add 14mmol N-C material to the above solution, wherein the N-C material is prepared by roasting melamine and glucose at 800°C for 4 hours at a mass ratio of 50:1; After stirring, dropwise add 0.3mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 120°C for 15 hours to obtain the catalyst PdAg 0.3 Ni 0.2 / N-C 700 , airtight storage.
[0035] (2) Hydrogenation reaction process
[0036] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 50 ° C, and then add 1,3-butane with a molar ratio of 1:2.0 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 2.8MPa, and the reaction space velocity is 3h -1 .
[0037] ...
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