A kind of preparation method of catalyst for synthesizing hexamethylene diamine by hydrogenation of adiponitrile
An alloy catalyst and catalyst technology are applied in the field of petrochemical catalysis, which can solve the problems of poor catalyst uniformity, serious environmental pollution, low activity and selectivity, etc., and achieve the effect of uniform distribution
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Embodiment 1
[0022] 1. Catalyst powder preparation:
[0023] With 500ml5wt% ammonia water as a complexing agent and 100ml5wt% nickel nitrate as a raw material, the mixed reaction generates a nickel-ammonia complex solution; under stirring conditions, 0.1wt% ferric nitrate solution is added at a speed of 1ml / min to form a mixed solution, The molar ratio of iron to nickel ions is 0.01:1; under stirring conditions, add 60-80 mesh powder ground from porous aluminum as a carrier, and the mass ratio of porous aluminum powder to nickel is 0.5:1; heat the mixed solution , carried out hydrothermal aging at 20°C for 1h, filtered and separated to obtain solid particles, dried and calcined, and passed through hydrogen at 0.1MPa300°C for 1h to obtain catalyst powder.
[0024] 2. Catalyst activation
[0025] Slowly add 10 g of the above catalyst powder into 0.2 mol / l NaOH solution under ice-water bath and stirring conditions, wherein the mass ratio of catalyst powder to NaOH solid is 0.25:1; 20°C and ...
Embodiment 2
[0027] 1. Catalyst powder preparation:
[0028] Using 200ml of 7wt% ammonia water as a complexing agent and 100ml of 10wt% nickel nitrate as a raw material, the mixed reaction produces a nickel ammonia complex solution; under stirring conditions, after mixing 0.5wt% of ferric nitrate, chromium nitrate and bismuth nitrate solution in a certain proportion Add at a speed of 2ml / min to form a mixed solution, wherein the molar ratio of chromium, bismuth and iron ions is 0.5:0.5:1, and the ratio of their total moles to nickel ions is 0.05:1; The 60-80 mesh powder made of porous aluminum is used as a carrier, and the mass ratio of porous aluminum powder to nickel is 1:1; the mixed solution is heated, hydrothermally aged at 50°C for 1 hour, filtered and separated to obtain solid particles, and dried and roasted , At 0.1MPa400°C, hydrogen was passed through for reduction for 4h to obtain catalyst powder.
[0029] 2. Catalyst activation
[0030] Slowly add the above catalyst powder in...
Embodiment 3
[0032] 1. Catalyst powder preparation:
[0033] With 300ml10wt% ammonia water as a complexing agent and 100ml20wt% nickel nitrate as a raw material, the mixed reaction generates a nickel-ammonia complex solution; under stirring conditions, mix 2wt% ferric nitrate and molybdenum nitrate in a certain proportion and then mix them at a rate of 3ml / min The speed is added to form a mixed solution, in which the molar ratio of molybdenum to iron ions is 3:1, and the ratio of their total moles to nickel ions is 0.1:1; under stirring conditions, add 60-80 mesh made of porous aluminum The powder is used as a carrier, and the mass ratio of porous aluminum powder to nickel is 1.5:1; the mixed solution is heated, hydrothermally aged at 80°C for 1h, filtered and separated to obtain solid particles, and after drying and roasting, hydrogen gas is introduced at 0.1MPa500°C After reduction for 2h, the catalyst powder was obtained.
[0034] 2. Catalyst activation
[0035] Slowly add the above c...
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