A method for continuous production of amino-terminated polyether
A technology of primary amino-terminated polyether and hydroxyl polyether, which is applied in the low-pressure hydrogenation of low-molecular-weight hydroxyl-terminated polyether to prepare amino-terminated polyether and its catalyst, and can solve the problems of low liquid space velocity, high pressure and temperature, Low catalytic activity and other problems, to achieve the effect of low volatility, high primary amine selectivity, high conversion rate
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Embodiment 1
[0018] Preparation of Ni-Cu-Cr-La-Al by coprecipitation method 2 o 3 Catalyst: Co-precipitate the nitrate of nickel, copper, chromium, lanthanum and sodium carbonate at a certain temperature to prepare the catalyst. Adopt to add metal content (reduction state) to be: nickel 50%, copper 30%, lanthanum 1.00%, metal nitrate solution concentration is 0.5mol / L, precipitant Na 2 CO 3 0.5mol / L, co-precipitation reaction occurs at 40°C, aged at 60°C for 30 minutes, suction filtration and washing are performed in sequence, and the carrier Al is selected 2 o 3 The amount is 14%, dried for 10 hours after suction filtration, through grinding and granulation, and roasted at 350 ° C for 2 hours, and finally the catalyst after the roasting is added to the catalyst matrix with 1% weight of oxalic acid and other auxiliary agents to mix and compress tablets to obtain Columnar catalyst 1 with a specific surface area of 168.58m 2 / g, the pore volume is 0.30ml / g.
Embodiment 2
[0020] Preparation of Ni-Cu-Cr-Pd-Al by Co-precipitation 2 o 3 Catalyst: Co-precipitate nickel, copper, chromium, palladium nitrate and potassium bicarbonate at a certain temperature to prepare a catalyst for Ni-Cu-Cr-Pd-Al 2 o 3 Catalyst preparation. Adopt to add the metal content (reduced state) to be: nickel 80%, copper 5%, palladium 0.005%, metal nitrate solution concentration is 1mol / L, precipitant K 2 CO 3 1mol / L, the precipitation temperature is 60°C, aging at 70°C for 30min, suction filtration and washing in sequence, and the carrier SiO 2 The content is 10%, dried for 10 hours after suction filtration, after grinding and granulating, roasting at 300°C for 2 hours, and finally adding 5.0% citric acid as the parent material to the calcined catalyst for tableting to obtain columnar catalyst 2. Surface area is 157.64m 2 / g, the pore volume is 0.35ml / g.
Embodiment 3
[0022] Preparation of Ni-Cu-Cr-La-SiO by Co-precipitation 2 / Catalyst: Co-precipitate the chloride of elements such as nickel and potassium carbonate at a certain temperature to prepare the catalyst. Adopting to add metal content (reduced state) is: nickel 20%, copper 20%, lanthanum 10%, metal nitrate solution concentration is 2mol / L, precipitating agent Na 2 CO 32mol / L, co-precipitation reaction occurs at 80°C, aged at 80°C for 30min, suction filtration and washing are performed in sequence, and the carrier is selected as Al 2 o 3 and SiO 2 The amount of the mixture (each accounting for 50% (weight), its addition is 50%, dried for 10 hours after suction filtration, through grinding and granulation, roasted at 400 ° C for 2 hours, and finally added the precursor 3.0% lemon to the catalyst after roasting Acid and oxalic acid mixture (respectively accounting for 50% (weight) carry out tabletting, obtain columnar catalyst 3, and this catalyst specific surface area is 165.31m ...
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Abstract
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