Method for preparing polyether amine catalyst, and polyether amine
The present invention relates to a method for preparing a polyether amine catalyst, and polyether amine. A polyether amine catalyst is a supported metal catalyst; γ-Al 2 O 3 is used as a carrier; basic cupric carbonate, basic nickel carbonate and basic cobalt carbonate are used as precursors of supported metals; and the polyether amine catalyst is prepared by performing twice adsorption roasting and once reduction by means of an equivalent-volumetic impregnation method. Easier decomposition is achieved by using basic carbonate, and only water and carbon dioxide are generated, such that processes and costs for treating waste gases can be saved. By using the polyether amine catalyst to prepare polyether amine, a conversion rate and primary amine selectivity can be improved, and the color of products can be reduced. Therefore, the obtained polyether amine can have higher activity and wider application.
1 . A method for preparing a polyether amine catalyst, wherein the polyether amine catalyst is a supported metal catalyst and γ-Al 2 O 3 is used as an alumina carrier, basic cupric carbonate, basic nickel carbonate and basic cobalt carbonate are used as precursors for supporting metals, and the polyether amine catalyst is prepared by performing twice adsorption roasting and once reduction by means of an equivalent-volumetic impregnation method, the method comprises:
S 1 . solution preparation: adding basic cupric carbonate, basic nickel carbonate and basic cobalt carbonate to deionized water, and performing stirring until the basic cupric carbonate, the basic nickel carbonate and the basic cobalt carbonate are completely dissolved, so as to obtain a solution A;
S 2 . immersion and adsorption: impregnating the alumina carrier into the solution A obtained in S 1 , allowing resulting mixture to stand after rotary immersion in a water bath, after a adsorption equilibrium of the alumina carrier is arrived, rising a temperature of a resulting system to 90° C., performing vacuum dehydration and drying, and then removing the alumina carrier, so as to obtain an intermediate carrier;
S 3 . roasting: placing the intermediate carrier obtained in S 2 into a muffle furnace for temperature programming, and performing roasting at a set temperature of 420° C.;
S 4 . twice adsorption and roasting: using the intermediate carrier roasted in S 3 as a carrier, repeating S 2 and S 3 for twice adsorption and roasting, wherein a metal salt ratio during a second immersion is the same as a ratio during a first immersion; and
S 5 . reduction: after cooling, performing, at 420° C. and a hydrogen atmosphere in a reduction furnace, rotary reduction on the intermediate carrier after twice adsorption and roasting, so as to obtain the polyether amine catalyst with γ-Al 2 O 3 as the alumina carrier.
2 . The method as claimed in claim 1 , wherein the water bath in S 2 is at a temperature of 40° C.; the rotary immersion is performed for 30 minutes; a time for standing is 30 minutes; and the vacuum dehydration is performed when the temperature of the resulting system rises to 90° C.
3 . The method as claimed in claim 1 , wherein the roasting in S 3 is performed for 5 hours.
4 . The method as claimed in claim 1 , wherein S 5 comprises: placing the intermediate carrier after twice adsorption and roasting into the reduction furnace, performing rotary reduction for 60 hours at 420° C. and a high-flow hydrogen atmosphere, then decreasing the temperature in the reduction furnace to 150° C., converting hydrogen into high-pure nitrogen, and performing passivating treatment on a surface of a resulting product, so as to obtain the polyether amine catalyst with γ-Al 2 O 3 as the alumina carrier.
5 . The method as claimed in claim 1 , wherein the stirring in S 1 is performed at 60° C. for 30 minutes.