Supported catalyst for preparation of amino-terminated polyether through continuous method

[0022] Example 1

[0023] A). Weigh 60g of alumina powder and place it in a Maffei furnace at 450°C for 5h, cool the alumina powder to room temperature, add 4.8g of 8% acetic acid aqueous solution to the alumina powder, use a 3.5mm mill With tablet molding, the molded alumina is fired in a Maffy furnace at 300°C for 2.5 hours. Weigh 178g nickel nitrate and 70g copper nitrate into a 40% aqueous solution, add the formed alumina carrier to the aqueous solution and soak for 10h, place the impregnated catalyst in an oven at 120°C for 3h, and finally place the dried catalyst Firing in a Maffei furnace at 450°C for 5h.

[0024] B). Measure 30ml of the catalyst obtained in the preparation step A and place it in the constant temperature section of a fixed bed. Under the conditions of heating rate 2 ℃/min, final reduction temperature 210 ℃, 10% hydrogen/90% nitrogen mixed gas, temperature programmed reduction 4 hours. Reduce the reactor temperature to 80°C, and pass 110L/h of high-purity hydrogen with a volumetric space velocity of 3.5h -1 Liquid ammonia, volumetric space velocity 2.5h -1 A polyether polyol with a molecular weight of 230 is synthesized under the conditions of a reaction temperature of 220°C and a reaction pressure of 3.5MPa, and the product is filtered and vacuum distilled to obtain a polyether ammonia product. After chemical analysis, the total amine value of the product was 7.82mmol/g, the reaction conversion rate reached 92.5%, and the purity of primary amine reached 93.45%.

[0025] Example 2

[0026] A). Weigh 60g of alumina powder and place it in a Maffy furnace at 430°C for 5h, cool the alumina powder to room temperature, add 6g of acetic acid aqueous solution with a concentration of 9.5% to the alumina powder, use a 3.5mm abrasive tool Compression molding, the molded alumina is calcined in a Maffy furnace at 300°C for 2.5 hours. Weigh 190g nickel nitrate and 60g copper nitrate into a 40% aqueous solution, add the formed alumina carrier to the aqueous solution and soak for 10 hours, place the impregnated catalyst in an oven at 120°C for 3 hours, and finally place the dried catalyst Calcined in a Maffei furnace at 480°C for 4.5 hours.

[0027] B). Measure 30ml of the catalyst obtained in the preparation step A and place it in the constant temperature section of a fixed bed. Under the conditions of heating rate 2 ℃/min, final reduction temperature 210 ℃, 10% hydrogen/90% nitrogen mixed gas, temperature programmed reduction 4 hours. Reduce the reactor temperature to 80°C, and pass in 150L/h of high-purity hydrogen with a volumetric space velocity of 2.5h -1 Liquid ammonia, volumetric space velocity 3h -1 A polyether polyol with a molecular weight of 430 is synthesized under the conditions of a reaction temperature of 230°C and a reaction pressure of 4MPa, and the product is filtered and vacuum-distilled to obtain a polyether ammonia product. After chemical analysis, the total amine value of the product was 4.32mmol/g, the reaction conversion rate reached 94.23%, and the purity of primary amine reached 96.18%.

[0028] Example 3

[0029] Measure 30ml of the catalyst obtained in the preparation step A in Example 2 and place it in the constant temperature section of the fixed bed, and program the temperature rise under the conditions of a heating rate of 4°C/min, a final reduction temperature of 225°C, and a 10% hydrogen/90% nitrogen mixture. Reduce for 4 hours. Lower the reactor temperature to 80℃, and pass in 110L/h of high-purity hydrogen, and the volumetric space velocity is 3h -1 Liquid ammonia, volumetric space velocity 3h -1 A polyether polyol with a molecular weight of 800 is synthesized under the conditions of a reaction temperature of 230°C and a reaction pressure of 4.5 MPa, and the product is filtered and vacuum distilled to obtain a polyether ammonia product. After chemical analysis, the total amine value of the product is 2.4mmol/g, the reaction conversion rate reaches 100%, and the purity of primary amine reaches 96.21%.