Method for preparing polyether amine by hydroamination of polyether polyol
A technology of polyether polyols and alcohol hydroamines, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc. It can solve the problems of poor catalyst stability, poor catalyst activity, and inability to realize continuous production.
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Embodiment 1
[0080] The catalyst is 10%Co-2%Re / Al 2 o 3 . Weigh 8.8 grams of 20-40 mesh Al 2 o 3 , dried at 120°C for 4 hours before use, and 20ml of the configuration contains 4.94 grams of Co(NO 3 ) 2 ·6H 2 O, 0.29 g NH 4 ReO 4 , an aqueous solution of 1.92 g of β-cyclodextrin, with which the above-mentioned Al 2 o 3 The carrier was air-dried naturally, dried at 100°C for 4h, calcined at 600°C for 4h, and the heating rate was 4°C / min.
[0081] Weigh 4g of the above-mentioned catalyst (20-40 mesh) and place it in the middle of the fixed-bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MPa, temperature 450°C, hydrogen volume space velocity 500h -1 , Time 2h. The reaction conditions are: pressure 6MPa, temperature 170°C, hydrogen volume space velocity 100h -1 , PPG230 (polyoxypropylene ether, average molecular weight about 230g / mol): NH 3 =1:10 (molar ratio), PPG230 liquid hourly space velocity 0.6h -1 . Af...
Embodiment 2
[0084] The catalyst is 10%Ni-10%Co-1%Re-1%Ru-0.5%Ce / Al 2 o 3 . Weigh 7.8 grams of 20-40 mesh Al 2 o 3 , dried at 120°C for 4 hours before use, and 20ml of configuration containing 4.95 grams of Ni(NO 3 ) 2 ·6H 2 O, 4.94 g Co(NO 3 ) 2 ·6H 2 O, 0.14 g NH 4 ReO 4 , 0.26 g RuCl 3 ·3H 2 O, 0.15 g Ce(NO 3 ) 3 ·6H 2 O, an aqueous solution of 4.08 g of ethylenediamine, impregnating the above-mentioned Al with this aqueous solution 2 o 3 The carrier was air-dried naturally, dried at 100°C for 4h, calcined at 400°C for 6h, and the heating rate was 5°C / min.
[0085] Weigh 4g of the above-mentioned catalyst (20-40 mesh) and place it in the middle of the fixed-bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MPa, temperature 400°C, hydrogen volume space velocity 500h -1 , time 2h. The reaction conditions are: pressure 8MPa, temperature 200°C, hydrogen volume space velocity 200h -1 , PPG230 (polyoxypro...
Embodiment 3
[0088] The catalyst is 20%Ni-2%Re / SiO 2 . Weigh 7.8 grams of 100 mesh SiO 2 , dried at 120°C for 4 hours before use, the SiO 2 Disperse in water to form a suspension, and stir at a medium speed at a constant temperature of 50°C. Configuration 20ml contains 9.91 grams of Ni (NO 3 ) 2 ·6H 2 O, 0.29 g NH 4 ReO 4 , 1.93 g of β-cyclodextrin precursor liquid. The precipitating agent used is 4mol / L KOH solution. Add the precursor liquid and the precipitating agent dropwise to the above suspension at a rate of 1 mL / min at the same time, keep the pH value at 9 until the precipitation is complete, wash the precipitate with deionized water until neutral, filter, dry in the air, and dry at 120°C 4 hours, 500°C roasting for 6 hours, the heating rate is 2°C / min.
[0089] Weigh 4g of the above-mentioned catalyst (100 mesh) and place it in the middle of the fixed bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MP...
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