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公开(公告)号:US20130331574A1
公开(公告)日:2013-12-12
申请号:US13910602
申请日:2013-06-05
Applicant: BASF SE
Inventor: Roland Bou Chedid , Johann-Peter Melder , Ulrich Abel , Roman Dostalek , Nina Challand , Bernd Stein , Michael Jodecke
IPC: C07D295/023
CPC classification number: C07D295/023
Abstract: Process for preparing piperazine of the formula I by reacting diethanolamine (DEOA) of the formula II with ammonia (NH3) in the presence of hydrogen and a supported, metal-containing catalyst, wherein the catalytically active mass of the catalyst, prior to its reduction with hydrogen, comprises 20 to 85% by weight of oxygen-containing compounds of zirconium, calculated as ZrO2, 1 to 30% by weight of oxygen-containing compounds of copper, calculated as CuO, 14 to 70% by weight of oxygen-containing compounds of nickel, calculated as NiO, and 0 to 5% by weight of oxygen-containing compounds of molybdenum, calculated as MoO3, and the reaction is carried out in the liquid phase at an absolute pressure in the range from 160 to 220 bar, a temperature in the range from 180 to 220° C., using ammonia in a molar ratio to DEOA used of from 5 to 20 and in the presence of 0.2 to 9.0% by weight of hydrogen, based on the total amount of DEOA used and ammonia.
Abstract translation: 通过使式II的二乙醇胺(DEOA)与氢气和负载的含金属催化剂的存在下的氨(NH 3)反应制备式I的哌嗪的方法,其中催化剂的催化活性物质在其还原之前 含氢量为20〜85重量%,以ZrO 2计,含氧化合物的锆为1〜30重量%,以CuO表示的含氧化合物的铜为14〜70重量% 以NiO计算的镍化合物和以重量计为MoO 3的0-5%重量的含氧化合物的钼,反应在液相中以160-220巴的绝对压力进行, 温度在180-220℃的范围内,使用的摩尔比为使用的DEOA为5至20的氨和在0.2至9.0重量%的氢气存在下,基于所用的DEOA的总量和 氨。