公开(公告)号：US08981093B2

公开(公告)日：2015-03-17

申请号：US13910554

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 Jödecke

IPC: C07D295/023 ,  C07D241/04 ,  C07C209/28 ,  C07C213/04 ,  C07D295/027

CPC classification number: C07D241/04 ,  C07C209/28 ,  C07C213/04 ,  C07D295/023 ,  C07D295/027

Abstract: Process for preparing piperazine of the formula I by reacting diethanolamine (DEOA) of the formula II with ammonia in the presence of hydrogen and a supported, metal-containing catalyst has been found, wherein the catalytically active mass of the catalyst, prior to its reduction with hydrogen, comprises oxygen-containing compounds of aluminum, copper, nickel and cobalt and in the range from 0.2 to 5.0% by weight of oxygen-containing compounds of tin, calculated as SnO, 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 25 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: 已经发现通过使式II的二乙醇胺（DEOA）与氢气和负载的含金属的催化剂的氨反应制备式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 与氢气一起包含铝，铜，镍和钴的含氧化合物，其含量为0.2至5.0重量％，以SnO计算的含氧化合物锡，反应在液相中进行 使用160-220巴的绝对压力，温度在180-220℃范围内，使用摩尔比为DEA的氨为5至25，在0.2至9.0重量％存在下 的氢气，基于使用的DEOA的总量和氨。

公开(公告)号：US20130331573A1

公开(公告)日：2013-12-12

申请号：US13910554

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 Jödecke

IPC: C07D241/04 ,  C07C213/04 ,  C07C209/28

CPC classification number: C07D241/04 ,  C07C209/28 ,  C07C213/04 ,  C07D295/023 ,  C07D295/027

Abstract: Process for preparing piperazine of the formula I by reacting diethanolamine (DEOA) of the formula II with ammonia in the presence of hydrogen and a supported, metal-containing catalyst has been found, wherein the catalytically active mass of the catalyst, prior to its reduction with hydrogen, comprises oxygen-containing compounds of aluminum, copper, nickel and cobalt and in the range from 0.2 to 5.0% by weight of oxygen-containing compounds of tin, calculated as SnO, 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 25 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: 已经发现通过使式II的二乙醇胺（DEOA）与氢气和负载的含金属的催化剂的氨反应制备式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 与氢气一起包含铝，铜，镍和钴的含氧化合物，其含量为0.2至5.0重量％，以SnO计算的含氧化合物锡，反应在液相中进行 使用160-220巴的绝对压力，温度在180-220℃范围内，使用摩尔比为DEA的氨为5至25，在0.2至9.0重量％存在下 的氢气，基于使用的DEOA的总量和氨。

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。