公开(公告)号：EP0324190A3

公开(公告)日：1990-09-19

申请号：EP88121923.2

申请日：1988-12-31

申请人： HÜLS AKTIENGESELLSCHAFT ,  MILES INC.

发明人： Schmelzer, Hans-Georg ,  Allen, Gary F. ,  Bub, Günther, Dr. ,  Otte, Werner, Dr.

IPC分类号： C07C209/72 ,  C07C211/35

CPC分类号： C07C209/72 ,  B01J23/462 ,  B01J35/1019 ,  B01J35/1061 ,  C07C2601/14 ,  C07C211/36

摘要： The present invention is directed to a process for the catalytic hydrogenation of a starting material containing 4,4′-diamino-diphenylmethane (4,4′-MDA) or its mixtures with 2,4′-diamino-diphenylmethane, 2,2′-diamino-diphenylmethane and/or higher ring compounds of the diphenylmethane series to a hydrogenation product having a trans-trans isomer content of 4,4′-diamino-dicyclohexylmethane (4,4′-HMDA) of about 15 to 40 weight percent, based on the diamine content of the hydrogenated product, by continuously hydrogenating in at least one fixed bed reactor at a temperature of about 100 to 190°C and a pressure of about 50 to 350 bar in the presence of a ruthenium catalyst on a catalyst support having a BET surface area of about 70 to 280 m²/g and an average pore diameter d p of about 10 to 320 Å, the catalyst being prepared by impregnating the catalyst support to a penetration depth of at least about 50 µm with a soluble ruthenium compound in an amount sufficient to provide a catalyst containing about 0.1 to 5 weight percent ruthenium and subsequently reducing the soluble ruthenium compound to ruthenium.

摘要翻译： 本发明涉及催化氢化含有4,4'-二氨基 - 二苯基甲烷（4,4min-MDA）或其与2,4min-二氨基 - 二苯基甲烷的混合物的起始材料的方法，2,2min - 二氨基 - 二苯基甲烷和/或高级环化合物与具有约15至40重量％的反式异构体含量为4,4'-二氨基 - 二环己基甲烷（4,4分钟-HMDA）的氢化产物， 基于氢化产物的二胺含量，在催化剂载体上的钌催化剂存在下，在约100至190℃的温度和约50至350巴的压力下在至少一个固定床反应器中连续氢化 具有约70至280m 2 / g的BET表面积和约10至320的平均孔径dp，所述催化剂是通过将催化剂载体浸渍至至少约50μm的渗透深度制备的， 一定量的可溶性钌化合物 足以提供含有约0.1至5重量％钌的催化剂，随后将可溶性钌化合物还原成钌。

公开(公告)号：EP0324190B1

公开(公告)日：1993-05-12

申请号：EP88121923.2

申请日：1988-12-31

申请人： HÜLS AKTIENGESELLSCHAFT ,  MILES INC.

发明人： Schmelzer, Hans-Georg ,  Allen, Gary F. ,  Bub, Günther, Dr. ,  Otte, Werner, Dr.

IPC分类号： C07C209/72 ,  C07C211/35

CPC分类号： C07C209/72 ,  B01J23/462 ,  B01J35/1019 ,  B01J35/1061 ,  C07C2601/14 ,  C07C211/36

公开(公告)号：EP0324190A2

公开(公告)日：1989-07-19

申请号：EP88121923.2

申请日：1988-12-31

申请人： HÜLS AKTIENGESELLSCHAFT ,  MILES INC.

发明人： Schmelzer, Hans-Georg ,  Allen, Gary F. ,  Bub, Günther, Dr. ,  Otte, Werner, Dr.

IPC分类号： C07C209/72 ,  C07C211/35

CPC分类号： C07C209/72 ,  B01J23/462 ,  B01J35/1019 ,  B01J35/1061 ,  C07C2601/14 ,  C07C211/36

摘要： The present invention is directed to a process for the catalytic hydrogenation of a starting material containing 4,4′-diamino-diphenylmethane (4,4′-MDA) or its mixtures with 2,4′-diamino-diphenylmethane, 2,2′-diamino-diphenylmethane and/or higher ring compounds of the diphenylmethane series to a hydrogenation product having a trans-trans isomer content of 4,4′-diamino-dicyclohexylmethane (4,4′-HMDA) of about 15 to 40 weight percent, based on the diamine content of the hydrogenated product, by continuously hydrogenating in at least one fixed bed reactor at a temperature of about 100 to 190°C and a pressure of about 50 to 350 bar in the presence of a ruthenium catalyst on a catalyst support having a BET surface area of about 70 to 280 m²/g and an average pore diameter d p of about 10 to 320 Å, the catalyst being prepared by impregnating the catalyst support to a penetration depth of at least about 50 µm with a soluble ruthenium compound in an amount sufficient to provide a catalyst containing about 0.1 to 5 weight percent ruthenium and subsequently reducing the soluble ruthenium compound to ruthenium.

摘要翻译： 本发明涉及一种制备含有4,4'-二氨基二苯基甲烷（4.4分钟-MDA）或它与2.4分钟氨基二苯基甲烷二混合物，2.2分钟原料的催化氢化 的约15至40％（重量）的二氨基二苯基甲烷二和/或二苯基甲烷系列的具有4,4'-二氨基二环己基甲烷的反式 - 反式异构体含量的氢化产物的更高环化合物（4.4分钟-HMDA）， 基于氢化产物的二胺的含量，通过在约100至190℃的温度和大约50至350巴的在钌催化剂的存在下在催化剂载体上的压力下连续氢化在至少一个固定床反应器 具有约70至280米<2> / g，并且在约10平均细孔直径d p，以320埃的BET表面积，所述催化剂通过浸渍催化剂载体的至少约50微米与渗透深度制备 的可溶性钌化合物中的量 足以提供含催化剂约0.1至5重量％的钌，并且随后减少可溶性钌化合物到钌。