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    • 1. 发明授权
    • Preparation of 3-aminomethyl-3,5,5-trimethylcyclohexylamine
    • 3-氨基甲基-3,5,5-三甲基环己胺的制备
    • US5756845A
    • 1998-05-26
    • US608485
    • 1996-02-28
    • Guido VoitTom WitzelBoris BreitscheidelWolfgang HarderHermann LuykenAxel PaulKarl-Heinz RossPeter Wahl
    • Guido VoitTom WitzelBoris BreitscheidelWolfgang HarderHermann LuykenAxel PaulKarl-Heinz RossPeter Wahl
    • B01J23/46B01J23/75B01J23/755C07B61/00C07C209/48C07C211/36
    • C07C209/48C07C2101/14
    • A process for the preparation of 3-aminomethyl-3,5,5-trimethylcyclohexylamine from 3-cyano-3,5,5-trimethylcyclohexanone which requires three spatially separated reaction spaces, in order to carry out the following three steps in sequence: a) reacting the 3-cyano-3,5,5-trimethylcyclohexanone with excess ammonia on acidic metal-oxide catalysts in a first reaction space at from 20.degree. to 150.degree. C. and from 50 to 300 bar, b) hydrogenating the resultant reaction products using hydrogen in a second reaction space in the presence of excess ammonia and preferably liquid ammonia on hydrogenation catalysts, optionally using basic components or on neutral or basic supports at from 50.degree. to 100.degree. C. and at from 50 to 300 bar, and c) hydrogenating the resultant reaction products in the presence of hydrogen and also ammonia in a third reaction space on hydrogenation catalysts, optionally using basic components or on neutral or basic supports at from 110.degree. to 160.degree. C. and at from 150 to 300 bar.These three steps in sequence provide a substantially complete reaction of the original 3-cyano-3,3,5-trimethylcyclohexanone reactant with a yield of 96% of the desired diamino product in which the cis-content of the diamine is 70%.
    • 从3-氰基-3,5,5-三甲基环己酮制备3-氨基甲基-3,5,5-三甲基环己胺的方法,其需要三个空间分离的反应空间,以便按顺序进行以下三个步骤:a )在20至150℃和50至300巴的第一反应空间中使3-氰基-3,5,5-三甲基环己酮与过量的氨在酸性金属氧化物催化剂上反应,b)将所得反应物氢化 在氢化催化剂存在下,在过量氨和优选液氨存在下在第二反应空间中使用氢的产物,任选使用碱性组分或在中性或碱性载体上在50至100℃和50至300巴条件下,以及 c)在氢化催化剂的第三反应空间中,在氢气和氨的存在下氢化所得反应产物,任选使用碱性组分或在中性或碱性载体上在110至160℃和150至300b ar。 这三个步骤依次提供原始3-氰基-3,3,5-三甲基环己酮反应物的基本上完全的反应物,其中二胺的顺式含量为70%的所需二氨基产物的产率为96%。
    • 9. 发明授权
    • Method for avoiding corrosion
    • 避免腐蚀的方法
    • US07309403B2
    • 2007-12-18
    • US10572783
    • 2004-09-24
    • Werner ReutemannTheodor WeberKarl-Heinz RossManfred Julius
    • Werner ReutemannTheodor WeberKarl-Heinz RossManfred Julius
    • B01D3/38B01D3/40C07C209/86C07C209/90
    • C07C211/04C07C209/86Y10S203/20Y10S203/24
    • The invention relates to a method of avoiding corrosion in the separation of methylamine from a product stream (10) which is obtained in the preparation of methylamines by gas-phase reaction of methanol and ammonia and includes monomethylamine, dimethylamine, trimethylamine, ammonia and methanol as components, where ammonia is separated off by pure distillation in a first column (1), the remaining components of the product stream obtained as bottoms (12) are fed to a second column (2). Trimethylamine (14) is separated off in the second column (2) by extractive distillation with introduction of water. The further of the product stream obtained as bottoms (15) from the second column (2) are fed to a third column (3), in which monomethylamine and dimethylamine are separated off at the top. The monomethylamine and dimethylamine are separated by distillation in a fourth column (4). To avoid corrosion alkali metal hydroxide is added to the second or third column (3).
    • 本发明涉及一种避免在甲醇与甲醇与氨的气相反应制备甲胺中得到的产物流(10)中分离甲胺的腐蚀方法,包括一甲胺,二甲胺,三甲胺,氨和甲醇 组分,其中在第一塔(1)中通过纯蒸馏分离氨,将作为塔底物(12)获得的产物流的剩余组分进料至第二塔(2)。 通过萃取蒸馏引入三水胺(14)在第二塔(2)中分离。 从第二塔(2)获得的作为塔底物(15)获得的产物流的其它组分进料到第三塔(3),其中一甲胺和二甲胺在顶部分离。 在第四列(4)中通过蒸馏分离一甲胺和二甲胺。 为了避免腐蚀,将碱金属氢氧化物加入到第二或第三塔(3)中。