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    • 22. 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%。
    • 26. 发明授权
    • Method for reducing the content of an unsaturated amine in a mixture containing an amine and a nitrile
    • 减少含有胺和腈的混合物中不饱和胺含量的方法
    • US06828457B2
    • 2004-12-07
    • US10432385
    • 2003-05-21
    • Frank OhlbachChristoph BenischHermann LuykenAndreas AnsmannRolf-Hartmuth FischerJohann-Peter MelderPeter BasslerStefan Maixner
    • Frank OhlbachChristoph BenischHermann LuykenAndreas AnsmannRolf-Hartmuth FischerJohann-Peter MelderPeter BasslerStefan Maixner
    • C07C25334
    • C07C209/84C07C253/34
    • A process is provided for reducing the content of a monounsaturated aliphatic amine (III) in a mixture (IV) containing an aminonitrile (I) or a diamine (II), or mixtures thereof, and the amine (III), wherein a) the mixture (IV) is reacted with an anionic nucleophile (V),  which contains a nucleophilic atom selected from the group comprising oxygen, nitrogen and sulfur,  which is capable of taking up an H+ ion to form an acid with a pKa ranging from 7 to 11, measured in water at 25° C., and  which has a relative nucleophilicity, measured in methyl perchlorate/methanol at 25° C.,  ranging from 3.4 to 4.7 when oxygen is the nucleophilic atom,  ranging from 4.5 to 5.8 when nitrogen is the nucleophilic atom, and  ranging from 5.5 to 6.8 when sulfur is the nucleophilic atom,  in an amount ranging from 0.01 to 10 mol per mole of amine (III) in the mixture (IV), to give a mixture (VI), and b) the aminonitrile (I) or the diamine (II), or mixtures thereof, are distilled from the mixture (VI) at a temperature ranging from 50 to 170° C. and a pressure ranging from 0.5 to 100 kPa.
    • 提供了一种降低含有氨基腈(I)或二胺(II)或其混合物的混合物(IV)中的单不饱和脂族胺(III)和胺(III)的含量的方法,其中a)混合物 (IV)与阴离子亲核试剂(V)反应,所述阴离子亲核试剂(V)含有选自氧,氮和硫的亲核原子,其能够吸收H +离子以形成pKa范围从 7至11,在25℃的水中测量,并且当氧是亲核原子时,在25℃的甲基高氯酸甲酯/甲醇中测量的范围为3.4至4.7,当氮气为4.5至5.8时,其具有相对的亲核性 是亲核原子,当硫是亲核原子时,其摩尔数为5.5至6.8,其量为每摩尔混合物(IV)中的胺(III)为0.01至10摩尔,得到混合物(Ⅵ),和b) 氨基腈(I)或二胺(II)或其混合物在温度下从混合物(VI)中蒸馏出 e范围为50至170℃,压力范围为0.5至100kPa。