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    • 1. 发明授权
    • Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts
    • 通过固定床负载的钯催化剂上的炔进行部分氢化制备C10-C30-烯烃
    • US06365790B2
    • 2002-04-02
    • US09734024
    • 2000-12-12
    • Klaus ReimerGerd KaibelUlrich KammelFranz Josef BröckerAndreas AnsmannHeinz EtzrodtManfred StroezelMathias HaakeLothar LaupichlerBernhard Bockstiegel
    • Klaus ReimerGerd KaibelUlrich KammelFranz Josef BröckerAndreas AnsmannHeinz EtzrodtManfred StroezelMathias HaakeLothar LaupichlerBernhard Bockstiegel
    • C07C2900
    • C07C29/17B01J23/44B01J23/50B01J35/04B01J35/06B01J37/0217B01J37/0225B01J37/08C07C5/09C07C2523/44C07C11/02C07C33/025C07C33/02
    • Alkenes are prepared by partial hydrogenation of alkynes in the liquid phase at from 20 to 250° C. and hydrogen partial pressures of from 0.3 to 200 bar over fixed-bed supported palladium catalysts which are obtainable by heating the support material in the air, cooling, applying a palladium compound and, if required, additionally other metal ions for doping purposes, molding and processing to give monolithic catalyst elements, by a process in which A) alkynes of 10 to 30 carbon atoms are used as starting compounds, B) the palladium compound and, if required, the other metal ions are applied to the support material by impregnation of the heated and cooled support material with a solution containing palladium salts and, if required, other metal ions and subsequent drying, and C) from 10 to 2000 ppm of carbon monoxide (CO) are added to the hydrogenation gas or a corresponding amount of CO is allowed to form in the liquid phase by slight decomposition of a compound which is added to the reaction mixture and eliminates CO under the reaction conditions. The process is particularly advantageous if the partial hydrogenation is carried out in a tube reactor by the trickle-bed or liquid phase procedure with product recycling at cross-sectional loadings of from 20 to 500 m3/m2*h. The process is particularly suitable for the preparation of 3,7,11,15-tetramethyl-1-hexadecen-3-ol (isophytol), 3,7,11-trimethyl-l-dodecen-3-ol (tetrahydronerolidol), 3,7,11-trimethyl-1,4-dodecadien-3-ol, 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol), 3,7-dimethyloct-1,6-dien-3-ol or 3,7-dimethyloct-1-en-3-ol from the corresponding alkynes.
    • 烯烃通过液相中炔烃在20至250℃的部分氢化和固定床负载的钯催化剂的0.3至200巴的氢分压来制备,其可通过加热空气中的载体材料,冷却 使用钯化合物,另外还需要另外的金属离子用于掺杂目的,通过使用10-30个碳原子的炔烃作为起始化合物的方法,模塑和加工以得到整体式催化剂元素,B)钯 如果需要,另外的金属离子通过用含有钯盐的溶液浸渍加热和冷却的载体材料以及如果需要的话其它金属离子并随后干燥而被施加到载体材料上,C)为10-2000ppm 的一氧化碳(CO)加入到氢化气体中,或者相应量的CO在液相中形成,通过轻微分解添加到真空中的化合物 并且在反应条件下消除CO。如果部分氢化在管式反应器中通过滴流床或液相方法进行,则该方法是特别有利的,其中产物回收的横截面负荷为20-500m 3 / m2 * h。 该方法特别适用于制备3,7,11,15-四甲基-1-十六碳烯-3-醇(异山梨糖醇),3,7,11-三甲基-1-十二碳烯-3-醇(四氢化吗啉醇),3 ,7,11-三甲基-1,4-十二碳二烯-3-醇,3,7,11-三甲基-1,6-十二碳二烯-3-醇(二氢吗啉醇),3,7-二甲基辛-1,6-二烯 - 3-醇或3,7-二甲基辛-1-烯-3-醇。
    • 8. 发明授权
    • Method for reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof
    • 降低含氨基腈,二胺,二腈或其混合物的混合物中不饱和胺含量的方法
    • US07385073B2
    • 2008-06-10
    • US10515281
    • 2003-05-21
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BaβlerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BaβlerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • C07C253/34
    • C07C253/34C07C255/24
    • A process for reducing the level of an aliphatic monounsaturated amine (IV) in a mixture (V) containing an aminonitrile (I) or a diamine (II) or a dinitrile (III) or mixtures thereof as well as said mine (IV) by a) reacting said mixture (V) with an anionic nucleophile (VI) which contains a nucleophilic atom selected from the group consisting of oxygen, nitrogen and sulfur, which is capable of taking up an H+ ion to form an acid having a pKa value in the range from 7 to 11, as measured in water at 25° C., and which has a relative nucleophilicity, as measured in methyl perchlorate/methanol at 25° C., in the range from 3.4 to 4.7 when said nucleophilic atom is oxygen, in the range from 4.5 to 5.8 when said nucleophilic atom is nitrogen, and in the range from 5.5 to 6.8 when said nucleophilic atom is sulfur, in an amount in the range from 0.01 to 10 mol per mole of said amine (IV) in said mixture (V) at a temperature in the range from 50 to 200° C. to obtain a mixture (VII), b) distilling said aminonitrile (I) or said diamine (II) or said dinitrile (III) or mixtures thereof from said mixture (VII) at a temperature in the range from 50 to 200° C. and at a pressure in the range from 0.1 to 100 kPa to obtain a bottom product (VIII), which comprises c) distilling an aminonitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof from said bottom product (VIII) at a temperature which is lower than that chosen in step b).
    • 在含有氨基腈(I)或二胺(II)或二腈(III)或其混合物以及所述矿(IV)的混合物(V)中降低脂族单不饱和胺(IV)的水平的方法, a)使所述混合物(V)与阴离子亲核试剂(VI)反应,所述阴离子亲核试剂(VI)含有选自氧,氮和硫的亲核原子,其能够吸收H + 形成在25℃下在水中测量的具有7至11的pK值的酸,其在25℃下在高氯酸甲酯/甲醇中测得的具有相对亲核性 当所述亲核原子为氧时,在3.4至4.7的范围内,当所述亲核原子为氮时,在4.5至5.8的范围内,当所述亲核原子为硫时在5.5至6.8的范围内,其量为 在所述混合物(V)中在50至200℃的温度范围内每摩尔所述胺(IV)为0.01至10摩尔的范围,以获得混合物 (VII)中,b)在50至200℃的温度下,从所述混合物(VII)中蒸馏所述氨基腈(I)或所述二胺(II)或所述二腈(III)或其混合物, 压力为0.1至100kPa,以获得底部产物(VIII),其包括c)在所述底部产物(VIII)中蒸馏氨基腈(I)或二胺(II)或二腈(III)或其混合物, 温度低于步骤b)中选择的温度。
    • 9. 发明申请
    • Method for purifying caprolactam
    • 己内酰胺纯化方法
    • US20060090994A1
    • 2006-05-04
    • US10534822
    • 2003-11-11
    • Hermann LuykenAndreas AnsmannChristoph BenischPeter BablerRolf-Hartmuth FischerStefan MaixnerJohann-Peter Melder
    • Hermann LuykenAndreas AnsmannChristoph BenischPeter BablerRolf-Hartmuth FischerStefan MaixnerJohann-Peter Melder
    • B01D3/34C07C51/44
    • C07D201/16
    • A process for purifying crude caprolactam which has been obtained by 1) converting a mixture (I) comprising 6-aminocapronitrile and water to a mixture (II) comprising caprolactam, ammonia, water, high boilers and low boilers in the presence of a catalyst, then 2) removing ammonia from mixture (II) to obtain a mixture (III) comprising caprolactam, water, high boilers and low boilers, then 3) completely or partly removing water from mixture (III) to obtain crude caprolactam (IV) comprising caprolactam, high boilers and low boilers, which comprises a) feeding the crude caprolactam and an inorganic acid which has a boiling point above the boiling point of caprolactam under the distillation conditions of the following steps b) to h) to a first distillation apparatus C1, b) distilling the crude caprolactam and the inorganic acid in the first distillation apparatus C1, and removing a first substream in the bottom region and a second substream in the top region of the distillation apparatus C1, c) feeding the second substream from step b) to a second distillation apparatus C2, d) distilling the second substream from step b) in the second distillation apparatus C2, and removing a first substream in the bottom region and a second substream in the top region of the distillation apparatus C2, e) feeding the first substream from step d) to a third distillation apparatus C3, f) distilling the first substream from d) in the third distillation apparatus C3, and removing a first substream in the bottom region and purified caprolactam in the top region of distillation apparatus C3, and g) feeding the first substream from step f) to the first distillation apparatus C1.
    • 一种纯化己内酰胺的方法,其通过以下步骤获得:1)在催化剂存在下,将包含6-氨基己腈和水的混合物(I)转化为包含己内酰胺,氨,水,高锅炉和低沸点的混合物(II) 然后2)从混合物(II)中除去氨以获得包含己内酰胺,水,高锅炉和低锅炉的混合物(III),然后3)从混合物(III)中完全或部分除去水,得到包含己内酰胺的粗己内酰胺(IV) ,高沸点锅炉和低锅炉,其包括:a)在第一蒸馏装置C1的下述步骤b)至h)的蒸馏条件下,将粗己内酰胺和沸点高于己内酰胺沸点的无机酸, b)在第一蒸馏装置C1中蒸馏粗己内酰胺和无机酸,并且除去蒸馏装置C1的顶部区域中的第一子流和顶部区域中的第二子流 c)将来自步骤b)的第二子流进料到第二蒸馏装置C2,d)在第二蒸馏装置C2中蒸馏步骤b)中的第二子流,并且除去第二蒸馏装置C2中的第一子流, e)蒸馏装置C2的顶部区域,e)将来自步骤d)的第一子流进料到第三蒸馏装置C3,f)将第一子流从d)蒸馏到第三蒸馏装置C3中,并且除去底部区域中的第一子流 和在蒸馏装置C3的顶部区域中纯化的己内酰胺,并且g)将来自步骤f)的第一子流进料到第一蒸馏装置C1。
    • 10. 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。