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    • 31. 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。
    • 33. 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。
    • 34. 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。
    • 35. 发明授权
    • Continuous method for producing polyamides from aminonitriles
    • 从氨腈生产聚酰胺的连续方法
    • US06815527B2
    • 2004-11-09
    • US10332579
    • 2003-01-10
    • Peter BasslerHelmut WinterlingRolf-Hartmuth FischerWolfgang Loth
    • Peter BasslerHelmut WinterlingRolf-Hartmuth FischerWolfgang Loth
    • C08G6904
    • C08G69/04C08G69/08C08G69/16
    • The continuous process for preparing a polyamide by reacting at least one aminonitrile with water comprises: (1) reacting at least one aminonitrile with water in the presence of an organic liquid diluent at from 90 to 400° C. and from 0.1 to 35×106 Pa in a flow tube containing a Brönsted acid catalyst selected from a beta-zeolite catalyst, a sheet-silicate catalyst or a titanium dioxide catalyst comprising from 70 to 100% by weight of anatase and from 0 to 30% by weight of rutile and in which up to 40% by weight of the titanium dioxide may be replaced by tungsten oxide, to obtain a reaction mixture, (2) further reacting the reaction mixture at from 150 to 400° C. and a pressure which is lower than the pressure in stage 1 in the presence of a Brönsted acid catalyst selected from a beta-zeolite catalyst, a sheet-silicate catalyst or a titanium dioxide catalyst comprising from 70 to 100% by weight of anatase and from 0 to 30% by weight of rutile and in which up to 40% by weight of the titanium dioxide may be replaced by tungsten oxide, the temperature and pressure being selected so as to obtain a first gas phase and a first liquid phase or a first solid phase or a mixture of first solid and first liquid phases and so that the first gas phase is separated from the first liquid phase or first solid phase or from the mixture of first liquid and first solid phases, and (3) admixing the first liquid or the first solid phase or the mixture of first liquid and first solid phases with a gaseous or liquid phase comprising water at from 150 to 370° C. and from 0.1 to 30×106 Pa, to obtain a product mixture.
    • 通过使至少一种氨基腈与水反应制备聚酰胺的连续方法包括:(1)在有机液体稀释剂存在下,在90至400℃和0.1至35×10 6时使至少一种氨基腈与水反应 在含有选自β-沸石催化剂,片状硅酸盐催化剂或二氧化钛催化剂的布朗斯台德酸催化剂的流动管中包含70至100重量%的锐钛矿和0至30重量%的金红石和 其中高达40重量%的二氧化钛可以被氧化钨代替,以获得反应混合物,(2)使反应混合物在150-400℃下进一步反应,并且压力低于压力 在选自β-沸石催化剂,片状硅酸盐催化剂或二氧化钛催化剂的布朗斯台德酸催化剂存在下,其包含70至100重量%的锐钛矿和0至30重量%的金红石,以及 其中高达40%的重量 二氧化钛可以被氧化钨代替,选择温度和压力以获得第一气相和第一液相或第一固相或第一固相和第一液相的混合物,使得第一气相 与第一液相或第一固相或第一液相和第一固相的混合物分离,和(3)将第一液体或第一固相或第一液相和第一固相的混合物与气体或 液相,其包含150至370℃和0.1至30×10 6 Pa的水,以获得产物混合物。
    • 36. 发明授权
    • Preparation of amines and aminonitriles
    • 胺和氨基腈的制备
    • US5789621A
    • 1998-08-04
    • US693983
    • 1996-08-08
    • Werner SchnurrGuido VoitKlemens FlickRolf-Hartmuth Fischer
    • Werner SchnurrGuido VoitKlemens FlickRolf-Hartmuth Fischer
    • B01J23/78B01J23/94B01J27/187B01J27/28B01J38/10C07B43/04C07B61/00C07C20060101C07C209/48C07C209/52C07C211/12C07C211/35C07C253/30C07C255/24C07C209/02
    • C07C209/48C07C209/52
    • A process for preparing an NH.sub.2 -containing compound by hydrogenating a compound containing at least one unsaturated carbon-nitrogen bond with hydrogen in the presence of a catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent which process includes the following steps: a) using a catalyst comprising a cobalt- and/or iron-containing catalyst, and b) after the conversion based on the compound to be hydrogenated and/or the selectivity based on the desired product has or have dropped below a defined value or the amount of an unwanted by-product has risen beyond a defined value, interrupting the hydrogenation by stopping the feed of the compound to be hydrogenated and of the solvent, if used, c) treating the catalyst at from 150.degree. to 400.degree. C. with hydrogen using a hydrogen pressure within the range from 0.1 to 30 MPa and a treatment time within the range from 2 to 48 h, and d) subsequently continuing the hydrogenation of the compound containing at least one unsaturated carbon-nitrogen bond.
    • 在催化剂存在下,在不低于室温和升高的氢分压的情况下,在存在或不存在溶剂的情况下,通过氢化含有至少一个不饱和碳 - 氮键的化合物与氢气来制备含NH 2的化合物的方法, 方法包括以下步骤:a)使用包含含钴和/或含铁催化剂的催化剂,和b)基于待氢化的化合物转化后,和/或基于所需产物的选择性具有或已经下降 低于定义的值或不想要的副产物的量已经超过定义的值,如果使用,则通过停止待氢化化合物的进料和溶剂的中断氢化,c)在150℃下处理催化剂 在氢气压力为0.1〜30MPa,处理时间为2〜48h的范围内,使氢气变为400℃,d)随后继续进行水压 该化合物含有至少一个不饱和碳 - 氮键。
    • 39. 发明申请
    • 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
    • US20050222449A1
    • 2005-10-06
    • US10515281
    • 2003-05-21
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BasslerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BasslerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • C07C209/84C07C211/09C07C211/12C07C253/34C07C255/09C07C255/24
    • 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 amine (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).
    • 含有氨基腈(I)或二胺(II)或二腈(III)或其混合物以及所述胺(IV)的混合物(V)中的脂肪族单不饱和胺(IV)的水平以及所述胺(IV) a)使所述混合物(V)与含有选自氧,氮和硫的亲核原子的阴离子亲核试剂(VI)反应,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。