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    • 1. 发明申请
    • PROCESS FOR CONTINUOUSLY CLEANING RAW CAPROLACTAM MADE FROM 6-AMINO CAPRONITRILE
    • 用于连续清洁方法OUT 6-氨基己腈生产ROH己内酰胺
    • WO1996020923A1
    • 1996-07-11
    • PCT/EP1995005103
    • 1995-12-22
    • BASF AKTIENGESELLSCHAFT
    • BASF AKTIENGESELLSCHAFTRITZ, JosefFISCHER, RolfSCHNURR, WernerACHHAMMER, GüntherLUYKEN, HermannFUCHS, Eberhard
    • C07D201/16
    • C07D201/16Y02P20/52
    • Cleaning raw caprolactam by hydration, subsequent treatment in an acid medium and final distillation in an alkaline medium, in which (a) 6-amino capronitrile is converted into raw caprolactam by reaction with water; (b) difficultly and easily boiling components are removed from the raw caprolactam from step (a); (c) the raw caprolactam from step (b) is treated with hydrogen at a temperature in the 50 to 150 DEG C range and a pressure in the 1.5 to 250 bar range in the presence of a hydration catalyst and, if desired, a solvent, to give a mixture A;(d1) mixture A is taken at a temperature in the 30 to 80 DEG C range and a pressure in the 1 to 5 bar range over an ion exchanger containing acid terminal groups to give a mixture B1 or (d2) mixture A is distilled in the presence of sulphuric acid, in which any solvent is removed before the addition of the sulphuric acid to give a mixture B2; and (e) mixture B1 or B2 is distilled in the presence of a base to yield pure caprolactam.
    • 通过氢化粗己内酰胺,在由碱性介质酸性介质中和随后的蒸馏后续处理的纯化的(a)6-氨基己腈通过与水到粗己内酰胺反应进行反应; (B)从粗己内酰胺从步骤(a)中分离的重和轻馏分; 在50至150℃下的范围内的温度(℃)从步骤(b)的粗己内酰胺和在加氢催化剂的存在下1.5至250巴的范围内的压力,并且如果需要的溶剂,用氢气以获得混合物 A; (D1)的混合物在30〜80℃的温度和1〜5巴以上的含末端酸基的离子交换剂的范围内的压力下,在溶剂A,导致得到混合物B1; 或(D2)的混合物A是在硫酸的存在下与硫酸的添加存在的任何溶剂除去的前蒸馏,从而得到混合物B2; 和(e)混合物B1或在碱的存在下混合物B2蒸馏以获得纯的己内酰胺。
    • 2. 发明申请
    • METHOD OF SIMULTANEOUSLY PREPARING CAPROLACTAM AND HEXAMETHYLENE DIAMINE
    • 程序己内酰胺和己二胺的同时生产
    • WO1996020931A1
    • 1996-07-11
    • PCT/EP1995005115
    • 1995-12-22
    • BASF AKTIENGESELLSCHAFT
    • BASF AKTIENGESELLSCHAFTACHHAMMER, GüntherBASSLER, PeterFISCHER, RolfFUCHS, EberhardLUYKEN, HermannSCHNURR, WernerWITZEL, Tom
    • C07D223/10
    • C07C209/48C07D201/08
    • The invention concerns the simultaneous preparation of caprolactam and hexamethylene diamine from adipodinitrile, by the following steps: (a) the adipodinitrile is partially hydrogenated, producing a mixture substantially containing 6-aminocapronitrile, hexamethylene diamine, ammonia, adipodinitrile and hexamethylene imine (= "the mixture"); (b) the mixture obtained in step (a) is distilled, producing ammonia, as the forerunnings, and a residue I, in the presence of a compound A which is inert in the distillation conditions, the ammonia not being separated totally; (c) the residue I, substantially containing "the mixture", inert compound A and ammonia, the ammonia content being less than that of the mixture used in step (b), is subjected to a second distillation, producing a mixture of the inert compound A and ammonia, as the forerunnings, and a residue II; (d) the base II, substantially containing "the mixture" and inert compound A, is subjected to distillation in a third column, producing the inert compound A, as the forerunnings, and a residue III; (e) the base III, substantially containing "the mixture" and optionally an inert compound B, is subjected to distillation in a fourth column, producing forerunnings KP1, which substantially contain hexamethylene imine, optionally inert compound B and hexamethylene diamine, and a residue IV; (f) the forerunnings KP1 are subjected in a fifth column to distillation, producing forerunnings KP2, which substantially contain hexamethylene imine and optionally inert compound B, and a residue V, which substantially contains hexamethylene diamine with a degree of purity of at least 95 %, the forerunnings KP2 being fed to the third column or optionally only partially fed to the third column, and the rest being discarded; and (g) the residue IV, substantially containing 6-aminocapronitrile and adipodinitrile, is subjected in a sixth column to distillation, producing 6-aminocapronitrile with a degree of purity of at least 95 %, as forerunnings, and adiponitrile in the residue. The resultant 6-aminocapronitrile is cyclized to form caprolactam.
    • 同时制备的己内酰胺和己二胺己二腈从开始通过(a)己二腈被部分氢化以得到主要含6-氨基己腈,六亚甲基二胺,氨,己二腈和六亚甲基亚胺的混合物(=“混合物”),以及(b)中 (a)使获得的蒸馏,得到氨作为顶部产物和塔底产物I,不被完全在惰性的蒸馏条件化合物下在存在分离,并且其中所述氨,和(c)的塔底产物I,基本上含有混合物 “共混物”,惰性的化合物和氨,氨含量大于所述混合物,将其在步骤(b)中使用的低,第二蒸馏以得到氨和惰性化合物的混合物作为塔顶产物和 底部产物II,和(d)的塔底产物II,主要包含“共混物”和惰性的化合物 A,在第三列中,蒸馏,得到惰性的化合物A作为塔顶产物和塔底产物III,(E)的塔底产物III,基本上含有“共混物”,以及如果需要,一种惰性化合物B,下经受,在第四列中,蒸馏 得到顶部产物KP1,基本上含有六亚甲基亚胺,如果需要惰性的化合物B和六亚甲基二胺,和塔底产物IV,(F)的塔顶产物KP1在第五列中,蒸馏,得到一顶部产物KP2,主要含有六亚甲基亚胺,并且如果需要的惰性化合物B 和底部产物V,以至少95%的纯度基本上六亚甲基二胺的含,被供应到所述第三塔的塔顶产物KP2或任选仅部分送入第三塔,其余部分被除去,和(g)塔底产物IV,主要含有 6-氨基己腈和Adipodinit RIL,进行,在第六列中,蒸馏,得到具有至少95%的纯度作为顶部产物和己二腈作为底部6-氨基己腈,和6-氨基己腈环化己内酰胺这样获得。