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    • 2. 发明公开
    • 입체적으로차폐된4-아미노피페리딘의정제방법
    • 用于净化异味的4-氨基哌啶的方法
    • KR1020000016253A
    • 2000-03-25
    • KR1019980709826
    • 1997-05-30
    • 바스프 에스이
    • 율리우스,만프레트루스트,하랄트크라우제,알프레트지겔,하르도지겔,볼프강비첼,톰
    • C07D211/58
    • C07D211/56
    • PURPOSE: A process for purifying sterically hindered 4-amino piperidines is provided which can maintain the low degree of intrinsic coloration and manufacture a product which is coupled with a low content of a by-product such as a stabilizing agent. CONSTITUTION: A process for purifying raw piperidines of formula (I), where R1 to R4 are C1 to C6 alkyl, R1 and R2 and/or R3 and R4 together are a CH2 chain with 2 to 5 C atoms is described. The process is characterized in that in an initial step high boiling point substances and possible water are eliminated by distillation from the raw piperidines, in a second step 0.01 to 5 wt %, in relation to the product of the first step, of a reducing agent are added and in a third step the piperidines are isolated by distillation.
    • 目的:提供一种纯化空间位阻的4-氨基哌啶的方法,其可以保持低的本征着色度,并制备与低含量的副产物如稳定剂偶联的产物。 组成:描述了式(I)的原始哌啶的方法,其中R 1至R 4为C 1至C 6烷基,R 1和R 2和/或R 3和R 4一起为具有2至5个C原子的CH2链。 该方法的特征在于,在初始步骤中,通过从原始哌啶中蒸馏除去高沸点物质和可能的水,在第二步中,相对于第一步产物,还原剂为0.01〜5重量% 并且在第三步中,通过蒸馏分离出哌啶。
    • 5. 发明公开
    • 카프로락탐및헥사메틸렌디아민의동시제조방법
    • 同时生产己内酰胺和六亚甲基二胺的方法
    • KR1019980701227A
    • 1998-05-15
    • KR1019970704616
    • 1995-12-22
    • 바스프 에스이
    • 아흐하머,귄테르바쓰러,페터피셔,롤프푹스,에베르하르트루이켄,헤르만쉬누르,베르너비첼,톰
    • C07D201/16
    • 본 발명은
      (a) 아디포니트릴을 부분 수소첨가 반응시켜 6-아미노카프로니트릴, 헥사메틸렌디아민, 암모니아, 아디포니트릴 및 헥사메틸렌이민을 실제로 포함하는 혼합물(=혼합물)을 제조하는단계,
      (b) 증류 조건하에서 불활성인 화합물 A의 존재하에, 암모니아는 전부 분리하지는 않으면서, 단계 (a)에서 얻은 혼합물을 증류하여 선구 물질 (forerunnig)로서 암모니아, 및 잔류물 I을 제조하는 단계,
      (c) 혼합물, 불활성 화합물 A 및 암모니아를 실제로 포함하고 암모니아의 함량은 단계(b)에서 사용된 혼합물의 함량보다 낮은 잔류물 I을 제 2 증류하여 선구 물질로서 불활성 화합물 A 및 암모니아의 혼합물, 및 잔류물 II를 제조하는 단계,
      (d) 혼합물 및 불활성 화합물 A를 실제로 포함하는 베이스 II를 제 3 컬럼에서 증류하여 선구 물질로서 불활성 화합물 A, 및 잔류물 III을 제조하는 단계,
      (e) 혼합물 및 임의로 불활성 화합물 B를 실제로 포함하는 베이스 III을 제 4 컬럼에서 증류하여, 헥사메틸렌이민, 임의로 불활성 화합물 B 및 헥사메틸렌디아민을 실제로 포함하는 선구 물질 KPI, 및 잔류물 IV을 제조하는 단계,
      (f) 선구 물질 KPI을 제 5 컬럼에서 증류하여 헥사메틸렌이민 및 임의로 불활성 화합물 B를 실제로 포함하는 선구 물질 KP2, 및 순도 95% 이상으로 헥사메틸렌디아민을 실제로 포함하는 잔류물 V를 제조하고, 선구 물질 KP2를 제 3 컬럼으로 공급하거나 또는 임의로 상기 일부반을 제 3 컬럼으로 공급하고, 나머지는 폐기하는 단계,
      (g) 6-아미노카프로니트릴 및 아디포니트릴을 실제로 포함하는 잔류물 IV를 제 6 컬럼에서 증류하여 선구 물질로서 95% 이상의 순도로 6-아미노카프로니트릴, 및 잔류물로서 아디포니트릴을 제조하는 단계로 이루어진, 아디포니트릴로부터의 카프로락탐 및 헥사메틸렌디아민의 동시 제조에 관한 것이다.
      생성된 6-아미노카프로니트릴은 고리화되어 카프로락탐을 형성한다.
    • 6. 发明公开
    • 이량체함량이낮은입체적으로차폐된4-아미노-피페리딘,그의제조방법및용도
    • 具有低二级含量的异味的4-氨基哌啶,其生产和使用
    • KR1020000016254A
    • 2000-03-25
    • KR1019980709827
    • 1997-05-28
    • 바스프 에스이
    • 율리우스,만프레트루스트,하랄트크라우제,알프레트지겔,하르도지겔,볼프강비첼,톰
    • C07D211/58C07D211/72
    • C08K5/3435C07D211/58
    • PURPOSE: A process for reducing the dimerization of piperidine is provided which gives a simple method for preparing 4-amino-piperidine at a low cost of production and can manufacture HALS compounds having a low content of a by-product. CONSTITUTION: A process for reducing the dimerization of piperidine of formula (I) in which R1 to R4 are C1 to C6 alkyl, R1 and R2 and/or R3 and R4 together are a CH2 chain with 2 to 5 C atoms is described. The process is characterized in that to the piperidine is added 0.001 to 0.2 wt % of a reducing agent of the formula MXH4-mYm, in which M is an alkaline metal, NR4, where R is the same or different C1-4 alkyl groups, or an equivalent of an alkaline earth metal or an equivalent zinc, X is boron or aluminium, Y is H or CN and m is 0 or 1. Also described is a mixture of piperidine (I), 0.001 to 0.2 wt % of a reducing agent and 1 to 1000 ppm of the dimer of the piperidine (I), and the production of HALS stabilizers therefrom.
    • 目的:提供一种减少哌啶二聚化的方法,其提供了以低成本生产制备4-氨基哌啶的简单方法,并可制备具有低含量副产物的HALS化合物。 描述:描述了其中R 1至R 4为C 1至C 6烷基,R 1和R 2和/或R 3和R 4一起是具有2至5个C原子的CH 2链的式(I)的哌啶的二聚反应的方法。 该方法的特征在于向哌啶中加入0.001至0.2重量%的式MXH4-mYm的还原剂,其中M为碱金属NR4,其中R为相同或不同的C1-4烷基, 或当量的碱土金属或当量的锌,X为硼或铝,Y为H或CN,m为0或1.还描述了哌啶(I),0.001至0.2重量%的还原性 试剂和1〜1000ppm的哌啶(I)的二聚体,以及由其制备HALS稳定剂。
    • 10. 发明授权
    • 카프로락탐및헥사메틸렌디아민의동시제조방법
    • KR100386706B1
    • 2003-08-21
    • KR1019970704616
    • 1995-12-22
    • 바스프 에스이
    • 아흐하머,귄테르바쓰러,페터피셔,롤프푹스,에베르하르트루이켄,헤르만쉬누르,베르너비첼,톰
    • C07D201/16
    • 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.
    • (a)己二腈部分氢化,产生基本上含有6-氨基己腈,六亚甲基二胺,氨,己二腈和六亚甲基亚胺(=“ 混合物“); (b)蒸馏步骤(a)中得到的混合物,在蒸馏条件为惰性的化合物A存在下,生成氨作为前馏分和残余物I,氨不完全分离; (c)将基本上含有“混合物”,惰性化合物A和氨(其氨含量低于步骤(b)中使用的混合物的氨含量)的残余物I进行第二次蒸馏,产生 惰性化合物A和氨,作为前体和残余物II; (d)基本上含有“混合物”的碱II, 和惰性化合物A在第三个塔中进行蒸馏,产生惰性化合物A作为前体和残余物III; (e)基本上含有“混合物”的基质III, 和任选的惰性化合物B在第四塔中进行蒸馏,产生基本上含有六亚甲基亚胺,任选惰性化合物B和六亚甲基二胺的残余物KP1和残余物IV; (f)使前体KP1在第五塔中进行蒸馏,产生基本上含有六亚甲基亚胺和任选惰性化合物B的前体KP2和基本上含有纯度至少为95%的六亚甲基二胺的残余物V, ,前级KP2被供给到第三塔或可选地仅部分供给到第三塔,其余的被丢弃; 和(g)基本上含有6-氨基己腈和己二腈的残余物IV在第六个塔中进行蒸馏,产生残留物中具有至少95%纯度的6-氨基己腈和残余物中的己二腈。 得到的6-氨基己腈环化形成己内酰胺。