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    • 4. 发明授权
    • Process for preparing higher unsaturated ketones
    • 制备高级不饱和酮的方法
    • US06300524B1
    • 2001-10-09
    • US09440281
    • 1999-11-15
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerUdo RheudeGerd KaibelThomas KrugLuise SpiskeHagen Jaedicke
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerUdo RheudeGerd KaibelThomas KrugLuise SpiskeHagen Jaedicke
    • C07C4500
    • C07C45/676Y02P20/582C07C49/255C07C49/203
    • The present invention relates to an improved process for preparing higher unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction , in a reactor system with fitted fractionation column, wherein A the &agr;,&bgr;-unsaturated alcohol is introduced into the reaction vessel together with the organic aluminum compound in the absence of effective amounts of a solvent, and the alkyl acetoacetate is metered into this mixture, B a reaction temperature which is as constant as possible at between 175° C. and 220° C., preferably between 180° C. and 200° C., is adjusted and C during the reaction the content of alkyl acetoacetate in the reaction mixture is adjusted to a value which is as constant as possible at between 1 and 3% by weight. It is advantageous in this process for the reaction temperature defined under B to be controlled by suitable variation of the heat input and/or by variation of the rate of addition of the alkyl acetoacetate, and for adequate mixing of the reaction mixture in the reaction vessel to be ensured This can be achieved with the aid of a stirrer, by pumping the reaction mixture through an external liquid circulation, by introducing the alkyl acetoacetate by means of a mixing nozzle or else by passing in a stream of inert gas. The process according to the invention is particularly suitable for the Carroll reaction of higher alcohols such as 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyl-1-octen-3-ol, 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (nerolidol), 3,7,11-trimethyl-1-dodecen-3-ol or 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol).
    • 本发明涉及一种改进的制备高级不饱和酮的方法,该方法通过在具有合适分馏塔的反应器系统中,在卡罗尔反应中使相应的α,β-不饱和醇与烷基乙酰乙酸酯反应,其中引入α,β-不饱和醇 在没有有效量的溶剂的情况下,将有机铝化合物与有机铝化合物一起加入到反应容器中,并将乙酰乙酸烷基酯计量加入到该混合物中,B在175℃和220℃之间的反应温度尽可能恒定 在反应过程中,优选在180℃和200℃之间调节和C,将反应混合物中乙酰乙酸烷基酯的含量调节至1至3重量%之间尽可能恒定的值。 在该方法中,通过适当变化的热输入和/或通过烷基的加成速率的变化来控制在B下限定的反应温度, 乙酰乙酸酯,并使反应混合物在反应容器中充分混合以确保这可以借助于搅拌器,通过泵送反应混合物通过外部液体循环,通过引入烷基乙酰乙酸酯通过混合喷嘴 或者通过流入惰性气体流。根据本发明的方法特别适用于高级醇如3,7-二甲基-1,6-辛二烯-3-醇(芳樟醇),3, 7,7-二甲基-1-辛烯-3-醇,3,7,11-三甲基-1,6,10-十二碳三烯-3-醇(橙花叔醇),3,7,11-三甲基-1-十二碳烯-3-醇 或3,7,11-三甲基-1,6-十二碳二烯-3-醇(二氢吗啉醇)。
    • 5. 发明授权
    • Process for preparing unsaturated ketones
    • 制备不饱和酮的方法
    • US06307106B1
    • 2001-10-23
    • US09440280
    • 1999-11-15
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerGerd KaibelHagen Jaedicke
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerGerd KaibelHagen Jaedicke
    • C07C4500
    • C07C45/68B01J19/1881B01J31/0211B01J2219/00038Y02P20/582C07C49/203
    • An improved process for preparing lower unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction in the presence of from 0.1 to 5 mol %, based on the alkyl acetoacetate to be reacted, of an organic aluminum compound as catalyst with elimination and continuous removal by distillation of the alkanol eliminated during the reaction from the alkyl acetoacetate in a reactor system with a fitted fractionation column, wherein A an &agr;,&bgr;-unsaturated alcohol which boils below 140° C. is introduced, in the absence of effective amounts of a solvent, together with the organic aluminum compound into the reaction vessel, B a reaction temperature which is as constant as possible between 170° C. and 250° C. is set under elevated pressure, C at this temperature, the alkyl acetoacetate is metered into the mixture, obtained in A, of the &agr;,&bgr;-unsaturated alcohol and the organic aluminum compound, and D during the reaction the content of alkyl acetoacetate in the reaction mixture is set at a value which is as constant as possible between 0.1 and 10% by weight.
    • 一种改进的制备低级不饱和酮的方法,该方法通过在卡罗尔反应中使相应的α,β-不饱和醇与烷基乙酰乙酸酯在0.1至5摩尔%存在下反应的待反应的乙酰乙酸烷基酯的有机铝化合物 作为催化剂,在具有适合的分馏塔的反应器系统中通过蒸馏从乙酰乙酸烷基酯反应中消除的烷醇消除并连续除去,其中引入沸点低于140℃的α,β-不饱和醇,在 没有有效量的溶剂与有机铝化合物一起进入反应容器B中,在170℃和250℃之间的反应温度一直保持在升高的压力下,在此温度下, 将乙酰乙酸烷基酯计量加入到A,得自α,β-不饱和醇和有机铝化合物的混合物中,并且在反应期间将D 将反应混合物中乙酰乙酸烷基酯的含量设定为0.1至10重量%之间尽可能恒定的值。
    • 9. 发明授权
    • Method and device for carrying out the distillative separation of C5+ cuts
    • 用于进行C5 +切割的蒸馏分离的方法和装置
    • US07169267B2
    • 2007-01-30
    • US10380551
    • 2001-09-19
    • Gerd KaibelCarsten OostManfred StroezelGerald MeyerPeter TrübenbachKarl-Heinz SartorJürgen Heners
    • Gerd KaibelCarsten OostManfred StroezelGerald MeyerPeter TrübenbachKarl-Heinz SartorJürgen Heners
    • B01D3/14B01D3/42
    • B01D3/141B01D3/14B01D3/146B01D3/4238C10G7/00C10G7/02C10G7/12Y10S203/20
    • A process is proposed for the separation of C5+ cuts by distillation into a low-boiler (A), a medium-boiler (B) and a high-boiler fraction (C) in one or more dividing-wall columns (TK), in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper, common column region (1), a lower, common column region (6), a feed part (2, 4) with rectifying section (2) and stripping section (4), and a withdrawal part (3, 5) with rectifying section (5) and stripping section (3), with feed of the C5+ cut (A, B, C) into the central region of the feed part (2, 4), discharge of the high-boiler fraction (C) from the bottom of the column, discharge of the low-boiler fraction (A) via the top of the column, and discharge of the medium-boiler fraction (B) from the central region of the withdrawal part (3, 5), wherein the dividing ratio of the liquid reflux at the upper end of the dividing wall (T) is set in such a way that the proportion of high-boiling key components in the liquid reflux over the stripping section (3) of the withdrawal part at the upper end of the dividing wall (T) is from 10 to 80%, preferably from 30 to 50%, of the limit value allowed in the medium-boiler fraction (B), and wherein the heating power in the evaporator at the bottom of the dividing-wall column (TK) is set in such a way that the concentration of the low-boiling key components in the liquid at the lower end of the dividing wall (T) is from 10 to 80%, preferably from 30 to 50%, of the limit value allowed in the medium-boiler fraction (B).
    • 提出了一种通过蒸馏将C 5+ H 3馏分分离成低沸点(A),中等锅炉(B)和高锅炉馏分(C)的方法,其中一个或多个 分隔壁(TK),其中分隔壁(T)沿柱的纵向方向布置,形成上部公共列区域(1),下部公共柱区域(6),进料 具有整流部分(2)和汽提部分(4)的部分(2,4)和具有整流部分(5)和汽提部分(3)的抽出部分(3,5),其中C 5 (A,B,C)进入进料部分(2,4)的中心区域,从塔底排出高沸点馏分(C),排出低沸点 馏分(A),并且从中间部分(3,5)的中心区域排出中间锅炉馏分(B),其中在上部的液体回流的分离比例 分隔壁(T)以这样的方式设置 在分隔壁(T)的上端的取出部分的汽提段(3)上的液体回流中的高沸点关键成分的比例为10〜80%,优选为30〜50% 在中间锅炉馏分(B)中允许的极限值,并且其中分隔壁塔(TK)底部的蒸发器中的加热功率被设定为使得低沸点关键成分 在分隔壁(T)的下端的液体中的中等锅炉馏分(B)中允许的极限值为10〜80%,优选为30〜50%。