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    • 2. 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)。
    • 4. 发明申请
    • METHOD FOR THE CONTINUOUS SEPARATION OF MIXTURES COMPRISING MORPHOLINE (MO), MONOAMINODIGLYCOL (ADG), AMMONIA AND WATER BY MEANS OF DISTILLATION
    • 通过蒸馏法连续分离包含摩尔(MO),单胺基(ADG),氨和水的混合物的方法
    • US20100084257A1
    • 2010-04-08
    • US12443563
    • 2007-09-12
    • Helmut SchmidtkeOliver BussmannRalph VerschUdo RheudeUwe LeykManfred JuliusMartin RudloffErhard Henkes
    • Helmut SchmidtkeOliver BussmannRalph VerschUdo RheudeUwe LeykManfred JuliusMartin RudloffErhard Henkes
    • C07C213/10C07D295/02B01D3/14C07C217/08
    • C07D295/027
    • Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K10; (ii) feeding a bottom fraction from K10 to a second distillation column K20 in which water and organic products are separated off at the top at a temperature at the top in the range from 45 to 198° C. and a pressure in the range from 0.1 to 15 bar, (iii) feeding a bottom fraction from K20 to a third distillation column K30, wherein the column K30 is a dividing wall column (DWC) which preferably has a dividing wall (DW) in the longitudinal direction of the column to form an upper combined column region (1), a lower combined column region (6), an inflow part (2, 4) having an enrichment section (2) and a stripping section (4), and also an offtake part (3, 5) having an enrichment section (3) and a stripping section (5), with the bottoms from K20 being fed in in the upper or middle third of the inflow part (2, 4), based on the number of theoretical plates of the inflow part, ADG and organic products having a boiling point of >190° C. (1.013 bar) being discharged at the bottom, organic products having a boiling point of ≦128° C. (1.013 bar) being discharged at the top and MO being discharged from the middle or lower third of the offtake part (3, 5) (side offtake), based on the number of theoretical plates of the offtake part.
    • 用于从二甘醇(DEG)与氨的反应连续分馏含有吗啉(MO),单氨基二甘醇(ADG),氨和水的混合物的方法,该方法包括:(i)在 第一蒸馏塔K10顶部; (ii)将底部馏分从K10进料至第二蒸馏塔K20,其中水和有机产物在顶部分离出,顶部温度为45-98℃,压力范围为 0.1至15巴,(iii)从K20向第三蒸馏塔K30供给底部馏分,其中塔K30是分隔壁塔(DWC),其优选在塔的纵向方向上具有分隔壁(DW)至 形成上部组合列区域(1),下部组合列区域(6),具有浓缩部分(2)和剥离部分(4)的流入部分(2,4),以及出口部分(3, 5)具有富集部分(3)和汽提部分(5),其中来自K20的底部在流入部分(2,4)的上部或中部三分之一中被输入,基于理论塔板的数量 流入部件,ADG和沸点> 190℃(1.013巴)的有机产物在底部排出,有机原料 沸点为≦̸ 128℃(1.013巴)在顶部排出,MO从出料部(3,5)的中部或下部三分之一(出口侧)排出,基于 理论板的出口部分。
    • 7. 发明授权
    • Process for preparing ionones
    • 紫罗兰酮的制备方法
    • US06288282B1
    • 2001-09-11
    • US09567268
    • 2000-05-09
    • Udo RheudeUlrich HörcherDietmar WellerManfred Stroezel
    • Udo RheudeUlrich HörcherDietmar WellerManfred Stroezel
    • C07C4921
    • C07C403/16C07C2601/16
    • Process for the continuous preparation of &agr;- and/or &bgr;-ionone or homologous compounds using concentrated sulfuric acid at temperatures from 20 to 90° C., in the presence of organic solvents or diluents with cooling and by subsequent termination of the reaction by hydrolysis of the reaction mixture with water or dilute sulfuric acid, wherein both the cyclization of pseudoionones and the subsequent hydrolysis of the reaction mixture are carried out in a virtually adiabatic reaction in one or more reaction mixing pump(s) which are connected in series and each of which consists essentially of a rotationally symmetrical mixing chamber formed from a peripheral wall and two end walls and of a mixing rotor made of material inert to sulfuric acid and with rotational drive, where the mixing chamber has at least one inlet opening for each component and one outlet opening for the reaction mixture, and annular channels in fluid connection to one another in the end walls, and wherein the heat of the two reactions is in each case partly or wholly removed with the aid of a downstream heat exchanger.
    • 使用浓硫酸在20〜90℃的温度下,在有机溶剂或稀释剂存在下,在冷却下,随后通过水解终止反应,连续制备α-和/或β-紫罗兰酮或同系化合物的方法 反应混合物与水或稀硫酸反应,其中假戊烯酮的环化和随后的反应混合物的水解在一个或多个反应混合泵中实质上绝热的反应中进行,所述反应混合泵串联连接, 其基本上由旋转对称的混合室组成,该混合室由周壁和两个端壁以及由硫酸惰性且具有旋转驱动的材料制成的混合转子,其中混合室具有用于每个部件的至少一个入口, 用于反应混合物的一个出口,以及在端壁中彼此流体连接的环形通道,其中热量 在每种情况下,两个反应在下游热交换器的帮助下部分或全部去除。