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    METHOD FOR CONCENTRATING AQUEOUS 3-HYDROXY-2,2-DIMETHYLPROPANAL SOLUTION
    3.
    发明申请
    METHOD FOR CONCENTRATING AQUEOUS 3-HYDROXY-2,2-DIMETHYLPROPANAL SOLUTION 有权
    浓缩水性3-羟基-2,2-二甲基丙烯酸溶液的方法

    公开(公告)号：US20130334028A1

    公开(公告)日：2013-12-19

    申请号：US14002442

    申请日：2012-03-02

    Applicant: Yutaka Matsuura ,  Ikutaro Kuzuhara ,  Masahiro Yamane

    Inventor： Yutaka Matsuura ,  Ikutaro Kuzuhara ,  Masahiro Yamane

    IPC: C07C45/84

    CPC classification number: C07C45/84 ,  C07D319/06 ,  C07C47/19

    Abstract: The present invention provides a method for concentrating an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof, which includes subjecting a mixed solution of an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof and an azeotropic agent to azeotropic distillation in a distillation column to distil off water and the azeotropic agent from the mixed solution, wherein the mixed solution is prepared by adding, as the azeotropic agent, at least one selected from the group consisting of 1-butanol, 2-butanol, 2-methyl-1-propanol, 1-pentanol and 1-hexanol to the aqueous solution.

    Abstract translation: 本发明提供一种浓缩含有至少3-羟基-2,2-二甲基丙醛和/或其二聚体的水溶液的方法，其包括将含至少3-羟基-2,2-二甲基丙醛和/ 2-二甲基丙醛和/或其二聚体和共沸剂在蒸馏塔中共沸蒸馏以从混合溶液中蒸馏出水和共沸剂，其中混合溶液通过作为共沸剂至少加入至少 一种选自1-丁醇，2-丁醇，2-甲基-1-丙醇，1-戊醇和1-己醇的水溶液。

    Method for producing acetaldehyde from acetic acid
    4.
    发明授权
    Method for producing acetaldehyde from acetic acid 失效
    乙酸生产乙醛的方法

    公开(公告)号：US6121498A

    公开(公告)日：2000-09-19

    申请号：US69953

    申请日：1998-04-30

    Applicant: Gerald C. Tustin ,  Leslie S. Depew ,  Nick A. Collins

    Inventor： Gerald C. Tustin ,  Leslie S. Depew ,  Nick A. Collins

    IPC: B01J23/89 ,  C07B61/00 ,  C07C45/41 ,  C07C45/84 ,  C07C47/06 ,  C07C47/00 ,  B01J23/00 ,  B01J23/42 ,  C07C45/00

    CPC classification number: B01J23/8906 ,  C07C45/41 ,  Y02P20/582

    Abstract: A method of producing acetaldehyde hydrogenates acetic acid in the presence of an iron oxide catalyst containing between 2.5 and 90 wt % Pd, more preferably 10 and 80 wt % Pd and most preferably 20 and 60 wt % Pd. The catalyst has a specific surface area of less than 150 m.sup.2 /g. Hydrogen and acetic acid are fed to a reactor in a hydrogen to acetic acid ratio of 2:1 to 25:1, more preferably in a hydrogen to acetic acid ratio of 3:1 to 15:1 and most preferably in a hydrogen to acetic acid ratio of 4:1 to 12:1. The hydrogenation is performed at a temperature of about 250.degree. C. to 400.degree. C., more preferably about 270.degree. C. to 350.degree. C. and most preferably about 280.degree. C. to 325.degree. C. The hydrogenation of acetic acid produces a partially gaseous product, and acetaldehyde is absorbed from the partially gaseous product with a solvent containing acetic acid. The gas remaining after the absorption step contains hydrogen, and this gas is recycled for the hydrogenation of acetic acid. The absorbed acetaldehyde is distilled to isolate same. After acetaldehyde is isolated from unreacted acetic acid and the other products via distillation, the unreacted acetic acid is separated from the other products using azeotropic distillation. Water is contained in the other products, and the azeotrope is an azeotrope of ethyl acetate and water. The unreacted acetic acid is separated in a column, and the column is controlled to contain an ethyl acetate rich azeotrope of ethyl acetate and water.

    Abstract translation: 在含有2.5-90wt％Pd，更优选10和80wt％Pd，最优选20-60wt％Pd的氧化铁催化剂存在下，乙醛的制备方法使乙酸氢化。 催化剂的比表面积小于150m2 / g。 将氢和乙酸以2:1至25:1的氢气与乙酸的比例加入到反应器中，更优选以3:1至15:1的氢气至乙酸比例加入，最优选在氢气至乙酸 酸比为4：1至12：1。 氢化在约250℃至400℃，更优选约270℃至350℃，最优选约280℃至325℃的温度下进行。乙酸的氢化产生 部分气态产物，并且乙醛由含有乙酸的溶剂从部分气态产物中吸收。 吸收步骤后残留的气体含有氢气，该气体被再循环用于乙酸的氢化。 将吸收的乙醛蒸馏除去。 通过蒸馏从未反应的乙酸和其它产物中分离乙醛后，使用共沸蒸馏将未反应的乙酸与其它产物分离。 其他产物中含有水，共沸物是乙酸乙酯和水的共沸物。 将未反应的乙酸在柱中分离，并将柱控制为含有乙酸乙酯和水的乙酸乙酯富共沸物。

    Process for the preparation of fluorinated aromatic compounds
    5.
    发明授权
    Process for the preparation of fluorinated aromatic compounds 失效
    氟化芳族化合物的制备方法

    公开(公告)号：US6114589A

    公开(公告)日：2000-09-05

    申请号：US170381

    申请日：1998-10-13

    Applicant: Thomas Schach ,  Thomas Wessel ,  Maren Gutermuth

    Inventor： Thomas Schach ,  Thomas Wessel ,  Maren Gutermuth

    IPC: B01J31/02 ,  C07B39/00 ,  C07B61/00 ,  C07C45/63 ,  C07C45/84 ,  C07C47/55 ,  C07C201/12 ,  C07C201/16 ,  C07C205/12 ,  C07C253/30

    CPC classification number: C07C253/30 ,  C07B39/00 ,  C07C201/12 ,  C07C45/63

    Abstract: The invention relates to a process for the preparation of fluorinated compoundsAz.sub.x ArF.sub.w Cl.sub.(y-w) R.sub.z (1)in which Az is a radical --F, --Cl, --Br, --NO.sub.2, --CN, --CF.sub.3, --CCl.sub.3, --CHO, --CO(C.sub.n H.sub.2n+1), --COX or --SO.sub.2 X, where X is F, Cl or Br, x is an integer from 1 to 3, Ar is a phenyl radical, pyridyl radical or naphthyl, w is an integer from 1 to y, y is an integer from 1 to 5, R is H, an alkyl radical or an alkoxy radical having from 1 to 10 carbon atoms, z is an integer from 1 to 5, (x+y+z) is the number of all substitutable valences on the radical Ar, which comprises reacting a compoundAz.sub.x ArCl.sub.y R.sub.z (2),with an alkali metal fluoride in the presence of a component a) or a mixture of component a) and at least one of components b), c), d) and/or e), component a) being one or more quaternary ammonium compounds which contain one or more radicals --(C.sub.m H.sub.2m O)R.sup.5, component b) being an amidophosphonium salt, component c) being a quaternary ammonium salt, component d) being a quaternary phosphonium salt, component e) being a polyether, and carrying out the reaction at from 50 to 250.degree. C., removing the compound of the formula (1) formed during the reaction by distillation, and the compound of the formula (2) is fed to the reaction mixture at a rate corresponding to the rate at which the compound of the formula (1) is removed.

    Abstract translation: 本发明涉及一种制备氟化化合物的方法，其中Z 1为基团-F，-Cl，-Br，-NO 2，-CN，-CF 3，-CCl 3，-CHO - ， - CO（CnH2n + 1），-COX或-SO2X，其中X为F，Cl或Br，x为1至3的整数，Ar为苯基，吡啶基或萘基，w为1至y的整数 y为1〜5的整数，R为H，烷基或碳原子数为1〜10的烷氧基，z为1〜5的整数，（x + y + z）为全部数 在基团Ar上具有可取代价，其包括使化合物AZxArClyRz（2）与碱金属氟化物在组分a）或组分a）和组分b），c），d）中的至少一种的存在下反应， 和/或e）组分a）是一种或多种含有一个或多个基团的季铵化合物 - （CmH2mO）R5，组分b）是酰胺鏻盐，组分c）是季铵盐，组分d）是 季鏻盐，组分e）b 取代聚醚，并在50-250℃下进行反应，通过蒸馏除去反应期间形成的式（1）化合物，将式（2）化合物加入到反应混合物中 对应于除去式（1）的化合物的速率的速率。

    Separation of 3,3-dimethylacrolein and -methyl-3-buten-1-ol by azeotropic distillation with water and glycerol
    8.
    发明授权
    Separation of 3,3-dimethylacrolein and -methyl-3-buten-1-ol by azeotropic distillation with water and glycerol 失效
    通过与水和甘油共沸蒸馏分离3,3-二甲基丙烯醛和 - 甲基-3-丁烯-1-醇

    公开(公告)号：US3894916A

    公开(公告)日：1975-07-15

    申请号：US39282173

    申请日：1973-08-29

    Applicant: BASF AG

    Inventor： FISCHER ROMAN ,  MAIER SIEGFRIED ,  KOERNIG WOLFGANG

    IPC: C07C27/30 ,  B01J23/00 ,  C07B61/00 ,  C07C27/00 ,  C07C29/80 ,  C07C33/02 ,  C07C33/025 ,  C07C45/00 ,  C07C45/84 ,  C07C47/20 ,  C07C47/21 ,  C07C67/00 ,  B01D3/34

    CPC classification number: C07C45/84 ,  C07C47/21

    Abstract: A process for separating, by distillation, a mixture consisting essentially of 3,3-dimethylacrolein and 3-methyl-3-buten-1-ol, wherein the mixture to be separated is distilled in the presence of water and glycerol, the 3,3-dimethyl-acrolein first being distilled off azeotropically with water and the 3-methyl-3-buten1-ol then being separated, as an azeotropic mixture with water, from the higher-boiling glycerol. It is also possible to isolate the 3,3-dimethylacrolein by distillation if the 3-methyl-3-buten1-ol is partially replaced by 3-methyl-2-buten-1-ol. The 3,3dimethylacrolein, which can be isolated in pure form by the process of the invention, is a valuable intermediate for the synthesis of natural substances such as citral, vitamin A and chrysanthemic acid.

    Abstract translation: 通过蒸馏分离基本上由3,3-二甲基丙烯醛和3-甲基-3-丁烯-1-醇组成的混合物的方法，其中待分离的混合物在水和甘油的存在下蒸馏， 首先与水共沸蒸馏出3-三甲基 - 丙烯醛，然后将3-甲基-3-丁烯-1-醇与较高沸点甘油作为与水的共沸混合物分离。 如果3-甲基-3-丁烯-1-醇部分被3-甲基-2-丁烯-1-醇代替，也可以通过蒸馏分离3,3-二甲基丙烯醛。 可以通过本发明的方法以纯形式分离的3,3-二甲基丙烯醛是合成天然物质如柠檬醛，维生素A和菊酸的有价值的中间体。

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