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    Method for producing vinyl esters
    3.
    发明授权
    Method for producing vinyl esters 有权
    乙烯基酯的制备方法

    公开(公告)号：US09174922B2

    公开(公告)日：2015-11-03

    申请号：US14372290

    申请日：2013-01-18

    Applicant: Oxea GmbH

    Inventor： Leif Johnen ,  Heinz Strutz ,  Kurt Schalapski ,  Norman Nowotny ,  Wolfgang Höfs ,  Sebastian Geisel

    IPC: C07C67/10 ,  C07C67/333 ,  C07C69/01 ,  C07C67/54

    CPC classification number: C07C67/333 ,  C07C67/10 ,  C07C67/54 ,  C07C69/01 ,  C07C69/24 ,  C07C69/78

    Abstract: The present invention relates to a continuous, catalytic process for preparing a vinyl ester of the formula R—C(O)O—CH═CH2 by reaction of a carboxylic acid of the formula R—C(O)OH with a transvinylating reagent of the formula R1—C(O)O—CH═CH2, wherein the reaction is effected at a temperature of 90 to 160° C. and at a pressure of 0.5 to 15 MPa without withdrawal of a reactant in the presence of a transition metal catalyst containing at least one transition metal from the group of ruthenium, osmium, rhodium, iridium, palladium and platinum, and then the resulting reaction mixture is separated into its constituents.

    Abstract translation: 本发明涉及通过式R-C（O）OH的羧酸与式R-C（O）OH的羧酸反应制备式R-C（O）O-CH = CH 2的乙烯基酯的连续催化方法， 式R 1 -C（O）O-CH = CH 2，其中反应在90至160℃的温度和0.5至15MPa的压力下进行，而在过渡金属的存在下不引发反应物 含有来自钌，锇，铑，铱，钯和铂的至少一种过渡金属的催化剂，然后将所得反应混合物分离成其组分。

    Transvinylation as a first stage of coupling production of vinyl esters and acetic acid or propionic acid reaction products
    4.
    发明授权
    Transvinylation as a first stage of coupling production of vinyl esters and acetic acid or propionic acid reaction products 有权
    作为乙烯基酯和乙酸或丙酸反应产物的偶联生产的第一阶段的转乙烯化

    公开(公告)号：US09174921B2

    公开(公告)日：2015-11-03

    申请号：US14372235

    申请日：2013-01-18

    Applicant: Oxea GmbH

    Inventor： Leif Johnen ,  Heinz Strutz

    IPC: C07C67/10 ,  C07C69/01 ,  C07C29/149 ,  C07C67/055 ,  C07C67/08 ,  C07C67/54 ,  C07C51/02 ,  C07C51/09 ,  C07C51/363 ,  C07C67/333

    CPC classification number: C07C67/333 ,  C07C29/149 ,  C07C51/02 ,  C07C51/09 ,  C07C51/363 ,  C07C67/055 ,  C07C67/08 ,  C07C67/10 ,  C07C67/54 ,  C07C69/01 ,  C07C69/24 ,  C07C69/78 ,  C07C53/16 ,  C07C53/19 ,  C07C69/15 ,  C07C31/08 ,  C07C31/10 ,  C07C53/40 ,  C07C53/42 ,  C07C53/12 ,  C07C53/122 ,  C07C53/08 ,  C07C69/14

    Abstract: Process for coproduction of a vinyl ester of the formula R—C(O)O—CH═CH2 by transvinylation reaction of a carboxylic acid of the formula R—C(O)OH with a transvinylating reagent of the formula R1—C(O)O—CH═CH2, characterized in that (a) the transvinylation reaction is conducted continuously at a temperature of 90 to 160° C. and at a pressure of 0.5 to 15 MPa without withdrawal of a reactant in the presence of a transition metal catalyst containing at least one transition metal selected from the group of ruthenium, osmium, rhodium, iridium, palladium and platinum; (b) the resulting reaction mixture is separated into its constituents and the vinyl ester of the formula R—C(O)O—CH═CH2 and the carboxylic acid of the formula R1—C(O)—OH are removed; and (c) the carboxylic acid obtained after step (b) is converted to a derivative of the formula R1—C(O)—X, R1—CH2—OH or R6—C(O)—OH in which X is vinyloxy, O—CH═CH2, halogen, alkoxy of the formula OR2 in which R2 is a substituted or unsubstituted hydrocarbyl radical having 1 to 10 carbon atoms, amino of the formula NR3R4 in which R3 and R4 are each independently hydrogen or a substituted or unsubstituted hydrocarbyl radical having 1 to 10 carbon atoms, or carboxyl of the formula O—C(O)—R5 in which R5 is hydrogen or a substituted or unsubstituted hydrocarbyl radical having 1 to 10 carbon atoms, and R6 is the partly or fully halogen-substituted R1 radical.

    Abstract translation: 通过式R-C（O）OH的羧酸与式R1-C（O）的转乙烯化试剂进行反式化反应，共同制备式R-C（O）O-CH = CH 2的乙烯基酯的方法 ）O-CH = CH 2，其特征在于：（a）在90至160℃的温度和0.5至15MPa的压力下连续进行转化反应，而在过渡金属存在下不引发反应物 含有选自钌，锇，铑，铱，钯和铂中的至少一种过渡金属的催化剂; （b）将所得反应混合物分离成其组分，并且除去式R-C（O）O-CH = CH 2的乙烯基酯和式R 1 -C（O）-OH的羧酸; 和（c）将步骤（b）后获得的羧酸转化为其中X为乙烯氧基的式R 1 -C（O）-X，R 1 -CH 2 -OH或R 6 -C（O）-OH的衍生物， O-CH = CH 2，卤素，式OR 2的烷氧基，其中R 2是具有1至10个碳原子的取代或未取代的烃基，式NR 3 R 4的氨基，其中R 3和R 4各自独立地为氢或取代或未取代的烃基 具有1-10个碳原子的基团，或其中R 5是氢的式O-C（O）-R 5的羧基或具有1至10个碳原子的取代或未取代的烃基，R 6是部分或完全卤素取代的 R1激进。

    Method for recovering di-trimethylolpropane and trimethylolpropane-enriched product streams from the side streams of trimethylolpropane production
    6.
    发明授权
    Method for recovering di-trimethylolpropane and trimethylolpropane-enriched product streams from the side streams of trimethylolpropane production 有权
    从三羟甲基丙烷生产的侧流回收二羟甲基丙烷和三羟甲基丙烷富集产物流的方法

    公开(公告)号：US09045451B2

    公开(公告)日：2015-06-02

    申请号：US14351205

    申请日：2012-10-24

    Applicant: Oxea GmbH

    Inventor： Guido D. Frey ,  Thorsten Kreickmann ,  Heinz Strutz

    IPC: C07C41/42 ,  C07C29/10 ,  C07D319/06 ,  C07C29/80 ,  C07C29/90 ,  C07C41/44

    CPC classification number: C07D319/06 ,  C07C29/10 ,  C07C29/80 ,  C07C29/90 ,  C07C41/42 ,  C07C41/44 ,  C07C31/22 ,  C07C43/132

    Abstract: Process for obtaining ditrimethylolpropane and trimethylolpropane-enriched product streams from the high-boiling fractions and residues which are obtained in the distillative purification of trimethylolpropane, characterized in that these high-boiling fractions and residues are combined and a polar solvent is added to produce a solution and the solution is treated at a temperature of 120 to 280° C. and at a pressure of 2 to 25 MPa with hydrogen in the presence of a solid nickel catalyst and an acidic compound. After catalytic treatment, the solution is subjected to multi-stage distillation including with a thin film evaporator with a column attachment in order to recover ditrimethylolpropane and trimethylolpropane-enriched product streams.

    Abstract translation: 从三沸石馏分和三羟甲基丙烷的蒸馏提纯中获得的高沸点馏分和残余物获得三羟甲基丙烷和三羟甲基丙烷富集产物流的方法，其特征在于将这些高沸点馏分和残余物合并，加入极性溶剂以产生溶液 在固体镍催化剂和酸性化合物的存在下，用氢气在120〜280℃的温度和2〜25MPa的压力下处理溶液。 在催化处理后，将溶液进行多级蒸馏，包括用柱式附件的薄膜蒸发器，以回收二羟甲基丙烷和富含三羟甲基丙烷的产物流。

    Method for obtaining polyol esters-enriched product streams from the side-streams in polyol ester production
    9.
    发明授权
    Method for obtaining polyol esters-enriched product streams from the side-streams in polyol ester production 有权

    公开(公告)号：US09840454B2

    公开(公告)日：2017-12-12

    申请号：US14915915

    申请日：2014-10-09

    Applicant: Oxea GmbH

    Inventor： Jens Kubitschke ,  Thorsten Kreickmann ,  Jörg Arnold ,  Heinz Strutz

    IPC: C07C67/54 ,  C07C67/08 ,  C07C67/58 ,  C07C67/60

    CPC classification number: C07C67/54 ,  C07C67/08 ,  C07C67/58 ,  C07C67/60 ,  C07C69/28

    Abstract: A process for obtaining product streams enriched with polyol esters from the secondary streams from polyol ester preparation, comprising a) the reaction of polyols of the general formula (II) H—(—O—[—CR1R2—]m—)o—OH  (II) in which R1 and R2 are each independently hydrogen, an alkyl radical having 1 to 5 carbon atoms or a hydroxyalkyl radical having 1 to 5 carbon atoms, m is an integer from 1 to 10, o is an integer from 2 to 15, with linear or branched aliphatic monocarboxylic acids having 3 to 20 carbon atom, with removal of the water formed; b) the removal of unconverted starting compounds from the crude ester formed; c) the treatment of the crude ester obtained in step b) with steam to form a volatile secondary stream; and d) the removal of the volatile secondary stream obtained in step c), characterized in that the volatile secondary stream obtained in step d) is separated into an aqueous phase and an organic phase and the organic phase removed is subjected to a further treatment with steam and a product stream enriched with polyol esters is obtained as residue.

    Method for producing 2-methylbutanal from the secondary flows arising in the production of mixtures of isomeric alpha, beta-unsaturated decenals
    10.
    发明授权
    Method for producing 2-methylbutanal from the secondary flows arising in the production of mixtures of isomeric alpha, beta-unsaturated decenals 有权
    从生产异构α，β-不饱和癸烯的混合物中产生的二次流产生2-甲基丁醛的方法

    公开(公告)号：US09517991B2

    公开(公告)日：2016-12-13

    申请号：US15033661

    申请日：2014-11-14

    Applicant: Oxea GmbH

    Inventor： Jens Theuerkauf ,  Heinz Strutz

    IPC: C07C45/50 ,  C07C45/62 ,  C07C29/00 ,  C07C45/82 ,  C07C45/74 ,  C07C29/17

    CPC classification number: C07C45/82 ,  C07C29/175 ,  C07C45/50 ,  C07C45/62 ,  C07C45/74 ,  C07C47/02 ,  C07C47/21

    Abstract: A process for preparing 2-methylbutanal from the secondary streams obtained in the preparation of mixtures of isomeric α,β-unsaturated decenals, characterized in that a) a mixture comprising linear butenes is reacted in the presence of transition metal compounds of group VIII of the Periodic Table of the Elements with carbon monoxide and hydrogen at elevated temperature and elevated pressure to give a pentanal mixture; b) the pentanal mixture obtained in step a) is converted in the presence of basic compounds to a mixture of isomeric α,β-unsaturated decenals; and c) the mixture obtained in step b) is separated into a stream enriched with unconverted 2-methylbutanal and a stream enriched with a mixture of isomeric α,β-unsaturated decenals; with the proviso that the stream which has been separated off in step c) and is enriched with unconverted 2-methylbutanal is reacted with formaldehyde.

    Abstract translation: 在制备异构α，β-不饱和癸醛的混合物中获得的二次流中制备2-甲基丁醛的方法，其特征在于a）包含线性丁烯的混合物在第VIII族的过渡金属化合物存在下反应 元素周期表与一氧化碳和氢气在升高的温度和升高的压力下得到戊醛混合物; b）将步骤a）中获得的戊醛混合物在碱性化合物的存在下转化成异构α，β-不饱和癸醛的混合物; 和c）将步骤b）中获得的混合物分离成富含未转化的2-甲基丁醛的流和富含异构α，β-不饱和癸醛混合物的流; 条件是在步骤c）中分离并富集未转化的2-甲基丁醛的料流与甲醛反应。

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