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    Process for separating acetone from carbonylation mixtures
    1.
    发明授权
    Process for separating acetone from carbonylation mixtures 失效
    从羰基化混合物中分离丙酮的方法

    公开(公告)号：US4444624A

    公开(公告)日：1984-04-24

    申请号：US412225

    申请日：1982-08-27

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： C07C45/00 ,  C07C45/49 ,  C07C45/78 ,  C07C45/82 ,  C07C45/83 ,  C07C49/08 ,  C07C67/00 ,  B01D3/40

    CPC分类号： C07C45/82 ,  C07C45/49 ,  C07C45/83

    摘要： The disclosure relates to a process for separating acetone from reaction mixtures originating from the reaction of methyl acetate and/or dimethylether with carbon monoxide and optionally hydrogen in the presence of a catalyst system consisting of carbonyl complexes of noble metals of group VIII of the Periodic System of the elements, acetic acid, an organophosphorus or organonitrogen compound, methyl iodide and optionally carbonyl-yielding compounds of common metals. To this end, the disclosure provides for the reaction mixture containing acetic anhydride, acetic acid, ethylidene diacetate, methyl iodide, acetone and methyl acetate which is distilled off from the catalyst solution, or just its low boiler fraction consisting of methyl acetate, methyl iodide and acetone to be subjected wholly or partially to an extractive distillation with acetic acid and for pure methyl iodide to be distilled off; for an acetone/methyl acetate mixture to be distilled off from the acetic acid extract; for this mixture to be separated in known fashion and for the acetic acid extractant to be recycled into the extraction stage, if desired after separation of the final reaction products comprised of acetic anhydride; ethylidene diacetate and acetic acid.

    摘要翻译： 本公开内容涉及在由周期性系统VIII族的贵金属的羰基络合物组成的催化剂体系的存在下，从丙酸甲酯和/或二甲醚与一氧化碳和任选的氢气反应的反应混合物中分离丙酮的方法 的元素，乙酸，有机磷或有机氮化合物，甲基碘和任选的产生羰基的常见金属化合物。 为此，本公开内容提供了从催化剂溶液中蒸馏掉的乙酸酐，乙酸，亚乙基二乙酸酯，甲基碘，丙酮和乙酸甲酯的反应混合物，或仅仅是其由乙酸甲酯，甲基碘 和丙酮完全或部分地进行与乙酸的萃取蒸馏，并将纯甲基碘蒸馏出; 对于从乙酸提取物中蒸出的丙酮/乙酸甲酯混合物; 为了将该混合物以已知方式分离，并且乙酸萃取剂再循环到萃取阶段，如果需要，在分离由乙酸酐组成的最终反应产物之后; 亚乙基二乙酸酯和乙酸。

    Process for making carboxylic acid halides
    5.
    发明授权
    Process for making carboxylic acid halides 失效
    制备羧酸卤化物的方法

    公开(公告)号：US4543217A

    公开(公告)日：1985-09-24

    申请号：US561805

    申请日：1983-12-15

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： B01J31/28 ,  C07B61/00 ,  C07C51/58 ,  C07C53/40 ,  C07C53/42 ,  C07C57/72

    CPC分类号： C07C51/58

    摘要： The disclosure relates to a process for making carboxylic acid halides by reacting an alkyl halide having 1 to 6 carbon atoms or aryl halide with carbon monoxide, optionally in admixture with up to 30 volume % hydrogen, under practically anhydrous conditions at temperatures of 350 to 575 K under pressures of 1 to 300 bars in the presence of a catalyst system containing at least one noble metal belonging to group VIII of the Periodic System of the elements or its compounds, iodine and/or its compounds and optionally an inert organic solvent. To this end, the disclosure provides for use to be made of a catalyst system which additionally contains a compound of the elements belonging to groups I to III of the Periodic System, and acetic acid.

    摘要翻译： 本公开内容涉及通过使具有1至6个碳原子的烷基卤或芳基卤化物与一氧化碳，任选地与至多30体积％的氢混合，在几乎无水条件下在350至575℃的温度下反应来制备羧酸卤化物的方法 在含有至少一种属于元素或其化合物的周期体系的VIII族的贵金属的催化剂体系存在下，在1至300巴的压力下，碘和/或其化合物和任选的惰性有机溶剂。 为此，本公开提供了使用另外含有属于周期系统的第I至III族的元素的化合物和乙酸的催化剂体系。

    Process for making carboxylic acid halides
    7.
    发明授权
    Process for making carboxylic acid halides 失效
    制备羧酸卤化物的方法

    公开(公告)号：US4414160A

    公开(公告)日：1983-11-08

    申请号：US301984

    申请日：1981-09-14

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： C07C53/38 ,  C07C51/58

    CPC分类号： C07C51/58

    摘要： The invention relates to the manufacture of carboxylic acid halides. To this end, an alkyl halide having from 1 to 6 carbon atoms or an aryl halide is reacted with carbon monoxide under practically anhydrous conditions at temperatures of 350 to 575 K. and under pressures of 1 to 300 bars in the presence of a catalyst system containing at least one of the noble metals selected from rhodium, palladium, iridium or their compounds, iodine and/or its compounds, methyl trialkyl phosphonium iodide and/or methyl triaryl phosphonium iodide, and optionally trialkyl phosphine oxide or triaryl phosphine oxide as well as an inert organic solvent. More specifically, the reaction mixture is admixed with 0.02 to 0.75 mol of hydrogen per mol of carbon monoxide.

    摘要翻译： 本发明涉及羧酸卤化物的制造。 为此，将具有1至6个碳原子的烷基卤或芳基卤化物在几乎无水条件下在350至575K的温度和1至300巴的压力下，在催化剂体系存在下与一氧化碳反应 含有选自铑，钯，铱或它们的化合物中的至少一种贵金属，碘和/或其化合物，碘化甲基三烷基碘和/或碘化三甲基三碘化鏻，和任选的三烷基氧化膦或三芳基氧化膦以及 惰性有机溶剂。 更具体地，将反应混合物与每摩尔一氧化碳0.02至0.75摩尔的氢气混合。

    Process for purifying and recovering contaminated catalyst solution obtained in the carbonylation of methyl acetate and/or dimethylether
    8.
    发明授权
    Process for purifying and recovering contaminated catalyst solution obtained in the carbonylation of methyl acetate and/or dimethylether 失效
    用于纯化和回收在乙酸甲酯和/或二甲醚的羰基化中获得的污染的催化剂溶液的方法

    公开(公告)号：US4629711A

    公开(公告)日：1986-12-16

    申请号：US852222

    申请日：1986-04-15

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： C07C53/12 ,  B01J31/00 ,  B01J31/20 ,  B01J31/40 ,  B01J38/00 ,  B01J38/52 ,  C07B61/00 ,  C07C27/00 ,  C07C51/00 ,  C07C51/48 ,  C07C51/54 ,  C07C51/573 ,  C07C67/00 ,  C07C67/37 ,  C07C69/16 ,  B01J38/68 ,  C01G55/00 ,  C07C51/56

    CPC分类号： B01J31/0268 ,  B01J31/0239 ,  B01J31/20 ,  B01J31/4046 ,  B01J38/52 ,  C07C51/48 ,  C07C51/573 ,  B01J2231/34 ,  B01J2531/822 ,  Y02P20/584

    摘要： Catalyst solution contaminated during the carbonylation of methyl acetate and/or dimethylether, containing carbonyl complexes of rhodium, quaternary heterocyclic aromatic nitrogen compounds or quaternary organophosphorus compounds as organic promoters, undistillable organic contaminants, acetic acid, acetic anhydride and ethylidene diacetate, is purified and recovered. To this end the contaminated catalyst solution is extracted with a dialkylether having from 1-4 carbon atoms and thereby freed from its organic contaminants, acetic acid, acetic anhydride and ethylidene diacetate, and the ether phase is separated from a precipitated promoter-containing catalyst complex; the ether phase is treated with iodine and/or methyl iodide, a further portion of precipitated promoter-containing catalyst complex is separated and united with the purified catalyst complex; the ether phase is distillatively separated into its constituents, recovered dialkylether is used for extraction, and fresh catalyst solution is prepared from the recovered mixture of acetic acid, acetic anhydride and ethylidene diacetate and united purified catalyst complex, and the organic contaminants retained in the residue coming from the ether phase distillation are expelled, and the purified catalyst is distillatively freed from residual dialkylether.

    摘要翻译： 将含有铑，四元杂环芳族氮化合物或季有机磷化合物的羰基络合物的乙酸甲酯和/或二甲醚羰基化的催化剂溶液作为有机促进剂，不可渗透的有机污染物，乙酸，乙酸酐和亚乙基二乙酸酯被纯化和回收 。 为此，将污染的催化剂溶液用具有1-4个碳原子的二烷基醚萃取，从而除去其有机污染物，乙酸，乙酸酐和亚乙基二乙酸酯，并将醚相与沉淀的含促进剂的催化剂络合物 ; 用碘和/或甲基碘处理醚相，将另一部分含沉淀促进剂的催化剂络合物分离并与纯化的催化剂络合物结合; 将醚相蒸馏分离成其成分，回收的二烷基醚用于萃取，从回收的乙酸，乙酸酐和亚乙基二乙酸酯混合物中制备新鲜的催化剂溶液，并将合并的纯化催化剂配合物，残留在残渣中的有机污染物 从乙醚相蒸馏得到的馏分被排出，纯化的催化剂蒸馏除去剩余的二烷基醚。

    Process for purifying and recovering contaminated catalyst solution obtained in the carbonylation of methyl acetate and/or dimethylether
    9.
    发明授权
    Process for purifying and recovering contaminated catalyst solution obtained in the carbonylation of methyl acetate and/or dimethylether 失效
    用于纯化和回收在乙酸甲酯和/或二甲醚的羰基化中获得的污染的催化剂溶液的方法

    公开(公告)号：US4442304A

    公开(公告)日：1984-04-10

    申请号：US402942

    申请日：1982-07-29

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： C07C67/37 ,  B01J31/40 ,  B01J38/00 ,  C07B61/00 ,  C07C27/00 ,  C07C51/00 ,  C07C51/12 ,  C07C51/42 ,  C07C51/573 ,  C07C53/08 ,  C07C53/12 ,  C07C67/00 ,  C07C69/16 ,  C07C67/36 ,  C07C51/56

    CPC分类号： B01J31/20 ,  B01J31/0239 ,  B01J31/0268 ,  B01J31/4038 ,  B01J31/4046 ,  B01J31/4092 ,  C07C51/42 ,  C07C51/573 ,  B01J2231/34 ,  B01J2531/82 ,  B01J2531/822 ,  B01J2531/824 ,  Y02P20/584

    摘要： The disclosure relates to a process for purifying and recovering a contaminated catalyst solution which is obtained in the carbonylation of methyl acetate and/or dimethylether, the catalyst solution containing carbonyl complexes of noble metals of group VIII of the Periodic System of the elements, quaternary heterocyclic aromatic nitrogen compounds or quaternary organophosphorus compounds as organic promoters, undistillable organic contaminants as well as acetic acid, acetic anhydride and ethylidene diacetate. To this end, the disclosure provides for the catalyst solution to be distillatively freed from its volatile constituents and for the remaining solid distillation residue to be water-treated, the noble metal/carbonyl-complex being precipitated together with the organic contaminants and the organic promoter becoming dissolved; for the precipitated and contaminated noble metal/carbonyl-complex to be removed by filtration and to be freed from the organic contaminants by extraction with aliphatic ethers; for the organic promoter to be recovered by evaporating the water or extracting it with halogenated hydrocarbons and for these latter to be evaporated; and for the purified noble metal/carbonyl-complex and the recovered organic promoter to be recycled into the carbonylation reaction.

    摘要翻译： 本公开涉及一种净化和回收在乙酸甲酯和/或二甲醚的羰基化中获得的污染的催化剂溶液的方法，所述催化剂溶液含有元素周期系的VIII族贵金属的羰基络合物，四元杂环 芳族氮化合物或季有机磷化合物作为有机促进剂，不可否认的有机污染物以及乙酸，乙酸酐和亚乙基二乙酸酯。 为此，本公开内容提供催化剂溶液可蒸馏除去其挥发性成分，并且剩余的固体蒸馏残余物被水处理，贵金属/羰基络合物与有机污染物和有机促进剂一起沉淀 变得溶解 用于通过过滤除去沉淀和污染的贵金属/羰基络合物，并通过用脂族醚萃取除去有机污染物; 通过蒸发水或用卤代烃提取有机助催化剂并使其后者被蒸发来回收有机促进剂; 并且将纯化的贵金属/羰基络合物和回收的有机促进剂再循环到羰基化反应中。

    Process for the manufacture of acrylic acid
    10.
    发明授权
    Process for the manufacture of acrylic acid 失效
    制备丙烯酸的方法

    公开(公告)号：US3985800A

    公开(公告)日：1976-10-12

    申请号：US393347

    申请日：1973-08-31

    申请人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    发明人： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

    IPC分类号： B01J23/00 ,  B01J23/882 ,  B01J35/10 ,  B01J37/00 ,  C07B61/00 ,  C07C51/00 ,  C07C51/25 ,  C07C57/055 ,  C07C67/00 ,  C07C57/04 ,  C07C51/26

    CPC分类号： B01J37/0018 ,  B01J23/882 ,  B01J35/10 ,  B01J37/0009 ,  C07C51/252 ,  B01J35/1009 ,  B01J35/1038

    摘要： Production of acrylic acid by reacting acrolein with molecular oxygen in the presence of steam and, if desired, inert gases at elevated temperature in contact with a fixed bed of cobalt molybdate catalyst prepared by precipitating cobalt molybdate from the combined aqueous solutions of a cobalt salt, of a molybdenum compound and of ammonia at a temperature of about 60.degree.C and at a pH of at most 7; filtering off, washing and drying the precipitate at a temperature of at least 100.degree.C; heating the dry cobalt molybdate for several hours at elevated temperatures, grinding and transforming it into shapes; and sintering the cobalt molybdate shapes for several hours. The acrylic acid is more particularly produced in contact with a catalyst prepared by combining the aqueous solution of the cobalt salt with that of the molybdenum compound in the atomic ratio of Co:Mo of about 1.05:1; establishing in the combined solutions a pH between 3.8 and 6.0; drying the precipitate at 110.degree.-170.degree.C; heating the dry cobalt molybdate to temperatures between 250.degree. and 550.degree.C; and sintering the cobalt molybdate shapes at temperatures between 500.degree. and 700.degree.C so as to obtain a cobalt molybdate catalyst having an inner surface area between 4 and 8 square meters/g and a volume of pores between 0.1 and 0.2 milliliters/g.

    摘要翻译： 通过在蒸汽存在下使丙烯醛与分子氧反应制备丙烯酸，如果需要，在升高的温度下，与钼酸钴催化剂接触的惰性气体接触，该催化剂是通过从钴盐的组合水溶液中沉淀钼酸钴制备的， 的钼化合物和氨在约60℃和pH至多为7的温度下进行; 在至少100℃的温度下过滤掉，洗涤和干燥沉淀物; 在高温下加热干燥的钼酸钴几个小时，研磨并将其转变成形状; 并将钼酸钴形状烧结数小时。 丙烯酸更特别地与通过以约1.05:1的Co:Mo原子比组合钴盐水溶液与钼化合物的水溶液而制备的催化剂接触; 在组合溶液中建立pH在3.8和6.0之间; 在110°-170℃干燥沉淀物; 将干燥的钼酸钴加热至250-550℃; 并在500〜700℃的温度下烧结钼酸钴形状，得到内表面积为4〜8平方米/ g，孔体积为0.1〜0.2毫升/克的钼酸钴催化剂。