Process for separating water from mixtures thereof with vinyl acetate
and acetic acid
    1.
    发明授权
    Process for separating water from mixtures thereof with vinyl acetate and acetic acid 失效
    从乙酸乙烯酯和乙酸与其混合物中分离水的方法

    公开(公告)号:US4353783A

    公开(公告)日:1982-10-12

    申请号:US201752

    申请日:1980-10-29

    摘要: Process for separating water from a gas mixture, obtained in the manufacture of vinyl acetate by reacting ethylene with acetic acid and oxygen in contact with catalysts containing palladium or palladium compounds in the gaseous phase said gas mixture consisting essentially of acetic acid, vinyl acetate, water, carbon dioxide and ethylene, wherein(a) the gas mixture leaving the reaction zone is condensed to give a condensate containing the major portion of acetic acid, vinyl acetate and water and(b) an acetic acid solution containing the residual amount of vinyl acetate and water being prepared by absorption of the non-condensed gas in acetic acid, is characterized in that(c) the condensate obtained in step (a) and the solution obtained in step (b) are introduced separately from each other into the same distillation column, the feeding point of the condensate being above the feeding point of the solution, the water is distilled off at the head of said column as azeotrope together with the vinyl acetate and(d) the water phase is removed from the distillate separating into a water phase and a vinyl acetate phase.

    摘要翻译: 从气相混合物中分离水的方法,所述气体混合物是通过使乙烯与乙酸和氧气在气相中与含有钯或钯化合物的催化剂接触而在乙酸乙烯酯的制备中获得的,所述气体混合物主要由乙酸,乙酸乙烯酯,水 ,二氧化碳和乙烯,其中(a)离开反应区的气体混合物被冷凝,得到含有主要部分的乙酸,乙酸乙烯酯和水的冷凝物和(b)含有残留量的乙酸乙烯酯的乙酸溶液 和通过在乙酸中吸收非冷凝气体制备的水,其特征在于(c)将步骤(a)中获得的冷凝物和步骤(b)中获得的溶液彼此分开引入相同的蒸馏 柱,冷凝水的进料点高于溶液的进料点,水在所述塔的头部被蒸馏出来,作为共沸物一起 h乙酸乙烯酯和(d)从分离成水相和乙酸乙烯酯相的馏出物中除去水相。

    Process for the isolation of vinyl acetate
    4.
    发明授权
    Process for the isolation of vinyl acetate 失效
    乙酸乙烯酯分离方法

    公开(公告)号:US4818347A

    公开(公告)日:1989-04-04

    申请号:US133248

    申请日:1987-12-10

    摘要: The invention relates to a process for the isolation of vinyl acetate from a gas mixture containing vinyl acetate, ethyl acetate, water and carbon dioxide formed in the reaction of ethylene with acetic acid and oxygen in the gas phase over catalysts containing palladium or palladium compounds. The gas mixture leaving the reaction zone is passed into a distillation column and the gas mixture leaving the top thereof is cooled. The gas which is not condensed during the cooling is washed with acetic acid in a washing column, an acetic acid solution containing vinyl acetate being obtained. The bottom product from the distillation column is passed to a second distillation column and a side stream containing ethyl acetate is removed from an enrichment zone above the bottom thereof, all or some of the bottom product from the second distillation column, which product chiefly consists of acetic acid, being used for the wash in the washing column. The top vapor of the second distillation column is cooled. A portion of the organic phase of the condensate thereby formed is passed, together with the acetic acid solution obtained as the bottom product in the washing column, into a third distillation column, which may have an intermediate tray. The bottom product of the third distillation column is passed into a fourth distillation column. Pure vinyl acetate is removed at the top of the fourth distillation column.

    摘要翻译: 本发明涉及一种从包含乙酸乙烯酯,乙酸乙酯,水和二氧化碳的气体混合物中分离乙酸乙烯酯的方法,该方法是在乙烯与乙酸和气相中的氧反应生成的催化剂中形成的钯和钯化合物。 将离开反应区的气体混合物送入蒸馏塔,并将离开其顶部的气体混合物冷却。 冷却期间未冷凝的气体在洗涤塔中用乙酸洗涤,得到含有乙酸乙烯酯的乙酸溶液。 将来自蒸馏塔的底部产物通入第二蒸馏塔,并且从其底部的富集区除去含有乙酸乙酯的侧流,其中所有或一些来自第二蒸馏塔的底部产物主要由 乙酸,用于洗涤柱中的洗涤。 第二蒸馏塔的顶部蒸气被冷却。 将由此形成的冷凝物的有机相的一部分与在洗涤塔中作为底部产物获得的乙酸溶液一起进入可以具有中间塔盘的第三蒸馏塔。 将第三蒸馏塔的底部产物送入第四蒸馏塔。 在第四蒸馏塔的顶部除去纯乙酸乙烯酯。

    Process for the preparation of vinyl acetate
    5.
    发明授权
    Process for the preparation of vinyl acetate 失效
    乙酸乙烯酯的制备方法

    公开(公告)号:US4902823A

    公开(公告)日:1990-02-20

    申请号:US307733

    申请日:1989-02-07

    摘要: The invention relates to a process for the preparation of vinyl acetate in the gas phase from ethylene, acetic acid and oxygen or oxygen-containing gases on a catalyst which contains palladium and/or compounds thereof and if appropriate additionally gold and/or gold compounds and, as activators, alkali metal compounds and if appropriate additionally cadmium compounds, on a support. The support consists of cylindrical particles with curved front faces. The support material is aerogenic SiO.sub.2 or an aerogenic SiO.sub.2 -Al.sub.2 O.sub.3 mixture having a surface area of 50-250 m.sup.2 /g and a pore volume of 0.4-1.2 ml/g, which is formed to the extent of at least 50% by pores having a diameter of 50-200 .ANG..

    摘要翻译: 本发明涉及一种在含有钯和/或其化合物的催化剂上由乙烯,乙酸和氧气或含氧气体在气相中制备乙酸乙烯酯的方法,如果合适的话,本发明涉及金和/或金化合物和 ,作为活化剂,碱金属化合物和如果合适的话另外是镉化合物。 支撑体由具有弯曲前表面的圆柱形颗粒组成。 载体材料是表面积为50-250m2 / g,孔体积为0.4-1.2ml / g的生成SiO 2或发射SiO 2 -Al 2 O 3混合物,其通过具有至少50% 直径为50-200 ANGSTROM。

    Method of separating vinylphosphonic acid from crude mixtures
    6.
    发明授权
    Method of separating vinylphosphonic acid from crude mixtures 失效
    从粗混合物中分离乙烯基膦酸的方法

    公开(公告)号:US5391815A

    公开(公告)日:1995-02-21

    申请号:US978702

    申请日:1993-02-03

    申请人: Gunter Roscher

    发明人: Gunter Roscher

    IPC分类号: C07F9/02 C07F9/38

    CPC分类号: C07F9/3826 C07F9/025

    摘要: Method of separating vinylphosphonic acid from crude mixtures.The invention relates to a method for separating vinylphosphonic acid from crude mixtures, the separation being carried out by extraction with alcohols and/or ketones, which in each case comprise at least 5 carbon atoms.According to the invention, vinylphosphonic acid can be obtained in high purity and good yield from highly contaminated crude mixtures.

    摘要翻译: PCT No.PCT / EP91 / 01412 Sec。 371日期:1993年2月3日 102(e)日期1993年2月3日PCT PCT 1991年7月27日PCT公布。 出版物WO92 / 02524 日本1992年2月20日。从粗混合物中分离乙烯基膦酸的方法。 本发明涉及一种从粗混合物中分离乙烯基膦酸的方法,该分离是通过用醇和/或酮进行萃取,每种情况都包含至少5个碳原子。 根据本发明,可以从高度污染的粗混合物中获得高纯度和高收率的乙烯基膦酸。

    Process for the oxidation of dialkyl esters of 2-hydroxy-ethylphosphonic
acid
    8.
    发明授权
    Process for the oxidation of dialkyl esters of 2-hydroxy-ethylphosphonic acid 失效
    2-羟基乙酸磷酸二烷基酯氧化方法

    公开(公告)号:US5210259A

    公开(公告)日:1993-05-11

    申请号:US859416

    申请日:1992-05-22

    CPC分类号: C07F9/657181 C07F9/4006

    摘要: A process for the preparation of diesters of carboxymethylphosphonic acid of the formula: (RO).sub.2 P(O)CH.sub.2 CO.sub.2 H, in which R is a straight-chain or branched alkyl radical having 1 to 20 carbon atoms, a cycloaliphatic radical having 5 to 8 carbon atoms, a phenyl or naphthyl radical which can be substituted, an aralkyl radical having 7 to 10 carbon atoms, or in which the (RO).sub.2 P group forms a ring having 2 to 5 carbon atoms which can be substituted, characterized in that dialkyl ester of 2-hydroxyethylphosphonic acid of the formula (RO).sub.2 P(O)CH.sub.2 CH.sub.2 OH, in which R has the abovementioned meaning, is reacted with oxygen in the presence of water and a catalyst which contains at least one metal selected from the platinum metals group.

    摘要翻译: PCT No.PCT / EP90 / 01980 Sec。 371日期:1992年5月22日 102(e)日期1992年5月22日PCT 1990年11月20日PCT PCT。 第WO91 / 08210号公报 日期:1991年6月13日。一种制备下式的羧甲基膦酸二酯的方法:(RO)2P(O)CH 2 CO 2 H,其中R是具有1至20个碳原子的直链或支链烷基, 具有5至8个碳原子的脂环族基团,可被取代的苯基或萘基,具有7至10个碳原子的芳烷基,或其中(RO)2P基团形成具有2至5个碳原子的环,其可以是 其特征在于,式(RO)2 P(O)CH 2 CH 2 OH的2-羟乙基膦酸的二烷基酯(其中R具有上述含义)在水和催化剂的存在下与氧反应,所述催化剂含有至少一种金属 选自铂金属组。

    Process for the manufacture of N,N'-diacetylethylene diamine
    9.
    发明授权
    Process for the manufacture of N,N'-diacetylethylene diamine 失效
    制备N,N'-二乙酰乙二胺的方法

    公开(公告)号:US4219500A

    公开(公告)日:1980-08-26

    申请号:US53033

    申请日:1979-06-28

    CPC分类号: C07C231/02

    摘要: N,N'-Diacetylethylene diamine (DAED) is produced by first adding the stoichiometric amount of acetic acid (2 mols per mol of ethylene diamine) at least partially in the form of aqueous acetic acid to ethylene diamine, distilling off in a second step the water contained in the reaction mixture, adding acetic acid in excess to the remaining product, distilling off the aqueous acetic acid formed and recycling it into the first process step. The DAED remains as sump product after distillation of the acetic acid.

    摘要翻译: 通过首先将至少部分为乙酸水溶液的化学计量的乙酸(2摩尔/摩尔乙二胺)加入到乙二胺中,在第二步骤中蒸馏出来制备N,N'-二乙酰基乙二胺(DAED) 包含在反应混合物中的水,向剩余的产物中过量加入乙酸,蒸馏形成的乙酸水溶液并将其再循环到第一工艺步骤中。 在乙酸蒸馏后,DAED仍然作为贮槽产品。

    Process for preparing vinyl-phosphonic acids
    10.
    发明授权
    Process for preparing vinyl-phosphonic acids 失效
    制备乙烯基膦酸的方法

    公开(公告)号:US5811575A

    公开(公告)日:1998-09-22

    申请号:US857318

    申请日:1997-05-16

    CPC分类号: C07F9/3895 C07F9/3826

    摘要: The present invention relates to a process for preparing vinylphosphonic acids of the formula ##STR1## in which m is an integer from 1 to 20 by heating 2-chloroethylphosphonic acids of the formula ##STR2## in which n is an integer equal to or smaller than m, if desired in the form of a solution, in the absence or presence of a catalyst to a temperature of 180 to 350.degree. C. and eliminating hydrogen chloride and, where appropriate, water under atmospheric pressure or reduced pressure and, if desired, hydrolysing the vinylphosphonic acids of the formula (I).

    摘要翻译: 本发明涉及一种制备式(I)的乙烯基膦酸的方法,其中m为1至20的整数,通过加热式(II)的2-氯乙基膦酸,其中n为 等于或小于m的整数,如果需要,在溶液形式下,在不存在或不存在催化剂的情况下,温度为180-350℃,并且在适当的情况下除去氯化氢,并在适当情况下,在大气压下还原 压力,如果需要,水解式(I)的乙烯基膦酸。