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    • 1. 发明授权
    • Process for purifying and recovering the contaminated catalyst solution
arising in the carbonylation of methanol and/or methyl acetate and/or
dimethyl ether
    • 用于纯化和回收在甲醇和/或乙酸甲酯和/或二甲醚的羰基化中产生的污染的催化剂溶液的方法
    • US5002914A
    • 1991-03-26
    • US491352
    • 1990-03-09
    • Heinz ErpenbachWinfried LorkNorbert WeferlingPeter Prinz
    • Heinz ErpenbachWinfried LorkNorbert WeferlingPeter Prinz
    • B01J38/00B01J31/40C07B61/00C07C27/00C07C51/12C07C51/42C07C51/48C07C51/56C07C51/573C07C53/08C07C53/12C07C67/36C07C67/37C07C67/48C07C69/16
    • C07C51/56C07C51/12C07C51/42C07C51/48C07C51/573C07C67/48Y02P20/584
    • A process for purifying and recovering the contaminated catalyst solution arising from the carbonylation of methanol, methyl acetate and/or dimethyl ether. The solution contains carbonyl complexes of rhodium, quaternary organophosphorus compounds as organic promoters, undistillable organic impurities, and acetic acid, acetic anhydride and ethylidene diacetate. The carbonyl complex of rhodium together with acetic acid, acetic anhydride and ethylidene diacetate are extracted from the contaminated catalyst solution by using a tri-C.sub.3 - to C.sub.8 -alkylphosphine. The trialkylphosphine phase is separated from the promoter phase and is separated into the volatile constituents acetic acid, acetic anhydride and ethylidene diacetate as well as trialkylphosphine. The rhodium carbonyl complex remaining as the residue and the recovered trialkylphosphine is used for further extraction. The contaminated promoter phase is freed of the organic impurities by extraction with dialkyl ethers, carboxylic acid esters or hydrocarbons and, after the extractant phase has been separated off, is recombined with the recovered acetic acid/acetic anhydride and ethylidene diacetate mixture and with the rhodium carbonyl complex and recycled to the carbonylation reactor. The impurities remaining as the residue from a distillation of the extractant phase which has been separated off are removed from the system.
    • 一种纯化和回收由甲醇,乙酸甲酯和/或二甲醚羰基化产生的污染的催化剂溶液的方法。 该溶液含有铑羰基络合物,季有机磷化合物作为有机促进剂,不可渗透的有机杂质,以及乙酸,乙酸酐和亚乙基二乙酸酯。 通过使用三-C 3 -C 8烷基膦,从污染的催化剂溶液中提取铑与乙酸,乙酸酐和亚乙基二乙酸酯的羰基络合物。 将三烷基膦相与助催化剂相分离,并分离成挥发性成分乙酸,乙酸酐和亚乙基二乙酸酯以及三烷基膦。 剩余的作为残留物的铑羰基络合物和回收的三烷基膦用于进一步萃取。 被污染的促进剂相通过用二烷基醚,羧酸酯或烃萃取除去有机杂质,并且在萃取相分离后,与回收的乙酸/乙酸酐和亚乙基二乙酸酯混合物与铑重组 羰基络合物并循环到羰基化反应器中。 从分离出的萃取相的蒸馏中残留的杂质作为残留物从体系中除去。
    • 2. 发明授权
    • Process for separating acetone from carbonylation mixtures
    • 从羰基化混合物中分离丙酮的方法
    • US4444624A
    • 1984-04-24
    • US412225
    • 1982-08-27
    • Heinz ErpenbachKlaus GehrmannWinfried LorkPeter Prinz
    • Heinz ErpenbachKlaus GehrmannWinfried LorkPeter Prinz
    • C07C45/00C07C45/49C07C45/78C07C45/82C07C45/83C07C49/08C07C67/00B01D3/40
    • C07C45/82C07C45/49C07C45/83
    • 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.
    • 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。
    • 6. 发明授权
    • Process for making carboxylic acid halides
    • 制备羧酸卤化物的方法
    • US4414160A
    • 1983-11-08
    • US301984
    • 1981-09-14
    • Heinz ErpenbachKlaus GehrmannWinfried LorkPeter Prinz
    • Heinz ErpenbachKlaus GehrmannWinfried LorkPeter Prinz
    • C07C53/38C07C51/58
    • C07C51/58
    • 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.
    • 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。