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    • 1. 发明授权
    • Process for the preparation of acetic acid and acetic anhydride
    • 乙酸和乙酸酐的制备方法
    • US5380929A
    • 1995-01-10
    • US236669
    • 1994-05-02
    • Heinz ErpenbachKlaus GehrmannErhard JagersGeorg Kohl
    • Heinz ErpenbachKlaus GehrmannErhard JagersGeorg Kohl
    • B01J31/20C07B61/00C07C51/12C07C51/56C07C53/08C07C53/12
    • C07C51/12C07C51/56
    • To prepare acetic acid and acetic anhydride, methanol and methyl acetate are reacted under anhydrous conditions with carbon monoxide in the presence of a catalyst system containing carbonyl complexes of group VIII noble metals, methyl iodide, an alkali metal acetate or iodide, or quaternary organophosphonium or organoammonium acetate or iodide, The hot carbonylation mixture is decompressed, the evaporated components are fed to a first distillation zone, and the catalyst solution which remains is fed back to the reaction zone. In the first distillation zone, the volatile carbonylation products are subjected to fractional distillation; the low-boiling methyl iodide and methyl acetate pass back into the reaction zone, and the bottom product produced is a mixture of acetic acid and acetic anhydride, which is split into the pure components in a second distillation zone and a third distillation zone.
    • 为了制备乙酸和乙酸酐,在无水条件下,甲醇和乙酸甲酯在含有VIII族贵金属,甲基碘,碱金属乙酸酯或碘化物的羰基络合物或季有机鏻的催化剂体系存在下与一氧化碳反应,或 乙酸有机铵或碘化物。将热羰基化混合物减压,将蒸发的组分进料至第一蒸馏区,将剩余的催化剂溶液反馈回反应区。 在第一蒸馏区中,将挥发性羰基化产物进行分馏; 低沸点甲基碘和乙酸甲酯回到反应区,产生的底部产物是乙酸和乙酸酐的混合物,其在第二蒸馏区和第三蒸馏区被分成纯组分。
    • 4. 发明授权
    • Process for separating the catalyst system from the reaction mixtures of
carbonylation reactions
    • 将催化剂体系与羰基化反应的反应混合物分离的方法
    • US4549937A
    • 1985-10-29
    • US442107
    • 1982-11-16
    • Heinz ErpenbachKlaus GehrmannPeter HorstermannHans-Klaus KubbelerGeorg Kohl
    • Heinz ErpenbachKlaus GehrmannPeter HorstermannHans-Klaus KubbelerGeorg Kohl
    • C07C69/34B01J31/00C07C51/00C07C51/573C07C53/12C07C67/00C07C67/54C07C69/16B01D3/06C07C51/56
    • C07C51/573C07C67/54
    • The disclosure relates to a process for separating the catalyst system from reaction mixtures which are obtained by reacting methyl acetate and/or dimethylether with carbon monoxide and optionally hydrogen at elevated temperatures to acetic anhydride and optionally ethylidene diacetate in the presence of a catalyst system consisting of carbonyl complexes of noble metals belonging to group VIII of the Periodic System, acetic acid, an organophosphorus or organonitrogen compound, methyl iodide and optionally compounds of carbonyl-yielding common metals, and which issue from the reaction zone under a pressure of 25 to 150 bars at a temperature of 100.degree. to 250.degree. C. More particularly, the reaction mixture coming from the reaction zone is introduced into a separator heated to 60.degree. to 140.degree. C. and released to a pressure of 0.5 to 3.5 bars with spontaneous evaporation of the bulk of volatile constituents; the stream of liquid matter coming from the separator is delivered to a distilling zone and the bulk of still volatile constituents is distilled off therein under a pressure of 0.05 to 1 bar at a base temperature of 70.degree. to 170.degree. C.; and catalyst solution retained as base product is recycled to the reaction zone.
    • 本公开涉及一种从反应混合物中分离催化剂体系的方法,其通过使乙酸甲酯和/或二甲醚与一氧化碳和任选的氢气在高温下反应而获得,所述方法是在催化剂体系存在下在高温下在乙酸酐和任选的亚乙基二乙酸酯 属于周期系第VIII族的贵金属的羰基络合物,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的化合物,并且在25至150巴的压力下从反应区发出 更优选地,将来自反应区的反应混合物引入加热至60℃至140℃的隔膜中,并释放至0.5至3.5巴的压力,并自发蒸发 大部分挥发性成分; 来自分离器的液体物流被输送到蒸馏区,并且在基本温度为70至170℃的压力下,在0.05至1巴的压力下蒸馏出大部分挥发性挥发性成分。 将作为基础产物保留的催化剂溶液再循环至反应区。
    • 8. 发明授权
    • Process for removing metallic corrosion products from carbonylation
reactions carried out under anhydrous conditions
    • 从非强制性条件下运输的碳化反应中除去金属腐蚀产物的方法
    • US5124290A
    • 1992-06-23
    • US777066
    • 1991-10-16
    • Heinz ErpenbachReinhard GradlErhard JagersAndreas SeidelPeter Prinz
    • Heinz ErpenbachReinhard GradlErhard JagersAndreas SeidelPeter Prinz
    • B01J38/00C07B61/00C07C51/12C07C51/42C07C51/47C07C51/573C07C53/08C07C53/12
    • C07C51/573C07C51/47
    • A process for removing metallic corrosion products from carbonylation reactions which are carried out under anhydrous conditions and in which methyl acetate and/or methanol and/or dimethyl ether are reacted over a noble metal catalyst system which comprises a noble metal of group VIII of the periodic table of the elements, a co-catalyst, such as iodide or bromide, in particular methyl iodide, and a promoter, such as an organophosphonium or organoammonium salt, and if appropriate a lithium salt, to give acetic acid and/or acetic anhydride is described, the process comprisinga) bringing the reaction solution which is contaminated with metallic corrosion products and contains the catalyst system into contact with an ion exchanger;b) separating this reaction solution which has been brought into contact in this way from the ion exchanger;c) desorbing the promoter adsorbed on the ion exchanger before regeneration with acetic acid and/or acetic anhydride;d) combining the eluate obtained in step c) with the reaction solution separated off in step b) and recycling the components together into the carbonylation reaction;e) regenerating the ion exchanger obtained from step c) with a strong mineral acid; andf) washing the ion exchanger regenerated in this way with acetic acid and/or acetic anhydride until free from water, before use in step a).
    • 一种在无水条件下进行羰基化反应的金属腐蚀产物的方法,其中乙酸甲酯和/或甲醇和/或二甲醚在贵金属催化剂体系上反应,贵金属催化剂体系包含周期性的第VIII族贵金属 表中的元素,助催化剂如碘化物或溴化物,特别是甲基碘,以及促进剂如有机鏻盐或有机铵盐,以及如果合适的话,锂盐,得到乙酸和/或乙酸酐是 描述了该方法,该方法包括:a)将被金属腐蚀产物污染的反应溶液带入与离子交换器接触的催化剂体系; b)将已经以这种方式接触的反应溶液从离子交换器分离; c)在用乙酸和/或乙酸酐再生之前解吸吸附在离子交换剂上的促进剂; d)将步骤c)中获得的洗脱液与步骤b)中分离的反应溶液合并,并将组分一起再循环到羰基化反应中; e)用强无机酸再生步骤c)获得的离子交换剂; 以及f)在步骤a)中使用之前,用乙酸和/或乙酸酐洗涤离子交换剂,直至不含水再洗涤。