公开(公告)号：US5620567A

公开(公告)日：1997-04-15

申请号：US283280

申请日：1994-07-29

Applicant: Andreas Seidel ,  Alfred Hauser ,  Peter Prinz

Inventor： Andreas Seidel ,  Alfred Hauser ,  Peter Prinz

IPC: C07C51/44 ,  C07C51/487 ,  C07C53/08 ,  B01D3/34

CPC classification number: C07C51/44 ,  C07C51/487

Abstract: A process for the removal of aldehydes and acetals from industrially prepared acetic acid, wherein the contaminated acetic acid is reacted in the presence of a Bronstedt acid and 0.05 to 1% by weight of water and, if required, of 3 to 10 equivalents, calculated on aldehyde and acetal, of a high boiling polyhydric alcohol, and isolating the purified acetic acid by fractional distillation.

Abstract translation: 一种用于从工业上制备的乙酸中除去醛和缩醛的方法，其中被污染的乙酸在Br + E，umI + EE n t酸和0.05-1％（重量）水的存在下反应，如果需要 ，按醛和缩醛计算为3至10当量的高沸点多元醇，并通过分馏分离纯化的乙酸。

公开(公告)号：US4556644A

公开(公告)日：1985-12-03

申请号：US405070

申请日：1982-08-04

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: C07C67/37 ,  B01J31/40 ,  B01J38/00 ,  C07C27/00 ,  C07C51/00 ,  C07C51/12 ,  C07C51/48 ,  C07C51/573 ,  C07C53/08 ,  C07C53/12 ,  C07C67/00 ,  C07C69/16 ,  C07C51/54 ,  C07C51/56

CPC classification number: B01J31/0268 ,  B01J31/0239 ,  B01J31/20 ,  B01J31/4038 ,  B01J31/4046 ,  C07C51/48 ,  C07C51/573 ,  C07C67/36 ,  C07C67/37 ,  C07C67/54 ,  B01J2231/34 ,  B01J2531/82 ,  B01J2531/822 ,  B01J2531/824 ,  Y02P20/584

Abstract: 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, and optionally compounds of carbonyl-yielding common metals as inorganic 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 freed from the organic contaminants by extraction with aliphatic ethers; and for the remaining undissolved mixture of noble metal/carbonyl-complex, organic and optionally inorganic promoters to be filtered off and recycled into the carbonylation reaction.

Abstract translation: 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，以及任选的产生羰基的常见金属作为无机助催化剂，不可挥发的有机污染物以及乙酸，乙酸酐和亚乙基二乙酸酯的化合物。 为此，本公开内容提供了催化剂溶液从其挥发性成分中蒸馏除去，并且剩余的固体蒸馏残余物通过用脂族醚萃取除去有机污染物; 并且对于剩余的未溶解的贵金属/羰基络合物的混合物，有机和任选的无机助催化剂被滤出并再循环到羰基化反应中。

公开(公告)号：US4440570A

公开(公告)日：1984-04-03

申请号：US402961

申请日：1982-07-29

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: 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 ,  C22B11/00 ,  C01G55/00 ,  C07D213/06 ,  C07F9/54

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

Abstract: 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 for the noble metal to be recovered terefrom in known fashion; for the organic promoter to be recovered by evaporating the water or extracting it with halogenated hydrocarbons and for these latter to be evaporated.

Abstract translation: 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 通过过滤除去沉淀和污染的贵金属/羰基络合物，以及以已知方式回收的贵金属; 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而回收。

公开(公告)号：US4664753A

公开(公告)日：1987-05-12

申请号：US637860

申请日：1984-08-06

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: C07C69/16 ,  C07C51/00 ,  C07C51/44 ,  C07C51/487 ,  C07C53/08 ,  C07C53/12 ,  C07C67/00 ,  C07C67/54 ,  C07C51/573

CPC classification number: C07C51/487 ,  C07C51/44 ,  C07C67/60

Abstract: The disclosure relates to a process for separating iodine and its compounds from the carbonlyation products acetic acid, acetic anhydride or ethylidene diacetate obtained by subjecting dimethylether, methyl acetate or methanol to a carbonylation reaction. For reducing the quantity of total iodine contaminating the carbonlyation products to less than 20 ppb iodine, the disclosure provides for the carbonylation products to be treated at temperatures of 20.degree. to 250.degree. C. with an alkyl or aryl phosphine or a heterocyclic aromatic nitrogen compound and at least one of the metals copper, silver, zinc or cadmium or their compounds and to be distillatively separated from the iodine thereby fixed in non-volatile form.

Abstract translation: 本公开内容涉及通过使二甲醚，乙酸甲酯或甲醇进行羰基化反应而获得的将其及其化合物与碳酸化产物乙酸，乙酸酐或亚乙基二乙酸酯分离的方法。 为了将污染碳酸化产物的总碘的量减少到低于20ppb的碘，本公开提供了在20℃至250℃的温度下用烷基或芳基膦或杂环芳族氮化合物处理的羰基化产物 和至少一种金属铜，银，锌或镉或其化合物，并与碘蒸馏分离，从而固定成非挥发性形式。

公开(公告)号：US4543217A

公开(公告)日：1985-09-24

申请号：US561805

申请日：1983-12-15

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

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

CPC classification number: C07C51/58

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US5243819A

公开(公告)日：1993-09-14

申请号：US850392

申请日：1992-03-11

Applicant: Siegfried Woerner ,  Peter Reiser ,  Peter Prinz

Inventor： Siegfried Woerner ,  Peter Reiser ,  Peter Prinz

IPC: F01N3/025 ,  F01N3/031 ,  F02B3/06

CPC classification number: F01N3/031 ,  F01N3/025 ,  F01N2330/06 ,  F02B3/06 ,  Y10S55/30

Abstract: An exhaust gas cleaning device for diesel engines has an exhaust gas soot filter (2) with a filter body (6) that is supported in a housing (4) and is regenerated by combustion of the soot when its temperature rises above the middle operating exhaust gas temperature range. A burner (26) is provided, having a combustion air fan (28) whose hot gas side is in flow communication with the exhaust gas soot filter (2), and the filter body (6) is supported in its housing in such a manner that at least a large part of its outer surface is heated externally during operation of the burner (26).

Abstract translation: 一种用于柴油发动机的废气净化装置具有排气烟尘过滤器（2），其具有被支撑在壳体（4）中的过滤器体（6），并且当烟囱的温度升高到中间运行排气口 气体温度范围。 设有燃烧器（26），其具有燃烧空气风扇（28），其燃烧气体侧与废气烟灰过滤器（2）流动连通，并且过滤体（6）以这种方式支撑在其壳体 至少其外表面的大部分在燃烧器（26）的操作期间被外部加热。

公开(公告)号：US4985383A

公开(公告)日：1991-01-15

申请号：US470945

申请日：1990-01-26

Applicant: Heinz Erpenbach ,  Winfried Lork ,  Andreas Seidel ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Winfried Lork ,  Andreas Seidel ,  Peter Prinz

IPC: B01J38/00 ,  B01J31/40 ,  C07B61/00 ,  C07C27/00 ,  C07C51/12 ,  C07C51/373 ,  C07C51/42 ,  C07C51/56 ,  C07C51/573 ,  C07C53/08 ,  C07C53/12 ,  C07C67/36 ,  C07C67/37 ,  C07C69/16

CPC classification number: B01J31/0268 ,  B01J31/20 ,  B01J31/4038 ,  B01J31/4046 ,  C07C51/373 ,  C07C51/42 ,  B01J2231/34 ,  B01J2531/82 ,  B01J2531/822 ,  Y02P20/584

Abstract: In a process for removing the metallic corrosion products from a contaminated catalyst solution produced on carbonylation of methanol and/or methyl acetate and/or dimethyl ether and containing carbonyl complexes of noble metals from group VIII of the Periodic Table of the elements, quaternary organo-phosphorus compounds as organic promoters, metallic corrosion products and acetic acid, acetic anhydride, ethylidene diacetate and, in some cases, undistillable organic compounds, the catalyst solution is treated with water, the noble metal carbonyl complex and the undistillable organic compounds, if present, being precipitated, while the organic promoter and the metallic corrosion products remain in solution; the aqueous phase is separated from the precipitated noble metal carbonyl complex and the organic promoter is extracted from the aqueous phase using C.sub.4 -C.sub.8 -alkanols, the promoter is recovered by evaporating the extractant, the promoter is recombined with the precipitated nobel metal carbonyl complex and with the undistillable organic compounds, if present, and the purified catalyst solution is recycled into the process after addition of acetic acid and/or acetic anhydride; finally, the aqueous phase with the metallic corrosion products is purged.

Abstract translation: 在从甲醇和/或乙酸甲酯和/或二甲醚羰基化产生的污染的催化剂溶液中除去金属腐蚀产物并含有元素周期表第VIII族贵金属的羰基络合物的方法中， 磷化合物作为有机促进剂，金属腐蚀产物和乙酸，乙酸酐，亚乙基二乙酸酯，在一些情况下是不挥发的有机化合物，催化剂溶液用水，贵金属羰基络合物和不可否认的有机化合物（如果存在） 同时有机促进剂和金属腐蚀产物残留在溶液中; 将水相与沉淀的贵金属羰基络合物分离，并使用C 4 -C 8 - 链烷醇从水相中萃取有机促进剂，通过蒸发萃取剂回收促进剂，将促进剂与沉淀的诺贝尔金属羰基络合物和 如果存在的话，有无化学有机化合物，并且在加入乙酸和/或乙酸酐之后将纯化的催化剂溶液再循环到该方法中; 最后，清洗含金属腐蚀产物的水相。

公开(公告)号：US4629711A

公开(公告)日：1986-12-16

申请号：US852222

申请日：1986-04-15

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: 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 classification number: B01J31/0268 ,  B01J31/0239 ,  B01J31/20 ,  B01J31/4046 ,  B01J38/52 ,  C07C51/48 ,  C07C51/573 ,  B01J2231/34 ,  B01J2531/822 ,  Y02P20/584

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US4442304A

公开(公告)日：1984-04-10

申请号：US402942

申请日：1982-07-29

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: 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 classification number: 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

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US3985800A

公开(公告)日：1976-10-12

申请号：US393347

申请日：1973-08-31

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

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

CPC classification number: B01J37/0018 ,  B01J23/882 ,  B01J35/10 ,  B01J37/0009 ,  C07C51/252 ,  B01J35/1009 ,  B01J35/1038

Abstract: 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.

Abstract translation: 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。