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11. 发明授权

US4442304A Process for purifying and recovering contaminated catalyst solution obtained in the carbonylation of methyl acetate and/or dimethylether 失效
标题翻译：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。

12. 发明授权

US3985800A Process for the manufacture of acrylic acid 失效
标题翻译：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。

13. 发明授权

US4746640A Process for purifying and recovering catalyst solution contaminated during the carbonylation of methyl acetate and/or dimethylether 失效
标题翻译：纯化和回收在乙酸甲酯和/或二甲醚羰基化过程中污染的催化剂溶液的方法
公开(公告)号：US4746640A
公开(公告)日：1988-05-24
申请号：US25962
申请日：1987-03-16
申请人： Heinz Erpenbach , Klaus Gehrmann , Winfried Lork
发明人： Heinz Erpenbach , Klaus Gehrmann , Winfried Lork
IPC分类号： B01J38/00 , B01J31/40 , C07B61/00 , C07C51/00 , C07C51/12 , C07C53/12 , C07C67/00 , C07C67/37 , C07C69/14 , B01J38/68 , C07C51/56 , C07C67/36
CPC分类号： B01J31/0268 , B01J31/0239 , B01J31/20 , B01J31/4046 , C07C51/42 , C07C51/48 , C07C51/573 , C07C67/48 , B01J2231/34 , B01J2531/822 , Y02P20/584
摘要： Catalyst solution contaminated during the carbonylation of methyl acetate and/or dimethylether. To this end, the contaminated catalyst solution is subjected in a first processing stage to extraction with a dialkylether and alkanol, each of which has from 1-4 carbon atoms per alkyl group, and thereby freed from its organic contaminants, from acetic acid, acetic anhydride and ethylidene diacetate, and the ether phase is separated from the purified promoter-containing catalyst solution; next, the ether phase is treated in a second processing stage with iodine and/or methyl iodide; the precipitated promoter containing catalyst complex is separated and dissolved in the purified catalyst solution coming from the first processing stage; the ether phase is separated into its constituents by distilling it; recovered dialkylether and alkanol are used again in the extraction stage; fresh catalyst solution is prepared from the recovered mixture of acetic acid, acetic anhydride and ethylidene diacetate and from the united purified catalyst solution while residual dialkylether and alkanol are distilled off, and the organic contaminants retained in the residue of the ether phase distillation are expelled.
摘要翻译：催化剂溶液在乙酸甲酯和/或二甲醚的羰基化过程中被污染。为此，将污染的催化剂溶液在第一个处理阶段进行，用二烷基醚和链烷醇进行萃取，每个烷基烷基和烷醇每个烷基具有1-4个碳原子，从而从乙酸，乙酸中除去其有机污染物酸酐和亚乙基二乙酸酯，并从纯化的含有助催化剂的催化剂溶液中分离出醚相; 接下来，乙醚相在碘和/或碘甲烷的第二个处理阶段进行处理; 将含有沉淀促进剂的催化剂配合物分离并溶解在来自第一处理阶段的纯化催化剂溶液中; 通过蒸馏将乙醚相分离成其成分; 在提取阶段再次使用回收的二烷基醚和链烷醇; 从回收的乙酸，乙酸酐和亚乙基二乙酸酯的混合物中制备新鲜的催化剂溶液，并从合并的纯化的催化剂溶液中蒸出残余的二烷基醚和链烷醇，并且保留在醚相蒸馏残余物中的有机污染物被排出。

14. 发明授权

US5047377A Process for the purification and recovery of the contaminated solution of the catalyst produced on carbonylation of methanol and/or methyl acetate and/or dimethyl ether 失效
标题翻译：纯化和回收在甲醇和/或乙酸甲酯和/或二甲醚的羰基化产生的催化剂的污染溶液的方法
公开(公告)号：US5047377A
公开(公告)日：1991-09-10
申请号：US563396
申请日：1990-08-06
申请人： Heinz Erpenbach , Eitel Goedicke , Winfried Lork , Heribert Tetzlaff
发明人： Heinz Erpenbach , Eitel Goedicke , Winfried Lork , Heribert Tetzlaff
IPC分类号： B01J38/00 , B01J31/40 , B01J38/04 , C07B61/00 , C07C27/00 , C07C27/26 , C07C51/12 , C07C51/42 , C07C51/54 , C07C51/56 , C07C51/573 , C07C53/08 , C07C53/12 , C07C67/37 , C07C69/16
CPC分类号： B01J31/4069 , B01J31/0239 , B01J31/0268 , B01J31/20 , B01J31/26 , B01J31/4046 , B01J38/04 , C07C51/42 , C07C51/573 , C07C67/48 , B01J2038/005 , B01J2231/34 , B01J2531/822 , Y02P20/544 , Y02P20/584
摘要： In a process for the purification and recovery of a contaminated catalyst solution produced during carbonylation of methanol and/or methyl acetate and/or dimethyl ether and containing carbonyl complexes of rhodium, organic and/or inorganic promoters, undistillable organic impurities and acetic acid, acetic anhydride and ethylidene diacetate, the organic impurities and acetic acid, acetic anhydride and ethylidene diacetate are removed from the contaminatd catalyst solution by extraction at pressures from 35 to 450 bar and temperatures from 0.degree. to 120.degree. C. with a liquefied or supercritical gas, and the phase of the liquefied or supercritical gas is separated from the purified, promoter-containing catalyst solution, the phase of the liquefied or supercritical gas is separated by flash vaporization, the recovered gas is re-employed for extraction, acetic acid, acetic anhydride and ethylidene diacetate are separated off from the component which remains liquid, and are combined with the purified catalyst complex to prepare fresh catalyst solution and, finally, the organic impurities remaining as the residue on separation of the phase of the liquefied or supercritical gas is purged.
摘要翻译：在用于纯化和回收在甲醇和/或乙酸甲酯和/或二甲醚的羰基化过程中产生的污染的催化剂溶液的方法中，并且含有铑，有机和/或无机促进剂，不可挥发的有机杂质和乙酸的羰基络合物，乙酸酸酐和亚乙基二乙酸酯，通过用液化或超临界气体在35至450巴的压力和0至120℃的温度下萃取，从污染的催化剂溶液中除去有机杂质和乙酸，乙酸酐和亚乙基二乙酸酯，液化或超临界气体的相与纯化的助催化剂催化剂溶液分离，液化或超临界气体的相通过闪蒸分离，回收的气体再次用于萃取，乙酸，乙酸酐和亚乙基二乙酸酯从保持液体的组分中分离出来，并与纯化催化剂配合物，制备新鲜的催化剂溶液，最后，清除液化或超临界气体相分离残余物中剩余的有机杂质。

15. 发明授权

US4252983A Production of acetic anhydride and acetic acid from acetaldehyde 失效
标题翻译：从乙醛生产乙酸酐和乙酸
公开(公告)号：US4252983A
公开(公告)日：1981-02-24
申请号：US969102
申请日：1978-12-13
申请人： Heinz Erpenbach , Klaus Gehrmann , Alfred Hauser , Kurt Karrenbauer , Winfried Lork
发明人： Heinz Erpenbach , Klaus Gehrmann , Alfred Hauser , Kurt Karrenbauer , Winfried Lork
IPC分类号： B01J31/00 , C07B61/00 , C07C51/00 , C07C51/235 , C07C53/08 , C07C53/12 , C07C67/00
CPC分类号： C07C51/235
摘要： Acetic acid and acetic anhydride are produced continuously from acetaldehyde which is reacted by oxidizing it with gaseous oxygen in liquid phase in the presence of copper acylate and cobalt acylate as a catalyst and in the presence of an aliphatic carboxylic acid ester as a diluent. More specifically, the reaction is effected at temperatures of 62.degree. to 90.degree. C. over a period of less than 20 minutes with the use of the diluent and acetaldehyde in a quantitative ratio of 60:40 to 40:60; the resulting reaction products are delivered to a distilling zone in which the carboxylic acid ester and water are distilled off overhead and separated into two phases. Next, the organic phase is recycled with a reflux ratio of at least 1:1 to the distilling zone; base product accumulating in the distilling zone is delivered to an evaporating zone in which 2 to 12 parts by weight of an acetic acid/acetic anhydride-mixture as distillate are produced per part by weight of catalyst solution as base product.
摘要翻译：乙酸和乙酸酐是从乙醛连续生产的，该乙醛通过在酰化铜和催化剂钴作为催化剂存在下，在脂肪族羧酸酯作为稀释剂的存在下，以液相的气态氧氧化反应生成乙醛。更具体地，使用稀释剂和乙醛以60:40至40:60的定量比例，在低于20分钟的时间内，在62℃至90℃的温度下进行反应; 将所得反应产物输送到蒸馏区，其中将羧酸酯和水从塔顶馏出并分离成两相。接下来，有机相以至少1:1的回流比再循环到蒸馏区; 在蒸馏区积存的基础产物被输送到蒸发区，其中每重量份作为基础产物的催化剂溶液产生2至12重量份的作为馏出物的乙酸/乙酸酐混合物。

16. 发明授权

US4352761A Production of acetyl chloride 失效
标题翻译：生产乙酰氯
公开(公告)号：US4352761A
公开(公告)日：1982-10-05
申请号：US256387
申请日：1981-04-22
申请人： Heinz Erpenbach , Klaus Gehrmann , Winfried Lork , Peter Pring
发明人： Heinz Erpenbach , Klaus Gehrmann , Winfried Lork , Peter Pring
IPC分类号： C07C53/40 , B01J23/00 , B01J27/00 , B01J27/132 , B01J27/16 , B01J31/02 , B01J31/18 , C07B61/00 , C07C51/00 , C07C51/58 , C07C67/00
CPC分类号： B01J31/1875 , C07C51/58 , B01J2531/822 , B01J2531/824 , B01J2531/827 , Y02P20/582
摘要： The invention relates to a process for making acetyl chloride by reacting methoxy chloride with carbon monoxide under practically anhydrous conditions, at temperatures of 350.degree. to 575.degree. K, under pressures of 1 to 300 bars, and 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 and optionally trialkylphosphine oxide or triarylphosphine oxide, as well as an inert organic solvent. The invention provides more specifically for the reaction to be effected in the presence of a catalyst system containing n-heptane as the inert solvent and as additional ingredients methyltrialkyl phosphonium iodide and/or methyltriarylphosphonium iodide and at least one compound of chromium, molybdenum or tungsten.
摘要翻译：本发明涉及一种在几乎无水条件下，甲氧基氯与一氧化碳在350〜575℃的温度，1〜300巴的压力下反应制备乙酰氯的方法，在含有选自铑，钯，铱或其化合物中的至少一种贵金属，碘和/或其化合物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。本发明更具体地涉及在含有正庚烷作为惰性溶剂的催化剂体系和作为其它成分的碘化甲基三烷基鏻和/或甲基三芳基碘化鏻和至少一种铬，钼或钨化合物的存在下进行的反应。

17. 发明授权

US4280010A Continuous production of alkyl acrylates free from ether 失效
标题翻译：连续生产不含醚的丙烯酸烷基酯
公开(公告)号：US4280010A
公开(公告)日：1981-07-21
申请号：US66511
申请日：1979-08-14
申请人： Heinz Erpenbach , Klaus Gehrmann , Hans-Klaus Kubbeler , Winfried Lork
发明人： Heinz Erpenbach , Klaus Gehrmann , Hans-Klaus Kubbeler , Winfried Lork
IPC分类号： C07C69/54 , C07C67/08
CPC分类号： C07C67/08 , C07C67/54 , Y02P20/584
摘要： Alkyl acrylates free from ether are made continuously by reacting acrylic acid with a C.sub.1 -C.sub.4 -alkanol, in a molar ratio of 1:1 to 1:2, in liquid phase, at 80.degree. to 130.degree. C., under 100 to 760 mm Hg, in the presence of an acid catalyst.
摘要翻译：不含醚的丙烯酸烷基酯通过丙烯酸与C1-C4链烷醇以摩尔比1：1至1：2在液相中，在80至130℃，100至760 mm Hg，在酸催化剂存在下。

18. 发明授权

US5166452A Process for inhibiting and destroying peroxides in dialkyl ethers 失效
标题翻译：在二氯乙烷中抑制和破坏过氧化物的方法
公开(公告)号：US5166452A
公开(公告)日：1992-11-24
申请号：US756341
申请日：1991-09-06
申请人： Reinhard Gradl , Heinz Erpenbach , Norbert Weferling , Erhard Jagers
发明人： Reinhard Gradl , Heinz Erpenbach , Norbert Weferling , Erhard Jagers
IPC分类号： C07C41/44 , C07C41/46 , C07C43/04
CPC分类号： C07C41/46
摘要： A process for inhibiting and destroying peroxides in dialkyl ethers having the general formula R.sub.1 OR.sub.2 in which R.sub.1 and R.sub.2 are alkyl groups having 1 to 6 carbon atoms, which comprises adding, as inhibitor, a quaternary alkyl iodide of the general formula[CH.sub.3 alk.sub.3 P]Ito the dialkyl ethers.
摘要翻译：一种用于抑制和破坏具有通式R1OR2的二烷基醚中的过氧化物的方法，其中R 1和R 2是具有1至6个碳原子的烷基，其包括将作为抑制剂的通式[CH 3 Cl 3 P] I的季烷基碘加入到二烷基醚。

19. 发明授权

US5124290A Process for removing metallic corrosion products from carbonylation reactions carried out under anhydrous conditions 失效
标题翻译：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
公开(公告)号：US5124290A
公开(公告)日：1992-06-23
申请号：US777066
申请日：1991-10-16
申请人： Heinz Erpenbach , Reinhard Gradl , Erhard Jagers , Andreas Seidel , Peter Prinz
发明人： Heinz Erpenbach , Reinhard Gradl , Erhard Jagers , Andreas Seidel , Peter Prinz
IPC分类号： B01J38/00 , C07B61/00 , C07C51/12 , C07C51/42 , C07C51/47 , C07C51/573 , C07C53/08 , C07C53/12
CPC分类号： C07C51/573 , C07C51/47
摘要： 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).
摘要翻译：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。

20. 发明授权

US4892971A Process for the preparation of n-acetylphenylalanine 失效
标题翻译：制备正乙酰苯丙氨酸的方法
公开(公告)号：US4892971A
公开(公告)日：1990-01-09
申请号：US257715
申请日：1988-10-14
申请人： Heinz Erpenbach , Klaus Gehrmann , Peter Horstermann
发明人： Heinz Erpenbach , Klaus Gehrmann , Peter Horstermann
IPC分类号： C07C231/00 , B01J23/44 , C07B61/00 , C07C67/00 , C07C231/12 , C07C231/14 , C07C233/47 , C07C237/00
CPC分类号： C07C237/00
摘要： In the process for the preparation of N-acetylphenylalanine by opening the ring of 2-methyl-4-benzylidene-1,3-oxazolin-5-one with water to give 2-acetaminocinnamic acid and subsequently catalytically hydrogenating the latter, both reaction stages are carried out in a mixture of an aliphatic C.sub.3 -ketone to C.sub.10 -ketone or a water-miscible ether and water as the solvent, and the hydrogenation of the 2-acetaminocinnamic acid is carried out at temperatures of 10.degree. to 50.degree. C. and pressures of 1 to 15 bar in the presence of a supported palladium catalyst.
摘要翻译：在通过用水打开2-甲基-4-亚苄基-1,3-恶唑啉-5-酮的环以制备N-乙酰基苯丙氨酸的方法中，得到2-乙酰氨基肉桂酸，随后催化氢化后者，两个反应阶段在脂肪族C 3-酮与C 10 - 酮或水混溶性醚和水作为溶剂的混合物中进行，2-乙酰氨基肉豆蔻酸的氢化在10〜50℃的温度下进行。和在负载的钯催化剂存在下，压力为1至15巴。

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