公开(公告)号：US4385965A

公开(公告)日：1983-05-31

申请号：US342975

申请日：1982-01-26

申请人： Wolfgang H. E. Muller ,  Manfred Kaufhold

发明人： Wolfgang H. E. Muller ,  Manfred Kaufhold

IPC分类号： C07C41/00 ,  C07C41/58 ,  C07C43/303 ,  C07C67/00 ,  B01D3/26

CPC分类号： C07C41/58

摘要： In a process for recovering pure methylal from methanol-methylal mixtures, which can optionally contain still further compounds, the separation conducted in a rectification device comprising two rectifying columns. In the first rectifying column, the mixture to be separated is rectified under a pressure lower than that in the second column, into a methylal-rich, methanol-poor distillate, and into a practically methylal-free, methanol-rich sump product. The methylal-rich distillate of the first rectification is then separated in a second rectifying column, operated under a higher pressure than the first rectification column, into a compound stream containing methanol and methylal, which is then recycled to the first rectifying column, and into pure methylal as the sump product. In a specific refinement, the first rectification is preferably operated under a pressure of 1-22 bar absolute and the second rectification preferably under a pressure of 9-30 bar absolute, with the second rectification being operated under a pressure which is at least 8 bar higher than that of the first rectification.

摘要翻译： 在从可以任选地含有其它化合物的甲醇 - 甲缩醛混合物中回收纯甲缩醛的方法中，在包括两个精馏塔的精馏装置中进行分离。 在第一精馏塔中，将待分离的混合物在低于第二塔的压力下进行精馏，成为富含甲缩醛的不饱和甲醇的馏出物，并进入实际上无甲醛的富含甲醇的油槽产物。 然后将第一精馏的甲缩醛馏出物在比第一精馏塔高的压力下操作的第二精馏塔中分离成含有甲醇和甲缩醛的复合物流，然后将其再循环至第一精馏塔，并进入 纯甲缩醛作为贮槽产品。 在特定的改进中，第一精馏优选在1-22巴绝对压力下操作，优选在9-30巴绝对压力下进行第二次精馏，第二次精馏在至少8巴的压力下操作 高于首次整改。

公开(公告)号：US4421691A

公开(公告)日：1983-12-20

申请号：US270851

申请日：1981-06-05

申请人： Wolfgang H. E. Muller ,  Peter Hofmann

发明人： Wolfgang H. E. Muller ,  Peter Hofmann

IPC分类号： C07C69/02 ,  B01J23/94 ,  B01J31/00 ,  B01J31/02 ,  C07B61/00 ,  C07C20060101 ,  C07C67/00 ,  C07C67/04 ,  C07C67/38 ,  C07C69/24

CPC分类号： C07C67/38

摘要： A process for preparing fatty acid esters by reacting olefins, alkanols and carbon monoxide in the presence of a compound of cobalt and a promoter consisting of pyridine, non-orthosubstituted alkylpyridines or mixtures thereof. The reaction output is at first treated with a gas containing oxygen in a non-damaging manner and then reprocessed in two distillation stages. The first distillation stage is operated at a higher pressure than the second. In the first distillation stage there is produced a distillate free of cobalt and a sump product containing all of the cobalt used as catalyst. In the second distillation stage the sump product of the first distillation stage is again distilled to produce another distillate free of cobalt and a cobalt concentrate as sump product. This cobalt concentrate is incorporated into pyridine, a non-orthosubstituted alkylpyridine or a mixture thereof to form a suspension. The suspension is then treated by a mixture of carbon monoxide and hydrogen at a temperature of 100.degree. to 250.degree. C. and a pressure at least 50 bars, and this treatment product is fed back into the fatty acid ester synthesis.

摘要翻译： 在钴化合物和由吡啶，非取代的烷基吡啶或其混合物组成的促进剂的存在下，使烯烃，aklanols和一氧化碳反应制备脂肪酸酯的方法。 首先用非破坏性方式用含氧气体处理反应产物，然后在两个蒸馏阶段再处理。 第一个蒸馏阶段的操作压力高于第二个。 在第一蒸馏阶段，产生不含钴的馏出物和含有用作催化剂的所有钴的贮槽产物。 在第二蒸馏阶段，再次蒸馏第一蒸馏阶段的贮槽产物以产生不含钴的另一种馏出物和作为贮槽产物的钴浓缩物。 将该钴浓缩物并入吡啶，非邻位取代的烷基吡啶或其混合物中以形成悬浮液。 然后将悬浮液在一氧化碳和氢气的混合物中在100至250℃的温度和至少50巴的压力下处理，并将该处理产物反馈到脂肪酸酯合成中。

公开(公告)号：US5091594A

公开(公告)日：1992-02-25

申请号：US625400

申请日：1990-12-11

申请人： Friedrich-Wilhelm Kupper ,  Wolfgang H. E. Muller ,  Alfred Oberholz

发明人： Friedrich-Wilhelm Kupper ,  Wolfgang H. E. Muller ,  Alfred Oberholz

IPC分类号： B01J31/14 ,  C07B61/00 ,  C07C37/14 ,  C07C39/06

CPC分类号： C07C37/14

摘要： For producing 2,6-di-tert-butylphenol and products therefrom, utilizing small quantities of aluminum tris-(2-tert-butylphenolate as a catalyst by reaction of 2-tert-butylphenol with isobutene in the liquid phase, the reaction is performed in the presence of diluents such as liquid saturated aliphatic or cycloaliphatic hydrocarbons, C.sub.5 -C.sub.16 alkenes of formula R.sub.1 --CH.dbd.CH.sub.2 or R.sub.2 --CH.dbd.CH--R.sub.3, C.sub.5 to C.sub.12 cycloalkenes, which contain no branching on the C.dbd.C-bond, excess isobutene or mixtures thereof, at temperatures of 0.degree. C. to 80.degree. C., pressures of 0.1 to 11 bars and catalyst amounts of 0.005 to 5 mol %, based on 2-tert-butylphenol. High conversions are obtained with few undesirable trialkylated products.

摘要翻译： 为了制备2,6-二叔丁基苯酚及其产物，使用少量的三 - （2-叔丁基苯酚）铝作为催化剂，通过2-叔丁基苯酚与异丁烯在液相中反应，进行反应 在稀释剂如液体饱和脂族或脂环族烃存在下，式R 1 -CH = CH 2或R 2 -CH = CH-R 3的C5-C16烯烃，C = C键上不含支链的C 5 -C 12环烯烃 ，过量异丁烯或其混合物，在0℃至80℃的温度下，0.1至11巴的压力和0.005至5摩尔％的催化剂量，基于2-叔丁基苯酚，获得高转化率，少量 不希望的三烷基化产物。

公开(公告)号：US4332645A

公开(公告)日：1982-06-01

申请号：US167443

申请日：1980-07-10

申请人： Wolfgang H. E. Muller ,  Michael Zolffel

发明人： Wolfgang H. E. Muller ,  Michael Zolffel

IPC分类号： C07C29/80 ,  C02F1/04 ,  C07C27/00 ,  C07C31/04 ,  C07C67/00 ,  C07D307/08 ,  B01D3/00 ,  C07D307/00

CPC分类号： C07D307/08 ,  Y10S203/20

摘要： A process for the continuous separation of methanol and water from a feed mixture containing predominantly tetrahydrofuran admixed with water, methanol and small amounts of additional compounds, in a rectifying apparatus having at last two rectifying columns, of which two are operated at different pressures which involves feeding the raw material into a first column operated under lower pressure, and introducing the distillate from the column operated under a lower pressure to a second column operated under a higher pressure, while a product stream from the second column operated under a higher pressure is reintroduced into the first column operated under a lower pressure. In this process the product stream withdrawn from the second column operated under a higher pressure is withdrawn as a side stream from the stripping or enrichment section of the second column and is returned into the first column operated under a lower pressure, while a methanol-enriched product stream containing practically all of the methanol introduced with the raw material into the rectifying apparatus is withdrawn from the head of the second column operated under a higher pressure. The first column is operated for example at atmospheric pressure and the second column is operated at a pressure of from 1 to 25 bar.

摘要翻译： 在最后两个精馏塔的精馏装置中，甲醇和水从主要包含四氢呋喃混合的进料混合物中连续分离出来的方法，其中两个精馏塔在不同的压力下操作， 将原料进料到在较低压力下操作的第一塔中，并将来自在较低压力下操作的塔的馏出物引入到在较高压力下操作的第二塔中，同时再次引入来自第二塔的产物流 进入在较低压力下运行的第一列。 在该方法中，从较高压力下运行的第二塔排出的产物流作为来自第二塔的汽提或富集段的侧流排出，并返回到在较低压力下运行的第一塔中，同时富含甲醇 将从原料中引入的几乎所有的甲醇的整个装入整流装置的产物流从高压运转的第二塔的头部取出。 第一列例如在大气压下操作，第二列在1至25巴的压力下操作。

公开(公告)号：US4421692A

公开(公告)日：1983-12-20

申请号：US318661

申请日：1981-11-05

申请人： Peter Hofmann ,  Wolfgang H. E. Muller

发明人： Peter Hofmann ,  Wolfgang H. E. Muller

IPC分类号： C07C67/38 ,  B01J31/00 ,  C07B61/00 ,  C07C27/00 ,  C07C29/136 ,  C07C29/149 ,  C07C31/02 ,  C07C67/00 ,  C11C3/02

CPC分类号： C07C29/149

摘要： A method for preparing carboxylic acid alkylester after products free of nitrogen containing compounds. These after products, free of nitrogen containing compounds, are prepared by:(1) reacting olefins with carbon monoxide and alkanols in the presence of a catalyst system consisting of a cobalt compound and pyridine, non-orthosubstituted alkylpyridines or a mixture of these pyridines at elevated pressures and elevated temperatures to produce carboxylic acid alkylesters containing nitrogenated compounds resulting from the pyridines;(2) hydrogenating the carboxylic acid alkylesters to produce after products which include alcohols; and(3) treating the after products with acid ion exchangers to remove the nitrogenated compounds.

摘要翻译： 在不含氮化合物的产品之后制备羧酸烷基酯的方法。 这些不含氮化合物的产物通过以下方法制备：（1）在由钴化合物和吡啶，非邻位取代的烷基吡啶或这些吡啶的混合物组成的催化剂体系存在下，使烯烃与一氧化碳和链烷醇反应 升高的压力和升高的温度以产生含有由吡啶衍生的含氮化合物的羧酸烷基酯; （2）使羧酸烷基酯氢化以产生包括醇的产物; 和（3）用酸性离子交换剂处理后产物以除去含氮化合物。

公开(公告)号：US4222823A

公开(公告)日：1980-09-16

申请号：US720356

申请日：1976-09-03

申请人： Reinhold Wickbold ,  Wolfgang H. E. Muller ,  Hans Regner ,  Gunter Scharein ,  Franz Langheim ,  Rolf Ruthemeier ,  Karl-Hans Simmrock ,  Rolf Baumann

发明人： Reinhold Wickbold ,  Wolfgang H. E. Muller ,  Hans Regner ,  Gunter Scharein ,  Franz Langheim ,  Rolf Ruthemeier ,  Karl-Hans Simmrock ,  Rolf Baumann

IPC分类号： B01J19/00 ,  C07C17/00 ,  C07C17/38 ,  C07C19/01 ,  C07C21/04 ,  C07C67/00 ,  B01D1/22 ,  C01B7/08 ,  C10B57/04

CPC分类号： C07C17/38

摘要： The processing of liquid chlorinated hydrocarbon residues, which may contain solids and which form viscous to solid deposits during the separation of readily boiling components, into(1) distillable organic components,(2) hydrogen chloride, and(3) solid matter with a low chlorine content,is improved by gently concentrating the residues in a first step and, in a second step, decomposing the residues at temperatures of about 200.degree.-400.degree. C., preferably 270.degree.-330.degree. C., with a continuous separation of the vapor phase components from the solid components.

摘要翻译： 液体氯化烃残渣的处理可能含有固体，并且在容易沸腾的组分分离过程中形成粘稠的固体沉积物，成为（1）可蒸馏的有机组分，（2）氯化氢和（3）低浓度的固体物质 氯含量通过在第一步骤中轻轻浓缩残余物而得到改善，并且在第二步骤中，在约200-400℃，优选270-330℃的温度下分解残余物，连续分离 来自固体组分的气相成分。

公开(公告)号：US4571284A

公开(公告)日：1986-02-18

申请号：US673405

申请日：1984-11-20

申请人： Wolfgang H. E. Muller ,  Werner Boxkes ,  Heinz Scholten

发明人： Wolfgang H. E. Muller ,  Werner Boxkes ,  Heinz Scholten

IPC分类号： C07D265/30 ,  C07D295/02 ,  C07D295/027 ,  B01D3/10

CPC分类号： C07D295/027

摘要： A separation of mixtures of water and 2,6-dimethylmorpholine is carried out by rectifying the mixtures at a pressure at the head of the column between 6 and 150 mbars. The separated 2,6-dimethylmorpholine has a maximum water content of 500 ppm by weight and it is possible to achieve for a corresponding design of the rectification water contents of less than 1 ppm by weight of dimethylmorpholine.

摘要翻译： 水和2,6-二甲基吗啉的混合物的分离是通过在塔顶部的压力下在6至150毫巴之间的压力下对混合物进行精馏来进行的。 分离的2,6-二甲基吗啉的最大含水量为500重量ppm，可以实现精馏水含量的相应设计小于1重量ppm的二甲基吗啉。

公开(公告)号：US4427593A

公开(公告)日：1984-01-24

申请号：US291915

申请日：1981-08-11

申请人： Peter Hofmann ,  Wolfgang H. E. Muller

发明人： Peter Hofmann ,  Wolfgang H. E. Muller

IPC分类号： C07C67/38 ,  B01J31/00 ,  B01J31/02 ,  B01J31/20 ,  B01J31/28 ,  B01J31/40 ,  C07B61/00 ,  C07C20060101 ,  C07C69/24 ,  C11C3/02

CPC分类号： C07C67/38

摘要： A process for producing predominantly linear aliphatic carboxylic acid esters by reacting olefins, carbon monoxide and alkanols at elevated pressures and elevated temperatures in the presence of a catalyst consisting of a cobalt compound and a promoter. The promoter is the possibly cobalt-free mixture of substances obtained when a reaction mixture that was prepared by reacting olefins, carbon monoxide and alkanol in the presence of a catalyst consisting of a cobalt compound and pyridine, a non-ortho-substituted alkylpyridine or mixtures at elevated pressure and elevated temperature is reprocessed. This mixture of substances has a higher boiling point than the esters formed as the reaction product and higher than the pyridine, non-ortho-substituted alkylpyridine or mixtures thereof used as the catalytic component.

摘要翻译： 通过在由钴化合物和助催化剂组成的催化剂存在下，在升高的压力和升高的温度下使烯烃，一氧化碳和链烷醇反应制备主要为直链的脂族羧酸酯的方法。 当在由钴化合物和吡啶组成的催化剂，非邻位取代的烷基吡啶或非邻位取代的烷基吡啶或其混合物存在下，通过使烯烃，一氧化碳和链烷醇反应制备的反应混合物时，助催化剂是可能不含钴的物质混合物 在升高的压力和升高的温度下进行后处理。 这种物质混合物的沸点高于作为反应产物形成的酯，并且高于用作催化组分的吡啶，非邻位取代的烷基吡啶或其混合物。

公开(公告)号：US4420429A

公开(公告)日：1983-12-13

申请号：US291952

申请日：1981-08-11

申请人： Wolfgang H. E. Muller ,  Peter Hofmann

发明人： Wolfgang H. E. Muller ,  Peter Hofmann

IPC分类号： C07C67/38 ,  B01J31/00 ,  B01J31/02 ,  B01J31/20 ,  C07B61/00 ,  C07C20060101 ,  C07C69/24 ,  C11C3/02

CPC分类号： C07C67/38 ,  Y02P20/582

摘要： A process for the production of alkyl esters of saturated aliphatic carboxylic acids made by reacting olefins with carbon monoxide and alkanol in the presence of a catalyst consisting of a cobalt compound and a promoter selected from pyridine, a non-ortho-substituted alkylpyridine or mixtures thereof at elevated pressure and temperature and with feedback of unconverted input materials, the water contained in the reaction mixture being separated as much as possible during the reprocessing from the flows of substances slated for feedback.

摘要翻译： 在由钴化合物和选自吡啶，非邻位取代的烷基吡啶或其混合物的助催化剂组成的催化剂存在下，通过使烯烃与一氧化碳和链烷醇反应制备的饱和脂族羧酸烷基酯的方法 在升高的压力和温度以及未转化的输入材料的反馈下，反应混合物中包含的水在从预期反应的物质的流中进行再处理期间尽可能地分离。

公开(公告)号：US4400300A

公开(公告)日：1983-08-23

申请号：US256384

申请日：1981-04-22

申请人： Wolfgang H. E. Muller ,  Peter Hofmann

发明人： Wolfgang H. E. Muller ,  Peter Hofmann

IPC分类号： C07C67/38 ,  B01J31/40 ,  B01J38/68 ,  C07C67/48

CPC分类号： B01J31/0244 ,  B01J31/04 ,  B01J31/20 ,  B01J31/403 ,  C07C67/38 ,  B01J2231/321 ,  B01J2531/845 ,  B01J31/181 ,  Y02P20/584

摘要： A process for recovering and reactivating catalysts used in the reaction of olefins with carbon monoxide and alkanols. The catalysts consist of a cobalt compound and pyridine, a non-ortho-substituted alkylpyridine or a mixture thereof as the promoter. The reacted mixture contains fatty acid ester, unconverted alkanol, uncoverted olefin, catalyst and promoter and this reacted mixture is treated with oxygen or an oxygenated gas at a temperature of about 20.degree.-150.degree. C. to oxidize the cobalt compound. The oxidized mixture is then separated by distillation to remove unconverted alkanol and olefin, the promoter, the reaction products and the distillation residue obtained thereby is mixed with pyridine, a non-ortho-substituted alkylpyridine or a mixture thereof. The suspension so obtained is treated with a mixture of carbon monoxide and hydrogen at a temperature of 100.degree. to 250.degree. C. and at a pressure of at least 50 bars.

摘要翻译： 用于回收和再活化烯烃与一氧化碳和链烷醇反应中使用的催化剂的方法。 催化剂由钴化合物和吡啶组成，非邻位取代的烷基吡啶或其混合物作为助催化剂。 反应的混合物含有脂肪酸酯，未转化的链烷醇，未转化的烯烃，催化剂和促进剂，并将该反应的混合物在约20-150℃的温度下用氧气或氧化气体处理以氧化钴化合物。 然后通过蒸馏分离氧化的混合物以除去未转化的链烷醇和烯烃，将由此得到的促进剂，反应产物和蒸馏残余物与吡啶，非邻位取代的烷基吡啶或其混合物混合。 如此获得的悬浮液在100-250℃的温度和至少50巴的压力下用一氧化碳和氢气的混合物处理。