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21.发明授权Isolation and regeneration of rhodium-containing catalysts from distillation residues of hydroformylation reactions 失效从加氢甲酰化反应的蒸馏残余物中分离和再生含铑催化剂
公开(公告)号：US4113754A
公开(公告)日：1978-09-12
申请号：US780297
申请日：1977-03-23
IPC分类号： B01J31/40 , B01J38/68 , B01J38/74 , C07B61/00 , C07C45/00 , C07C45/50 , C07C47/02 , C07C67/00 , C07F15/00
CPC分类号： B01J31/4046 , B01J31/20 , B01J31/24 , B01J31/2404 , C07C45/50 , B01J2231/321 , B01J2531/822 , Y02P20/582 , Y02P20/584
摘要： The isolation and regeneration of catalysts of type I or IIclRh(CO)(PR.sub.3).sub.2 Ihrh(CO)(PR.sub.3).sub.3 II,where the R's are identical or different hydrocarbon radicals, to give the catalysts in a pure form, is effected by regenerating aqueous rhodium salt solutions, as obtained on treating distillation residues of hydroformylation mixtures with oxygen-containing mineral acids and peroxides, by a method wherein the said aqueous rhodium salt solutions are treated with a cation exchanger, the latter is then separated from the solution, the absorbed rhodium ions are desorbed with hydrochloric acid, the hexachlororhodate solutions, containing hydrochloric acid, are reacted, in the presence of a water-soluble organic solvent and a tertiary phosphine PR.sub.3, with carbon monoxide, or with compounds which eliminate carbon monoxide, at from 0.degree. to 150.degree. C and from 1 to 5 bars, and the resulting complexes I or, if the process is carried out under hydrogenating conditions, the resulting complexes II, are separated off.
摘要翻译： 分离和再生I或II型ClRh（CO）（PR3）2I HRh（CO）（PR3）3II的催化剂，其中R是相同或不同的烃基，得到纯形式的催化剂，是通过 通过其中所述水合铑盐溶液用阳离子交换剂处理的方法，在用含氧无机酸和过氧化物处理加氢甲酰化混合物的蒸馏残余物时获得的再生铑水溶液溶液，然后将该铑盐溶液与溶液分离， 吸收的铑离子用盐酸解吸，含有盐酸的六氯乙酸溶液在水溶性有机溶剂和叔膦PR3存在下与一氧化碳或与一氧化碳消除的化合物反应， 0至150℃和1至5巴，所得的络合物I或如果该方法在氢化条件下进行，则得到的络合物II为sepa 评分。
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22.发明授权
公开(公告)号：US4454358A
公开(公告)日：1984-06-12
申请号：US337683
申请日：1982-01-07
IPC分类号： C07C29/132 , B01J31/00 , B01J31/20 , C07B61/00 , C07C27/00 , C07C27/04 , C07C29/149 , C07C29/80 , C07C29/92 , C07C31/08 , C07C67/00 , B01D3/00
CPC分类号： C07C29/80 , C07C29/149 , C07C67/08 , C07C67/36 , C07C67/54 , Y02P20/52 , Y10S203/06 , Y10S203/20
摘要： Ethanol is produced continuously via the carbonylation of methanol, by(a) carbonylating methanol, in a reactor R, in the presence of a carbonyl complex of a metal of group VIII of the periodic table and of a halogen compound,(b) separating, in a distillation column D1, the reactor discharge, into a top fraction comprising methyl acetate, methanol, dimethyl ether and an organohalogen compound, and into a bottom fraction comprising water, small quantities of acetic acid and the catalyst, if the latter is not in a fixed bed, the residence time being so adjusted that the greater part of the acetic acid reacts with the methanol present to give methyl acetate,(c) separating the top fraction from D1, in a distillation column D2, into a top fraction comprising small quantities of methyl acetate, methanol, dimethyl ether and the organo-halogen compound, and a bottom fraction comprising methyl acetate and methanol, and recycling the top fraction to reactor R,(d) distilling off, via the top of distillation column D3, the greater part of the water from the bottom fraction from D1and removing this water from circulation, and recycling to reactor R the bottom fraction consisting of small quantities of water, acetic acid and the catalyst,(e) using hydrogen to hydrogenate, in the hydrogenation reactor H, the bottom fraction from D2, in a conventional manner, to give a mixture of methanol and ethanol, and(f) separating the mixture into ethanol and methanol in a distillation column D4, and recycling the methanol to reactor R.
摘要翻译： 通过（a）在反应器R中羰基化甲醇，在周期表第VIII族金属的羰基络合物和卤素化合物的存在下，连续生产乙醇，（b）分离， 在蒸馏塔D1中，反应器排出成为包含乙酸甲酯，甲醇，二甲醚和有机卤素化合物的顶级馏分，并进入包含水，少量乙酸和催化剂的底部馏分，如果后者不在 固定床，停留时间如此调节，使得大部分乙酸与存在的甲醇反应得到乙酸甲酯，（c）将蒸馏塔D2中的顶馏分与D1分离成包含小分子的顶馏分 数量的乙酸甲酯，甲醇，二甲醚和有机卤素化合物，以及包含乙酸甲酯和甲醇的底部馏分，并将顶部馏分再循环到反应器R中，（d）通过顶部o蒸馏 f蒸馏塔D3，来自D1的底部馏分的大部分水从循环中除去，并且将反应器R再循环到由少量水，乙酸和催化剂组成的底部馏分，（e）使用氢气 以常规方式在氢化反应器H中将来自D2的塔底馏分氢化，得到甲醇和乙醇的混合物，和（f）将混合物在蒸馏塔D4中分离成乙醇和甲醇，并将甲醇再循环至 反应器
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23.发明授权
公开(公告)号：US4350572A
公开(公告)日：1982-09-21
申请号：US204637
申请日：1980-11-06
CPC分类号： C07C67/60
摘要： A process for purifying carboxylic acid esters which have been obtained by reacting olefinically unsaturated compounds with carbon monoxide and alkanols and which contain aldehydes or acetals, wherein the said esters are treated with a strongly acidic agent, with or without addition of water.
摘要翻译： 通过使烯属不饱和化合物与一氧化碳和链烷醇反应并且含有醛或缩醛而获得的羧酸酯的方法，其中所述酯用强酸性剂处理，或不加入水。
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公开(公告)号：US4305888A
公开(公告)日：1981-12-15
申请号：US813971
申请日：1977-07-08
IPC分类号： C07C55/02 , C07C51/00 , C07C55/10 , C07C55/12 , C07C55/14 , C07C55/16 , C07C55/18 , C07C55/20 , C07C55/21 , C07C67/00 , C07C209/00 , C07C211/09 , C07C87/14
摘要： A process for the manufacture of salts of alkanedicarboxylic acids of 4 to 12 carbon atoms and alkanediamines of 3 to 14 carbon atoms, comprising reacting esters of alkanols of 1 to 4 carbon atoms and alkanedicarboxylic acids of 4 to 12 carbon atoms with alkanediamines of 3 to 14 carbon atoms in stoichiometric amounts in the presence of water at an elevated temperature, with continuous removal of the alkanols formed, in which process the reaction is carried out, from the start, in the presence of the particular salt of alkanedicarboxylic acid and alkanediamine which is to be manufactured.
摘要翻译： 一种制备4至12个碳原子的链烷二羧酸盐和3至14个碳原子的烷二胺的方法，包括使1至4个碳原子的链烷醇与4至12个碳原子的烷基二羧酸酯与3个烷二胺反应 在高温存在下，在水存在下，化学计算量为14个碳原子，连续除去所形成的链烷醇，在该过程中进行反应，从一开始就在特定的烷基二羧酸和烷二胺盐存在下 将被制造。
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公开(公告)号：US4258203A
公开(公告)日：1981-03-24
申请号：US58944
申请日：1979-07-19
CPC分类号： C07C67/38
摘要： Multistep process for the preparation of butanedicarboxylic acid by the hydrogenation of carbon monoxide under pressure in the presence of a cobalt carbonyl catalyst, the improvement of heating at a temperature of 250.degree. to 350.degree. C. under superatmospheric pressure the resulting aqueous solution of cobalt carbonyl hydride that has been extracted with butadiene or with mixtures thereof before using in a subsequent step of the multistep process.
摘要翻译： 通过在羰基钴催化剂存在下加压一氧化碳制备丁烷二羧酸的多步法，在超大气压下在250℃至350℃的温度下加热，得到羰基钴水溶液 氢化物，在多步骤的后续步骤中使用之前已用丁二烯或其混合物萃取。
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公开(公告)号：US5817592A
公开(公告)日：1998-10-06
申请号：US590455
申请日：1996-01-23
IPC分类号： B01J23/42 , B01J23/96 , B01J37/16 , B01J38/64 , C01B21/14 , B01J21/18 , B01J23/16 , B01J27/185
CPC分类号： B01J23/42 , B01J37/16 , C01B21/1418
摘要： A process for the preparation of a hydrogenation catalyst by reduction of platinum in an oxidation stage of not less than 2 in an aqueous medium in the presence of a carboniferous support, optionally following partial poisoning with a sulfur, arsenic, tellurium, or antimony-containing compound, using a reducing agent, in which the reducing agent used is an ammonium or phosphonium salt of the general formula I �XR.sup.4 !.sub.n Y I in which X stands for N or P, R stands for hydrogen, C.sub.1 --C.sub.18 alkyl, C.sub.5 --C.sub.10 cycloalkyl, phenyl radical, and also a C.sub.1 --C.sub.4 alkyl radical substituted by phenyl, the phenyl radicals being mono-to tri-substituted by C.sub.1 --C.sub.6 alkyl, halogen, nitro or amino, if desired, provided that the radicals R may be the same or different but cannot simultaneously denote hydrogen, if X is P, n is an integer of 1 to 3, and Y is an organic anion which can reduce platinum in an oxidation stage other than zero to platinum in the oxidation stage of zero.
摘要翻译： 一种通过在含水载体的存在下在水性介质中在不少于2的氧化阶段还原铂的氢化催化剂的方法，任选地在用硫，砷，碲或含锑的部分中毒后 化合物，使用还原剂，其中所用的还原剂是通式I [XR4] nYinin的铵盐或鏻盐，其中X代表N或P，R代表氢，C1-C18烷基，C5-C10环烷基 苯基，以及被苯基取代的C1-C4烷基，如果需要，苯基由C1-C6烷基，卤素，硝基或氨基单取代至三取代，条件是基团R可以相同 或不同，但不能同时表示氢，如果X为P，n为1至3的整数，Y为有机阴离子，在氧化阶段为零的情况下，铂可以在除氧以外的氧化阶段中还原为铂。
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公开(公告)号：US07056356B2
公开(公告)日：2006-06-06
申请号：US10296442
申请日：2001-05-21
申请人： Peter Mark Allen , Christoph Gahn , Christopher William Rieker , Heinz-Walter Schneider , Robert Wagner
发明人： Peter Mark Allen , Christoph Gahn , Christopher William Rieker , Heinz-Walter Schneider , Robert Wagner
IPC分类号： B01D9/00
CPC分类号： B01D9/0022 , B01D9/0031 , B01D9/0036 , B01D9/0059
摘要： An apparatus and a process for crystallizing substances from solutions or dispersions containing these substances, in a crystallizer containing a classifying zone (3), comprise a) an inner and an outer circulation system (1; 2), the inner circulation system (1) being present in the crystallizer, the inlet of the outer circulation system (2) being connected to the inner circulation system (1) via the classifying zone (3), the outer circulation system, being present outside the crystallizer, the outlet of the outer circulation system (2) being connected to the inner circulation system (1) of the crystallizer, and a means for dissolving crystals being arranged in the outer circulation system (2), before its outlet, b) an inflow (4) for solution and/or dispersion, which inflow is present on the crystallizer or on the outer circulation system, and c) an outflow (5) for dispersions, which outflow is arranged on the crystallizer or on the outer circulation system. The novel apparatus has the special feature that a line (8) connecting the outer and inner circulation systems (1; 2) to one another and intended for transporting (recycling) dispersion and/or a line (8) for transporting (recycling) dispersion are additionally present, in which both its entrance and its exit are connected to the inner circulation system (1).
摘要翻译： 一种用于在含有分级区（3）的结晶器中使含有这些物质的溶液或分散液中的物质结晶的装置和方法包括：a）内循环系统（1; 2），内循环系统（1） 存在于结晶器中，外循环系统（2）的入口经由分级区（3）连接到内循环系统（1），外循环系统存在于结晶器外部，外部出口 循环系统（2）连接到结晶器的内循环系统（1），以及用于溶解布置在外循环系统（2）中的晶体在其出口之前的装置，b）用于溶液的流入物（4） /或分散体，其流入存在于结晶器或外循环系统上，以及c）用于分散体的流出物（5），该流出物布置在结晶器或外循环系统上。 该新型装置的特征在于，将外部和内部循环系统（1; 2）彼此连接并用于运输（再循环）分散体和/或用于运输（再循环）分散体的管线（8）的管线（8） 另外存在，其入口和出口都连接到内循环系统（1）。
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公开(公告)号：US5554353A
公开(公告)日：1996-09-10
申请号：US384321
申请日：1995-02-01
CPC分类号： C01B21/1418
摘要： A process for the preparation of hydroxylammonium salts by catalytic reduction of nitrogen monoxide using hydrogen in the presence of a hydrogenation catalyst, comprises(a) in a first step, filtering the reaction mixture obtained after the reaction, giving a solution of essentially hydroxylammonium salt and a filter residue essentially comprising a mixture of hydrogenation catalyst and a solution of essentially hydroxylammonium salt, and(b) in a second step, subjecting the filter residue to a further separation process in order to concentrate the hydrogenation catalyst, giving a mixture having a higher concentration of hydrogenation catalyst than the filter residue and a mixture having a lower concentration of hydrogenation catalyst than the filter residue.
摘要翻译： 在氢化催化剂存在下通过使用氢气催化还原一氧化氮制备羟基铵盐的方法包括（a）在第一步骤中，过滤反应后获得的反应混合物，得到基本上羟基铵盐的溶液和 基本上包含氢化催化剂和基本上羟基铵盐的溶液的混合物的过滤残余物，和（b）在第二步中，将过滤残余物进行进一步的分离过程以浓缩氢化催化剂，得到具有较高 氢化催化剂的浓度比过滤残渣和氢化催化剂浓度低于过滤残渣的混合物。
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公开(公告)号：US4730041A
公开(公告)日：1988-03-08
申请号：US7789
申请日：1987-01-28
申请人： Hans-Martin Hutmacher , Franz Merger , Franz J. Broecker , Rolf Fischer , Uwe Vagt , Wolfgang Harder , Claus-Ulrich Priester , Heinz-Walter Schneider , Wolfgang Richter
发明人： Hans-Martin Hutmacher , Franz Merger , Franz J. Broecker , Rolf Fischer , Uwe Vagt , Wolfgang Harder , Claus-Ulrich Priester , Heinz-Walter Schneider , Wolfgang Richter
IPC分类号： B01J23/74 , B01J23/78 , B01J25/00 , C07B61/00 , C07D201/08
CPC分类号： C07D201/08 , Y02P20/52
摘要： Caprolactam is prepared by a process in which(a) a 5-formylvalerate is reacted with excess ammonia and hydrogen in the presence of an alkanol as a solvent and in the presence of a hydrogenation catalyst under superatmospheric pressure in the liquid phase at from 40.degree. to 130.degree. C.,(b) excess ammonia and hydrogen are separated off from the reaction mixture and(c) the reaction mixture thus obtained is heated to 150.degree.-250.degree. C. and .epsilon.-caprolactam is obtained.
摘要翻译： 己内酰胺通过以下方法制备：其中（a）5-烷基戊酸酯与过量的氨和氢在烷醇作为溶剂的存在下和氢化催化剂的存在下在超大气压下在40℃的液相中反应 至130℃，（b）从反应混合物中分离出过量的氨和氢，（c）将所得反应混合物加热至150-250℃，得到ε-己内酰胺。
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公开(公告)号：US6083468A
公开(公告)日：2000-07-04
申请号：US155908
申请日：1998-10-08
CPC分类号： B01J23/42 , C01B21/1418
摘要： A hydrogenation catalyst is prepared by reduction of platinum in an oxidation state of not less than two using a reducing agent in an aqueous medium in the presence of a carbon-containing support after partial poisoning, where use is made of a compound of the general formula I ##STR1## where X, Y and Z can be identical or different and are hydrogen, C.sub.1 -C.sub.18 -alkyl, C.sub.5 -C.sub.10 -cycloalkyl, halogen, hydroxyl, C.sub.1 -C.sub.6 -alkoxy and --NR'R", where R, R' and R" can be identical or different and can be hydrogen, C.sub.1 -C.sub.18 -alkyl or C.sub.5 -C.sub.10 -cycloalkyl. Such a hydrogenation catalyst can be used for preparing hydroxylammonium salts and the process for preparing the above catalysts can also be used for regenerating hydrogenation catalysts based on platinum.
摘要翻译： PCT No.PCT / EP97 / 01617 Sec。 371日期：1998年10月8日 102（e）日期1998年10月8日PCT 1997年4月1日PCT PCT。 出版物WO97 / 37758 日期：1997年10月16日氢化催化剂是通过在部分中毒后在含碳载体存在下，在水性介质中使用还原剂还原不少于2的铂的氢化催化剂，其中使用 其中X，Y和Z可以相同或不同，为氢，C 1 -C 18 - 烷基，C 5 -C 10 - 环烷基，卤素，羟基，C 1 -C 6 - 烷氧基和-NR'R“的通式I化合物， 其中R，R'和R“可以相同或不同，并且可以是氢，C 1 -C 18 - 烷基或C 5 -C 10 - 环烷基。 这种氢化催化剂可用于制备羟铵盐，并且制备上述催化剂的方法也可用于再生基于铂的氢化催化剂。
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