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公开(公告)号：US4310686A
公开(公告)日：1982-01-12
申请号：US153572
申请日：1980-05-27
IPC分类号： C07C67/08 , B01J31/00 , B01J31/20 , C07B61/00 , C07C67/38 , C07C67/58 , C07C69/34 , C07C69/44
摘要： A process for the preparation of butanedicarboxylic acid esters, wherein(a) an aqueous cobalt salt solution is treated with excess carbon monoxide and hydrogen in the presence of active charcoal laden with cobalt carbonyl,(b) the resulting aqueous solution of cobalt carbonyl hydride is extracted with butadiene or a butadiene containing hydrocarbon mixture and the aqueous phase is separated off,(c) the butadiene, or butadiene/hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and excess C.sub.1 -C.sub.4 -alkanol in the presence of a tertiary nitrogen base,(d) the resulting reaction mixture is freed from the tertiary nitrogen base contained therein, down to a content of from 0.1 to 0.3 mole per mole of pentenoic acid ester, and from excess hydrocarbons, and the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and excess C.sub.1 -C.sub.4 -alkanol in the presence of the cobalt carbonyl and tertiary nitrogen base contained in the reaction mixture,(e) the reaction mixture is treated with an oxidizing agent in the presence of the aqueous acid solution which has been separated off in stage (b), and the mixture is separated into an organic phase, from which butanedicarboxylic acid esters are isolated by distillation, and an aqueous phase, and(f) the aqueous phase is extracted with water-immiscible solvents, the phases are separated, and the resulting aqueous phase is freed from alkanols and tertiary nitrogen base and is recycled to stage (a).
摘要翻译： 制备丁烷二羧酸酯的方法，其中（a）钴水溶液在过量的一氧化碳和氢气的存在下，在负载有羰基钴的活性炭存在下处理，（b）得到的氢化羰基碳水溶液为 用丁二烯或含丁二烯的烃混合物萃取并分离出水相，（c）含有羰基氢化钴，羰基钴和三丁基钴的三羰基化合物的丁二烯或丁二烯/烃混合物与一氧化碳和过量的C1 -C 4 - 链烷醇，（d）将所得反应混合物与其中所含的叔氮碱脱除，至每摩尔戊烯酸酯为0.1至0.3摩尔，过量 碳氢化合物和残留在反应混合物中的戊烯酸酯在羰基钴a存在下与一氧化碳和过量的C 1 -C 4烷醇反应 （e）反应混合物在步骤（b）中分离的酸性水溶液存在下用氧化剂处理，并将混合物分离成有机相 通过蒸馏分离丁二羧酸酯和水相，（f）水相用不与水混溶的溶剂萃取，分离相，所得水相脱离链烷醇和叔氮碱， 被回收到舞台（a）。
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2.发明授权Purification of carboxylates containing aldehydes, acetals and/or unsaturated compounds 失效含醛，缩醛和/或不饱和化合物的羧酸盐的纯化
公开(公告)号：US4523027A
公开(公告)日：1985-06-11
申请号：US518006
申请日：1983-07-28
CPC分类号： C07C67/60
摘要： Carboxylates which contain aldehydes, acetals and/or unsaturated compounds and are obtained by reacting an olefinically unsaturated compound with carbon monoxide and an alkanol are purified by a process wherein the said carboxylates are treated with hydrogen at elevated temperatures in the presence of an acidic ion exchanger or zeolite doped with one or more metals of group VIII of the periodic table, and the resulting low and/or high boilers are separated off by distillation.
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得到的含醛，缩醛和/或不饱和化合物的羧酸盐通过其中所述羧酸盐在酸性离子交换剂存在下在高温下用氢处理的方法进行纯化 或掺杂有周期表第Ⅷ族的一种或多种金属的沸石，并通过蒸馏分离得到的低和/或高沸点。
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公开(公告)号：US4316047A
公开(公告)日：1982-02-16
申请号：US166569
申请日：1980-07-07
IPC分类号： B01J31/00 , C07B61/00 , C07C69/533 , C07C67/38
CPC分类号： C07C69/533
摘要： A process for the preparation of C.sub.1 -C.sub.4 -alkyl pent-3-enoates, wherein butadiene, or a hydrocarbon mixture containing butadiene, either of which contains not more than 0.1% by weight of butynes, is reacted with carbon monoxide and an alkanol of 1 to 4 carbon atoms in the presence of a cobalt carbonyl catalyst and a tertiary nitrogen base, having a pK.sub.A of 3-11, at from 100.degree. to 140.degree. C. under a pressure of from 300 to 1,000 bar.
摘要翻译： 一种制备C 1 -C 4烷基戊-3-烯酸酯的方法，其中丁二烯或含有丁二烯的烃混合物（其中含有不超过0.1重量％的丁炔）与一氧化碳和链烷醇反应 在羰基钴催化剂和叔氮碱的存在下，在300-1000巴的压力下，pKA为3-11，在100-140℃下存在1至4个碳原子。
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公开(公告)号：US4801738A
公开(公告)日：1989-01-31
申请号：US608460
申请日：1984-05-09
IPC分类号： C07C67/313 , B01J29/12 , B01J31/00 , B01J31/20 , C07B61/00 , C07C67/333 , C07C67/38 , C07C69/67
CPC分类号： C07C67/347
摘要： .delta.-Formylvalerates are prepared by a process wherein a 3-pentenoate is treated with an isomerization catalyst at elevated temperatures and a 4-pentenoate is distilled off, and the resulting 4-pentenoate is reacted with carbon monoxide and hydrogen at from 80 to 160.degree. C. under from 1 to 30 bar in the presence of a rhodium carbonyl complex which has been modified with tertiary organic phosphines or phosphites.
摘要翻译： δ-甲酸戊酯通过其中3-异戊烯酸酯在高温下用异构化催化剂处理并蒸馏除去4-戊烯酸酯的方法制备，所得4-戊烯酸酯与一氧化碳和氢气在80至160℃下反应。 在1至30巴下，在用叔有机膦或亚磷酸酯改性的羰基铑络合物的存在下。
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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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6.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：US4259520A
公开(公告)日：1981-03-31
申请号：US2329
申请日：1979-01-10
IPC分类号： C07C67/38
CPC分类号： C07C67/38
摘要： In a process for the preparation of butanedicarboxylic acid esters by(a) reacting butadiene or hydrocarbon mixtures containing butadiene with carbon monoxide and a C.sub.1 -C.sub.4 -alkanol in the presence of a tertiary nitrogen base and a cobalt carbonyl catalyst at from 80.degree. to 150.degree. C. under superatmospheric pressure,(b) removing the greater part of the tertiary nitrogen base together with any excess hydrocarbon and(c) reacting the resulting pentenoic acid ester, in the presence of the catalyst remaining in the reaction mixture, and in the presence of the remaining amount of tertiary nitrogen base, with carbon monoxide and a C.sub.1 - to C.sub.4 -alkanol at from 140.degree. to 200.degree. C. under superatmospheric pressure, to give the butanedicarboxylic acid ester, the improvement wherein the reaction mixture in stage c) is substantially free from dissolved butadiene or butadiene bonded to the catalyst.Butanedicarboxylic acid esters may be used for the preparation of polymers.
摘要翻译： 在（a）将叔丁基或含有丁二烯的烃混合物与一氧化碳和C 1 -C 4烷醇在叔氮碱和羰基钴催化剂存在下反应制备丁烷二羧酸酯的方法中， （b）将大部分叔氮碱与任何过量的烃一起除去，和（c）使所得戊烯酸酯在残留在反应混合物中的催化剂存在下反应，并在 在超大气压下，在140℃至200℃下存在剩余量的叔氮碱，一氧化碳和一种C 1 -C 4烷醇，得到丁烷二羧酸酯，其中阶段c中的反应混合物 ）基本上不含结合到催化剂上的溶解的丁二烯或丁二烯。 丁二羧酸酯可用于制备聚合物。
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公开(公告)号：US4256909A
公开(公告)日：1981-03-17
申请号：US66552
申请日：1979-08-15
摘要： In a process for the preparation of dimethyl butanedicarboxylates, wherein(a) butadiene or a hydrocarbon mixture containing butadiene is reacted with carbon monoxide and methanol in the presence of a tertiary nitrogen base and a cobalt carbonyl catalyst at from 80.degree. to 150.degree. C. under superatmospheric pressure,(b) the greater part of the tertiary nitrogen base and any excess hydrocarbons are removed and(c) the methyl pentenoate thus obtained is reacted with carbon monoxide and methanol, in the presence of a cobalt carbonyl catalyst and the residual amount of tertiary nitrogen base, at from 140.degree. to 200.degree. C. under superatmospheric pressure, to give the dimethyl butanedicarboxylate, the improvement that the reaction mixture obtained in stage (a) after reaction of the butadiene is cooled until it separates into two phases, and a part-stream of from 20 to 80% by volume of the lower phase is recycled to stage (a).
摘要翻译： 在制备丁二酸二甲酯的方法中，其中（a）丁二烯或含有丁二烯的烃混合物在叔氮碱和羰基钴催化剂存在下在80-150℃下与一氧化碳和甲醇反应。 在超大气压下，（b）除去大部分叔氮碱和任何过量的烃，并且（c）由此获得的戊烯酸甲酯在羰基钴催化剂存在下与一氧化碳和甲醇反应，剩余量 的叔氮碱，在超大气压下，在140〜200℃下，得到丁二酸二甲酯，改善在丁二烯反应后阶段（a）中得到的反应混合物冷却至分离为两相， 并且将下层相的20〜80体积％的一部分流循环至（a）阶段。
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公开(公告)号：US4171451A
公开(公告)日：1979-10-16
申请号：US883216
申请日：1978-03-03
摘要： A process for the manufacture of butanedicarboxylic acid esters, wherein(a) an aqueous cobalt salt solution is treated, at from 50.degree. to 200.degree. C. and under a pressure of from 50 to 500 bars, with excess carbon monoxide and hydrogen in the presence of active charcoal laden with cobalt carbonyl,(b) the resulting aqueous solution of cobalt carbonyl hydride is extracted with butadiene or with a hydrocarbon mixture containing butadiene and the aqueous phase is separated off,(c) the butadiene, or butadiene-hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl is reacted with carbon monoxide and an excess of an alkanol of 1 to 4 carbon atoms in the presence of from 0.5 to 2 moles, per mole of butadiene, of a tertiary nitrogen base having a pK.sub.a of from 3 to 11, at from 80.degree. to 150.degree. C. under a pressure of from 300 to 2,000 bars, and(d) the resulting reaction mixture is freed from the tertiary nitrogen base contained therein, except for from 0.1 to 0.3 mole per mole of pentenoic acid ester, and from excess hydrocarbons, the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and an excess of an alkanol of 1 to 4 carbon atoms at from 140.degree. to 200.degree. C. and under pressures of from 100 to 400 bars in the presence of the amounts of cobalt carbonyl and tertiary nitrogen base contained in the reaction mixture, and excess alkanol and free nitrogen base are then distilled off, and(e) the reaction mixture which remains, and which contains cobalt catalyst, the butanedicarboxylic acid ester and by-products is treated with an oxidizing agent in an aqueous acid medium and the mixture is separated into an organic phase, from which the butanedicarboxylic acid ester is isolated by distillation, and into an aqueous phase containing cobalt salts.Butanedicarboxylic acid esters may be used for the manufacture of adipic acid and of nylons.
摘要翻译： 一种制备丁烷二羧酸酯的方法，其中（A）在50至200℃和50至500巴的压力下处理苛性钴盐溶液，其中过量的一氧化碳和氢气在 （B）碳酸氢盐的结晶水溶液是用丁二烯或含有二丁烯和水相的烃混合物分离的，（C）丁二烯或二苯乙烯混合物 ，含有碳酸氢二乙酯，碳酸氢钾和二苯乙酮三溴化硼与一氧化碳反应，另有1至4个碳原子的碱金属在0.5至2摩尔浓度范围内反应，每次可以达到丁二烯，碱性氮 在300至2,000巴的压力下具有3至11，80至150℃的PKa，以及（D）结合反应混合物来自含有其的碱性氮碱，除F 或从0.1至0.3毫升的硝酸酯和超级碳氢化合物，反应混合物中的硝酸酯反应在一氧化碳和超过1至4个碳原子的碱性物质在140°至200°的条件下反应 在反应混合物中所含的羰基钴和叔氮碱的量存在下，在100-400巴的压力下，然后蒸出过量的链烷醇和游离氮碱，和（E）反应混合物 剩余的，其中含有钴催化剂，溴化苹果酸酯和副产物与氧化剂在酸性介质中进行处理，并且混合物分离成有机相，其中通过蒸馏分离所述溴化乙酸酯，和 进入含有钴酸盐的水相。
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公开(公告)号：US4169956A
公开(公告)日：1979-10-02
申请号：US940463
申请日：1978-09-08
CPC分类号： C07C67/38
摘要： A process for the manufacture of butanedicarboxylic acid esters, wherein(a) an aqueous cobalt salt solution is treated with carbon monoxide and hydrogen in the presence of active charcoal,(b) the resulting aqueous solution is extracted with butadiene or with a hydrocarbon mixture containing butadiene,(c) the butadiene, or butadiene/hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and an excess of an alkanol of 1 to 4 carbon atoms in the presence of a tertiary nitrogen base,(d) the tertiary nitrogen bases contained in the resulting reaction mixture are removed from the latter to the extent of leaving from 0.1 to 0.3 mole per mole of pentenoic acid ester, excess hydrocarbons are also removed, the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and an alkanol of 1 to 4 carbon atoms, and thereafter excess alkanol and free nitrogen base are distilled off and(e) the residual reaction mixture, containing cobalt catalysts, butanedicarboxylic acids and by-products is treated with an oxidizing agent in an aqueous acid medium and the mixture is separated into an organic phase, from which butanedicarboxylic acid esters are isolated by distillation, and an aqueous phase containing cobalt salts, which phase is extracted with a water-immiscible solvent.
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