Continuous production of ethanol and plural stage distillation of the
same
    4.
    发明授权
    Continuous production of ethanol and plural stage distillation of the same 失效
    连续生产乙醇和多级蒸馏相同

    公开(公告)号:US4454358A

    公开(公告)日:1984-06-12

    申请号:US337683

    申请日:1982-01-07

    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

    Preparation of butanedicarboxylic esters
    6.
    发明授权
    Preparation of butanedicarboxylic esters 失效
    丁烷二羧酸酯的制备

    公开(公告)号:US4310686A

    公开(公告)日:1982-01-12

    申请号:US153572

    申请日:1980-05-27

    CPC分类号: C07C69/34 C07C67/38

    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)。

    Preparation of C.sub.1 -C.sub.4 -alkyl pent-3-enoates
    8.
    发明授权
    Preparation of C.sub.1 -C.sub.4 -alkyl pent-3-enoates 失效
    制备C1-C4烷基戊-3-烯酸酯

    公开(公告)号:US4316047A

    公开(公告)日:1982-02-16

    申请号:US166569

    申请日:1980-07-07

    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。

    Preparation of 5-methylbutyrolactone
    9.
    发明授权
    Preparation of 5-methylbutyrolactone 失效
    5-甲基丁酰胺的制备

    公开(公告)号:US5189182A

    公开(公告)日:1993-02-23

    申请号:US236199

    申请日:1988-08-25

    IPC分类号: C07D315/00

    CPC分类号: C07D315/00

    摘要: 5-Methylbutyrolactone is prepared by a process in which a pentenoic ester of the formula IX--CO.sub.2 R (I),where X is CH.sub.2 .dbd.CH--CH.sub.2 --CH.sub.2 --, CH.sub.3 --CH.dbd.CH--CH.sub.2 -- or CH.sub.3 --CH.sub.2 --CH.dbd.CH-- and R is alkyl, cycloalkyl, aralkyl or aryl, or a mixture of these esters is reacted with water at from 50.degree. to 350.degree. C. in the presence or absence of a diluenta) over a zeolite and/or phosphate catalyst orb) in the presence of from 0.01 to 0.25 mole of a sulfonic acid, a Lewis acid and/or a non-oxidizing mineral acid per mole of pentenoic ester or over from 0.1 to 40% by weight, based on the pentenoic ester, of a strongly acidic ion exchanger as a catalyst in a first stage, or the pentenoic ester of the formula I, where X and R have the stated meanings, is hydrolyzed in a first stage with the aid of a strongly acidic ion exchanger as a catalyst to give the pentenoic acid of the formula I, where R is hydrogen, and the resulting pentenoic acid is subjected to cyclization in a second stage in the presence of from 0.005 to 0.1 mole of a sulfonic acid, a Lewis acid or a non-oxidizing mineral acid per mole of pentenoic acid or over from 0.1 to 20% by weight, based on the pentenoic acid, of a strongly acidic ion exchanger at from 50.degree. to 350.degree. C.

    摘要翻译: 通过以下方法制备5-甲基丁内酯,其中式I X-CO 2 R(I)的戊烯酸酯,其中X为CH 2 = CH-CH 2 -CH 2 - ,CH 3 -CH = CH-CH 2 - 或CH 3 -CH 2 -CH = CH-和R是烷基,环烷基,芳烷基或芳基,或这些酯的混合物与水在50-350℃下在存在或不存在稀释剂a)的情况下与沸石和/或磷酸盐 催化剂或b)在0.01至0.25摩尔磺酸,路易斯酸和/或非氧化性无机酸/摩尔烯酸酯存在下或基于戊烯酸酯为0.1至40重量% 的作为第一阶段的催化剂的强酸性离子交换剂或其中X和R具有所述含义的式I的戊烯酸在第一阶段中借助于强酸性离子交换剂作为 催化剂得到式I的戊烯酸,其中R是氢,所得戊烯酸在第二阶段中在0.005t的存在下进行环化 o 0.1摩尔磺酸,路易斯酸或非氧化性无机酸/摩尔烯酸,或超过0.1-20重量%,基于戊烯酸,强酸性离子交换剂为50〜 350℃