Purification of esters of tetrahydro-pyran-4-carboxylic acid
    31.
    发明授权
    Purification of esters of tetrahydro-pyran-4-carboxylic acid 失效
    四氢 - 吡喃-4-羧酸酯的纯化

    公开(公告)号:US5414097A

    公开(公告)日:1995-05-09

    申请号:US185179

    申请日:1994-01-24

    IPC分类号: C07D309/08

    CPC分类号: C07D309/08

    摘要: A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.

    摘要翻译: 用于纯化式I的四氢吡喃-4-羧酸的酯的方法,其中R 1至R 3各自为C 1 -C 4 - 烷基,R 2和R 3各自为氢, 其中R 2和R 3具有上述含义,R 4是氢,1-6个碳的烷基或式-CO-R 2的酰基,其中式R 1 OH的醇在存在下 氧化物催化剂,通过蒸馏,其需要a)在具有5-25理论塔板的第一塔中,馏出物压力为700-1100毫巴,馏出物温度为50-80℃,醇和升高 至10%的水,b)将底部产物从第一塔转移到具有18-40理论塔板的第二塔中,其中在15和30之间计量水夹带剂,并循环,并且其以 馏出液压力为35-350毫巴,馏出物温度为18-70℃, 其中四氢吡喃-4-羧酸的酯在90℃-150℃下在板8和18之间除去,并且在适当的情况下,c)将底部产物从第二塔进料到具有5-25理论值的第三塔 将塔顶馏出物返回到馏出物压力为1-100毫巴,馏出液温度为90-140℃,以合成四氢吡喃-4-羧酸酯。

    Process for preparing 6-aminocapronitrile
    34.
    发明授权
    Process for preparing 6-aminocapronitrile 失效
    6-氨基己腈的制备方法

    公开(公告)号:US6121481A

    公开(公告)日:2000-09-19

    申请号:US230837

    申请日:1999-02-01

    CPC分类号: C07C253/30 C07C209/60

    摘要: The invention concerns a process for the preparation of 6-aminocapronitrile or 6-aminocapronitrile-hexamethylene diamine mixtures by: a) reacting 5-formylvaleronitrile with ammonia and hydrogen in the presence of hydrogenation catalysts selected from the group consisting of metals or metal compounds rhenium, copper and elements of group VIII of the periodic table of elements, a hydrogenation discharge product being obtained; and b) extracting from the hydrogenation discharge product 6-aminocapronitrile and optionally hexamethylene diamine, provided that the hydrogenation catalyst does not contain copper, nickel or copper and nickel as it's only components.

    摘要翻译: PCT No.PCT / EP97 / 03987第 371日期1999年2月1日 102(e)1999年2月1日PCT 1997年7月23日PCT公布。 公开号WO98 / 05631 日期1998年2月12日本发明涉及通过以下方法制备6-氨基己腈或6-氨基己腈 - 六亚甲基二胺混合物的方法:a)在选自金属的氢化催化剂存在下,使5-甲酰基戊腈与氨和氢反应 或金属化合物铼,铜和元素周期表第Ⅷ族元素,得到氢化放电产物; 和b)从氢化放电产物6-氨基己腈和任选的六亚甲基二胺中提取,条件是氢化催化剂不含铜,镍或铜和镍,因为它是唯一的组分。

    Process for continuous purification of crude caprolactam prepared from
6-aminocapronitrile
    36.
    发明授权
    Process for continuous purification of crude caprolactam prepared from 6-aminocapronitrile 失效
    从6-氨基己腈制备的己内酰胺的连续纯化方法

    公开(公告)号:US5496941A

    公开(公告)日:1996-03-05

    申请号:US375410

    申请日:1995-01-18

    IPC分类号: C07D201/08 C07D201/16

    CPC分类号: C07D201/16 Y02P20/52

    摘要: Crude capronitrile is purified by hydrogenation, subsequent treatment in an acidic medium and subsequent distillation in an alkaline medium, by a process in which(a) 6-aminocapronitrile is converted into crude caprolactam by reaction with water,(b) high boilers and low boilers are separated off from the crude caprolactam from step (a),(c) the crude caprolactam from step (b) is treated with hydrogen at from 50.degree. to 150.degree. C. and from 1.5 to 250 bar in the presence of a hydrogenation catalyst and, if desired, of a solvent to give a mixture A,(d1) mixture A in a solvent is passed, at from 30.degree. to 80.degree. C. and from 1 to 5 bar, over an ion exchanger containing terminal acid groups to give a mixture B1, or(d2) mixture A is distilled in the presence of sulfuric acid, any solvent present being removed before the addition of the sulfuric acid, to give a mixture B2, and(e) mixture B1 or mixture B2 is distilled in the presence of a base to give pure caprolactam.

    摘要翻译: 通过氢化纯化粗碳腈,随后在酸性介质中处理,随后在碱性介质中进行蒸馏,其中(a)通过与水反应将(a)6-氨基己腈转化为粗己内酰胺,(b)高锅炉和低锅炉 与步骤(a)中的粗己内酰胺分离,(c)步骤(b)中的粗己内酰胺在氢化催化剂存在下在50-150℃和1.5-250巴下用氢处理 并且如果需要,得到溶剂以得到混合物A,(d1)溶剂中的混合物A在30℃至80℃和1至5巴条件下通过含有末端酸基团的离子交换剂 得到混合物B1,或(d2)在硫酸存在下蒸馏混合物A,在加入硫酸之前,除去存在的任何溶剂,得到混合物B2,并且(e)蒸馏出混合物B1或混合物B2 在碱的存在下得到纯己内酰胺。