公开(公告)号：US4328154A

公开(公告)日：1982-05-04

申请号：US203367

申请日：1980-11-03

申请人： Paolo Senni ,  Mario Catoni ,  Domenico Astarita

发明人： Paolo Senni ,  Mario Catoni ,  Domenico Astarita

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： A process for the purification of raw caprolactam obtained by extraction h alkylated phenols from its sulphuric solution, re-extraction with water, oxidation preferably with KMnO.sub.4, evaporation of water and distillation, comprises, before the oxidation treatment, a "fast distillation", in the presence of an alkali. The oxidation is conducted at 0.degree.-80.degree. C. and at atmospheric pressure with 0.005-0.5% by weight of KMnO.sub.4. The amount of alkali (NaOH) used in the fast distillation is comprised between 0.05 and 0.5% by weight.

摘要翻译： 通过从其硫酸溶液中用烷基化酚萃取得到的己内酰胺的纯化方法，用水重新萃取，优选用KMnO 4进行氧化，蒸发水和蒸馏，在氧化处理之前包括“快速蒸馏” 碱的存在。 氧化在0〜80℃，大气压下进行，重量为0.005〜0.5％的KMnO4。 在快速蒸馏中使用的碱（NaOH）的量为0.05-0.5重量％。

公开(公告)号：US4293494A

公开(公告)日：1981-10-06

申请号：US143418

申请日：1980-04-24

申请人： Paolo Senni ,  Domenico Astarita

发明人： Paolo Senni ,  Domenico Astarita

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： A method for purifying raw caprolactam containing, as impurities, primary amides of the formula ##STR1## R being a hydrocarbon radical having 1-14 carbon atoms, and other by-products is described. The operations, carried out in the following order, consist in (a) treating a solution of raw caprolactam in a water insoluble organic solvent with water to extract most of the caprolactam in purified form, (b) separating the aqueous caprolactam solution and isolating the caprolactam, (c) treating the remaining organic solution with mineral acid to cause the formation of two phases, (d) separating these phases into a heavy phase containing the mineral acid, dilution water and most of the amides and by-products and a light phase containing the organic solvent and any residual amides and by-products, and (e) preferably recycling the light phase to (a). Further object of the invention is the purified caprolactam thus obtained.

摘要翻译： 描述了含有作为杂质的具有1-14个碳原子的烃基的式（I）的初级酰胺和其它副产物的原己内酰胺的纯化方法。 按以下顺序进行的操作包括：（a）用水处理含水的不溶于水的有机溶剂中的己内酰胺溶液以提取大部分纯化形式的己内酰胺，（b）分离己内酰胺水溶液并分离 己内酰胺，（c）用无机酸处理剩余的有机溶液以形成两相，（d）将这些相分离成含有无机酸，稀释水和大部分酰胺和副产物的重相和轻质 相包含有机溶剂和任何残留的酰胺和副产物，和（e）优选将轻相循环至（a）。 本发明的另一个目的是由此获得的纯化的己内酰胺。

公开(公告)号：US4326925A

公开(公告)日：1982-04-27

申请号：US122675

申请日：1980-02-19

申请人： Paolo Senni ,  Domenico Astarita

发明人： Paolo Senni ,  Domenico Astarita

IPC分类号： C07D201/16 ,  B01D3/34

CPC分类号： C07D201/16

摘要： A process for purifying caprolactame by continuous and/or discontinuous (oratch) vacuum distillation comprises a first stage fast vacuum distillation of the raw caprolactame possibly in the presence of an alkaline and/or alkaline-earth hydroxide, a second stage consisting of a vacuum rectification distillation of the caprolactame obtained in the first stage and a third stage consisting of the fast vacuum distillation of the caprolactame yielded from the second stage, in the presence of an alkaline and/or alkaline-earth hydroxide. The hydroxide amount in the third and possibly the first stage distillation as well varies from 0.05 to 5% preferably from 0.1% to 1%.

摘要翻译： 通过连续和/或不连续（或分批）真空蒸馏纯化己内酰胺的方法包括可能在碱性和/或碱土金属氢氧化物存在下的原始己内酰胺的第一阶段快速真空蒸馏，第二阶段由真空 在第一阶段获得的己内酰胺的精馏蒸馏和由碱和/或碱土金属氢氧化物存在下由第二阶段产生的己内酰胺的快速真空蒸馏组成的第三阶段。 在第三阶段和可能的第一阶段蒸馏中的氢氧化物量也为0.05至5％，优选为0.1％至1％。

公开(公告)号：US4578511A

公开(公告)日：1986-03-25

申请号：US587896

申请日：1984-03-09

申请人： Pietro P. Rossi ,  Paolo Senni ,  Sergio Ferruzzi

发明人： Pietro P. Rossi ,  Paolo Senni ,  Sergio Ferruzzi

IPC分类号： C07C51/48 ,  C07C51/43 ,  C07C63/06 ,  C07C51/42

CPC分类号： C07C51/43

摘要： The invention is concerned with a method of purifying benzoic acid, as obtained by catalytic oxidation of toluene and purification by rectification with the secondary streams being cycled back into the oxidation reactor, characterized in that the secondary streams flowing out of the stripping column undergo the following sequential steps: (a) at least one distillation and at least one crystallization in an organic solvent; (b) scrubbing of the crystals obtained from (a) with the same solvent as in (a); (c) cycling of the mother liquors from crystallization in (a) plus the scrubbing liquors as in (b) back into the dissolver; (d) further scrubbing of the crystals from (b) with the same solvent as in (a) and cycling back of the scrubbing liquors, the crystals scrubbed as in (d) being optionally (d1) further scrubbed with water.

摘要翻译： 本发明涉及一种纯化苯甲酸的方法，其通过甲苯的催化氧化获得并通过使二次流循环回到氧化反应器中的精馏进行纯化，其特征在于，从汽提塔流出的二次流经历以下步骤 顺序步骤：（a）在有机溶剂中进行至少一次蒸馏和至少一次结晶; （b）用与（a）中相同的溶剂洗涤由（a）获得的晶体; （c）母液从（a）中加入洗涤液（如（b））中的结晶循环回到溶解器中; （d）用（b）用与（a）中相同的溶剂进一步洗涤晶体并循环回洗液，如（d）中洗涤的晶体任选地（d1）进一步用水洗涤。

公开(公告)号：US4314940A

公开(公告)日：1982-02-09

申请号：US142860

申请日：1980-04-21

申请人： Paolo Senni ,  Nando Toderi

发明人： Paolo Senni ,  Nando Toderi

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： A method for the purification of raw caprolactam containing primary amidesf the formula ##STR1## wherein R is a hydrocarbon radical having 1-14 carbon atoms is described. The raw caprolactam is treated with at least one compound containing at least one hydroxyl group, in an amount of at least 20% by weight with respect to the raw caprolactam, at a temperature equal to or higher than that at which the ammonia, which is a part of the amide of formula I, is liberated. The caprolactam is then separated and isolated from the hydroxyl containing compound by known methods.

摘要翻译： 描述了含有其中R为具有1-14个碳原子的烃基的式（Ⅰ）的伯酰胺的原始己内酰胺的纯化方法。 在等于或高于氨的温度下，将至少一种含有至少一个羟基的化合物与至少20重量％的量相对于原己内酰胺一起处理， 一部分式I的酰胺被释放出来。 然后通过已知方法将己内酰胺分离并从含羟基化合物中分离。

公开(公告)号：US4647661A

公开(公告)日：1987-03-03

申请号：US845122

申请日：1986-03-27

申请人： Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

发明人： Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

IPC分类号： C07D201/16 ,  C07D201/08 ,  C07D201/10

CPC分类号： C07D201/08

摘要： A method of preparing .omega.-lactams, in particular caprolactam, comprising: a step of premixing cycloaliphatic acids having the formula ##STR1## where n=3-13, with a dehydrating agent; the first step of reaction with a nitrosating agent; the second step of reaction with the addition of a very small amount of water corresponding to a molar ratio U=H.sub.2 O/SO.sub.3 within the 0.1 to 0.9 range; and the step of reclaiming the unreacted cycloaliphatic acid. The method affords improved output from the lactamization reaction and reduced byproducts.

摘要翻译： 一种制备ω-内酰胺，特别是己内酰胺的方法，包括：将具有式“IMAGE”的其中n = 3-13的脂环族酸与脱水剂预混合的步骤; 与亚硝化剂反应的第一步; 反应的第二步骤是加入相当于0.1至0.9范围内的摩尔比U = H 2 O / SO 3的非常少量的水; 以及回收未反应的脂环族酸的步骤。 该方法提供了来自内酰胺化反应的改进的产物和减少的副产物。

公开(公告)号：US4606858A

公开(公告)日：1986-08-19

申请号：US699520

申请日：1985-02-07

申请人： Enrico Bondi ,  Paolo Senni

发明人： Enrico Bondi ,  Paolo Senni

IPC分类号： C07D223/10 ,  C07D201/16

CPC分类号： C07D201/16

摘要： The invention is concerned with a method of purifying caprolactam as obtained by Beckmann transposition or by nitrosation of cyclohexyl compounds, characterized in that it comprises the following steps:(a) the caprolactam oil is treated with ammonia to obtain a pH in the 8 to 10 range;(b) the caprolactam in water-ammonia solution yielded by (a) is extracted with toluene;(c.sub.1) any caprolactam still in the toluene solution yielded by (b) is treated with NaOH;(C.sub.2) the aqueous phase left over from the extraction with toluene (b) is removed.

摘要翻译： 本发明涉及通过Beckmann转位或通过环己基化合物的亚硝化得到的己内酰胺的纯化方法，其特征在于其包括以下步骤：（a）己内酰胺油用氨处理以获得8至10的pH 范围; （b）由（a）产生的水 - 氨溶液中的己内酰胺用甲苯萃取; （c1）由（b）产生的仍然在甲苯溶液中的任何己内酰胺用NaOH处理; （C2）除去用甲苯（b）从萃取液中留下的水相。