公开(公告)号：US4610768A

公开(公告)日：1986-09-09

申请号：US803752

申请日：1985-12-02

Applicant: Seid H. Moosavian

Inventor： Seid H. Moosavian

IPC: B01D3/36 ,  C07D201/16

CPC classification number: C07D201/16 ,  B01D3/36

Abstract: A process for drying lactams to extremely low water contents is provided which comprises mixing the lactam with hydrocarbon distilling from the mixture a water/hydrocarbon vapor and or condensate, contacting said vapor or condensate with a drying agent to remove water and returning the dried distillate to the mixture to permit recycling process is capable of providing anionic polymerization grade lactam with a water content of less than about 50 ppm.

Abstract translation: 提供了将内酰胺干燥至极低含水量的方法，其包括将内酰胺与从混合物中蒸馏出的水/烃蒸气和/或冷凝物混合，将所述蒸气或冷凝物与干燥剂接触以除去水并将干燥的馏出物返回到 允许再循环过程的混合物能够提供含水量小于约50ppm的阴离子聚合级内酰胺。

公开(公告)号：US4582642A

公开(公告)日：1986-04-15

申请号：US625143

申请日：1984-06-27

Applicant: Lamberto Crescentini ,  William B. Fisher ,  Richard E. Mayer ,  Joseph D. DeCaprio ,  Ronald K. Nilsen

Inventor： Lamberto Crescentini ,  William B. Fisher ,  Richard E. Mayer ,  Joseph D. DeCaprio ,  Ronald K. Nilsen

IPC: C07D201/16 ,  C07D201/12

CPC classification number: C07D201/16

Abstract: This invention is a method to recover caprolactam from a combined stream of mother liquor from a caprolactam crystallizer and other lactam containing aqueous streams, the improvement comprising steam distilling the combined stream at a temperature of from between about 180.degree. C. to 235.degree. C. in the absence of any depolymerization agent such as phosphoric acid; so that the residue from the steam distilling remains fluid; relatively low levels of caprolactam remain in the residue; less residue is generated; the recovered caprolactam has improved high quality; and losses of caprolactam due to side reactions are reduced.

Abstract translation: 本发明是从己内酰胺结晶器和其它含内含物含水流的母液的合并流中回收己内酰胺的方法，其改进包括在约180℃至235℃的温度下蒸馏合并的流。 在没有任何解聚剂如磷酸的情况下; 使蒸汽蒸馏残渣保持流体; 残余物中残留的己内酰胺水平相对较低; 产生较少的残留物; 回收的己内酰胺具有改善的高品质; 并且由于副反应而导致己内酰胺的损失降低。

公开(公告)号：US4293494A

公开(公告)日：1981-10-06

申请号：US143418

申请日：1980-04-24

Applicant: Paolo Senni ,  Domenico Astarita

Inventor： Paolo Senni ,  Domenico Astarita

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: 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.

Abstract translation: 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：US4276215A

公开(公告)日：1981-06-30

申请号：US818564

申请日：1977-07-25

Applicant: Eugene V. Hort ,  Waldo R. De Thomas

Inventor： Eugene V. Hort ,  Waldo R. De Thomas

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: 2-Pyrrolidone is purified by contact with particulate calcium oxide for a sufficient time at elevated temperatures followed by distilling and condensing the purified 2-pyrrolidone.

Abstract translation: 通过在高温下与颗粒状氧化钙接触足够的时间，然后蒸馏并冷凝纯化的2-吡咯烷酮，纯化2-吡咯烷酮。

公开(公告)号：US4170592A

公开(公告)日：1979-10-09

申请号：US832007

申请日：1977-09-09

Applicant: Harry Danziger ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Jurgen Schroter

Inventor： Harry Danziger ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Jurgen Schroter

IPC: C01C1/24 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the purification of a solution of .epsilon.-caprolactam in benzene, toluene or xylene by washing with a liquid, wherein the washing liquid is a solution of .epsilon.-caprolactam in water in a weight ratio of from 15 : 1 to 1 : 3, which is used in a quantity of from 5 to 20% by weight, based on the solution of caprolactam in benzene, toluene or xylene, and wherein there are several washing stages so that the equilibrium between the two solutions can be readjusted.

Abstract translation: 一种通过用液体洗涤来纯化ε-己内酰胺在苯，甲苯或二甲苯中的溶液的方法，其中洗涤液是ε-己内酰胺在水中的重量比为15:1至1:3的溶液 ，其用量为5至20重量％，基于己内酰胺在苯，甲苯或二甲苯中的溶液，并且其中有几个洗涤阶段，使得可以重新调节两种溶液之间的平衡。

公开(公告)号：US4049646A

公开(公告)日：1977-09-20

申请号：US261220

申请日：1972-06-09

Applicant: Herbert Furkert

Inventor： Herbert Furkert

IPC: C01B17/50 ,  C01C1/24 ,  C07D201/16 ,  C07D201/04

CPC classification number: C07D201/16 ,  C01B17/504 ,  C01C1/24 ,  Y02P20/129

Abstract: In a process for manufacturing a lactam which includes rearranging a cycloalkanone-oxime with sulfuric acid to form said lactam, neutralizing the rearrangement mixture with ammonia to form ammonium sulfate, and separating said lactam and said ammonium sulfate, the improvement which comprises:A. forming the ammonium sulfate into finely divided particles;B. burning the particles at a temperature of 850.degree. - 1250.degree. C. to form an SO.sub.2 -containing gas;C. oxidizing the SO.sub.2 -containing gas to form sulfuric acid; andD. recycling at least a portion of the sulfuric acid to the cycloalkanone-oxime rearrangement step.No external source of sulfuric acid is required. A portion of the SO.sub.2 -containing gas can be used for the manufacture of hydroxylamine sulfate, in which case no external source of SO.sub.2 need be required.

Abstract translation: 在制造内酰胺的方法中，其包括用硫酸重排环烷酮肟以形成所述内酰胺，用氨中和重排混合物形成硫酸铵，并分离所述内酰胺和所述硫酸铵，其改进包括：

公开(公告)号：US4021422A

公开(公告)日：1977-05-03

申请号：US601018

申请日：1975-08-01

Applicant: Abraham H. De Rooij ,  Jan Elmendorp

Inventor： Abraham H. De Rooij ,  Jan Elmendorp

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: In commercial processes for producing epsilon-caprolactam, the caprolactam product is in admixture with sulfuric acid. An improved process for removing sulfuric acid from the caprolactam results from treating the admixture with ammonia at superatmospheric pressure.

Abstract translation: 在用于生产ε-己内酰胺的商业方法中，己内酰胺产物与硫酸混合。 通过在超大气压下处理与氨的混合物，从己内酰胺中除去硫酸的改进方法。

公开(公告)号：US3975377A

公开(公告)日：1976-08-17

申请号：US562905

申请日：1975-03-28

Applicant: Claude Poulain

Inventor： Claude Poulain

IPC: C07D201/16 ,  C07D201/14

CPC classification number: C07D201/16

Abstract: A process for preparing pure N-alkyl-lactams obtained by the reaction, in an organic solvent medium of, the corresponding lactamate of an alkali metal and an alkyl halide. This process consists of treating a reactive mixture of N-alkyl-lactam containing the corresponding cyclo-alkylene imine as an impurity with a current of carbon dioxide, until the cyclo-alkylene imine precipitates completely in the form of an insoluble carbonate, and then separating it from the precipitate.

Abstract translation: 通过在相应的碱金属和烷基卤的乳酸盐的有机溶剂介质中通过反应制备纯N-烷基 - 内酰胺的方法。 该方法包括将含有作为杂质的相应环 - 亚烷基亚胺的N-烷基 - 内酰胺的反应性混合物与二氧化碳的电流进行处理，直到环 - 亚烷基亚胺完全沉淀为不溶性碳酸酯的形式，然后分离 它从沉淀中。

公开(公告)号：US3882102A

公开(公告)日：1975-05-06

申请号：US40904673

申请日：1973-10-24

Applicant: BAYER AG

Inventor： IMMEL OTTO ,  SCHWARZ HANS-HELMUT

IPC: C07D201/16 ,  C07D41/06

CPC classification number: C07D201/16

Abstract: The invention relates to a process for the purification of caprolactam which is obtained by rearrangement of cyclohexanone oxime in the gas phase in the presence of solid catalysts. The purification takes place by dissolving the crude lactam in benzene or in alkyl benzene with seven to eight carbon atoms and recrystallization whilst cooling.

Abstract translation: 本发明涉及通过在固相催化剂存在下在气相中重排环己酮肟而得到的己内酰胺的纯化方法。 通过将粗内酰胺溶解在苯或具有7至8个碳原子的烷基苯中并在冷却下重结晶来进行纯化。

公开(公告)号：US3820972A

公开(公告)日：1974-06-28

申请号：US24972872

申请日：1972-05-02

Applicant: STAMICARBON

Inventor： DE ROOIJ A

IPC: C05B11/06 ,  C07D201/16 ,  C05B11/08

CPC classification number: C07D201/16 ,  C05B11/06 ,  C05B11/08 ,  C05B19/00

Abstract: A process for the recovery of lactams from a Beckmann rearrangement mixture of lactams and sulphuric acid or sulphur trioxide, with the production of a phosphate-containing fertilizer is disclosed. The Beckmann rearrangement mixture is partially neutralized by the addition of ammonium or alkali metal hydroxide, sulphate or carbonate in an amount such that the molar ratio between the sulphate formed and the sum of the sulphate formed and the free sulphuric acid is at least 1/8:1. Thereafter, the resulting partially neutralized solution is extracted by a substantially water-immiscible, organic lactam solvent to separate lactam from the remainder of said mixture, and the remainder of said mixture after such extraction is used for the decomposition of rock phosphate with formation of gypsum and of a free phosphoric acid-containing solution. This latter solution, after removal of gypsum and neutralization of the solution with ammonia or alkali liquor is converted into a dihydrogen phosphate-containing solution from which dihydrogen phosphate, suitable for use in fertilizers, is recovered after evaporative concentration. The process provides for the ready separation of lactams from a Beckmann rearrangement reaction mixture, while at the same time producing, as a by-product, dihydrogen phosphate or a valuable dihydrogen phosphate containing fertilizer.