Abstract:
PROBLEM TO BE SOLVED: To provide a production method of ε-caprolactam, for producing high-quality ε-caprolactam, which has fewer impurities, with a good yield.SOLUTION: The production method includes: an ε-caprolactam purification step A of obtaining purified ε-caprolactam from crude ε-caprolactam by applying a drop-crystallization method; a first-stage ε-caprolactam recovery step B of applying a vaporization crystallization method to a crystallization mother liquid obtained in the ε-caprolactam purification step A, to obtain a first recovered ε-caprolactam and a first recovered mother liquid; and a second-stage ε-caprolactam recovery step C of at least partially removing a solvent included in the first recovered mother liquid, applying a melting crystallization method to the concentrated first recovered mother liquid to obtain a second recovered purified ε-caprolactam. The first recovered ε-caprolactam is recovered as a raw material for the ε-caprolactam purification step A, and the second recovered purified ε-caprolactam is recovered as a raw material for any one of or both of the ε-caprolactam purification step A and the first-stage ε-caprolactam recovery step B.
Abstract:
PROBLEM TO BE SOLVED: To provide a regenerated catalyst with high activity prepared from a used catalyst in subjecting a cyclohexanone oxime to a Beckmann rearrangement reaction in a gas phase. SOLUTION: A solid catalyst used in subjecting the cyclohexanone oxime to the Beckmann rearrangement reaction in the gas phase is brought into contact with an aqueous solution containing at least one kind selected from among quaternary ammonium compounds and lower alkylamines and ammonia. Thus, the ε-caprolactam is produced at a high yield for a long time by regenerating and reusing the ε-caprolactam-producing catalyst using the described method. COPYRIGHT: (C)2004,JPO
Abstract:
PROBLEM TO BE SOLVED: To provide a method for producing ε-caprolactam from cyclohexanone in one step with a high selectivity. SOLUTION: This method for producing ε-caprolactam comprises reacting cyclohexanone with a nitrogen source and oxygen. Therein, the reaction is carried out in the presence of an oxide catalyst containing at least one element M selected from the groups 3-12 in the periodic table. The reaction is desirably performed in the presence of an oxide catalyst containing silicon and at least one element M selected from the groups 3-12 in the periodic table.
Abstract:
PROBLEM TO BE SOLVED: To remove water contained in a cyclohexanone oxime hydrochloride oily substance to be supplied to a Beckmann's rearrangement reaction. SOLUTION: Cyclohexanone oxime hydrochloride salt is mixed with an organic solvent (e.g. a halogenated hydrocarbon, chloroform, or 1,2- dichloroethane) poor in compatibility with water and large in compatibility with the cyclohexanone oxime hydrochloride and subsequently subjected to an azeotropic distillation treatment to separate and remove water contained in the salt.
Abstract:
PURPOSE: To provide an industrially useful process for producing ε-caprolactam having a quality comparable to that of the conventional products inexpensively. CONSTITUTION: In this process for production of ε-caprolactam where cyclohexanol as a hydration product of cyclohexene is dehydrogenated to cyclohexanone, which is converted into cyclohexanone oxime with hydroxylamine, further, the oxime product is subjected to the Beckmann rearrangement to be converted into ε-caprolactam, the content of methylcyclopentanol is kept lower than 200ppm in the cyclohexanol fed to the dehydrogenation process.
Abstract:
The present disclosure discloses a method for preparing caprolactam including: (1) contacting cyclohexanone oxime with a catalyst to carry out reaction in the presence of ethanol and under the condition of gas phase Beckmann rearrangement reaction of cyclohexanone oxime; (2) separating the reaction product obtained in step (1) to produce an ethanol solution of crude caprolactam, and then separating the ethanol solution of crude caprolactam to obtain ethanol and crude caprolactam; (3) removing impurities with boiling points lower than that of caprolactam in the crude caprolactam to obtain a light component removal product; (4) mixing the light component removal product with a crystallization solvent to carry out crystallization and solid-liquid separation to obtain a crystalline crystal; (5) subjecting the crystalline crystal to a hydrogenation reaction; wherein the crystallization solvent contains 0.1-2 wt % of ethanol.
Abstract:
Disclosed herein is an efficient, economical, industrially advantageous, straight-through process for the preparation of cyclic amides, also referred as lactams, in substantially pure form and high yield, from the corresponding cyclic ketones and a hydroxylammonium salt, using a combination of amphoteric metal oxide or amphoteric masked metal oxide and a base.