Abstract:
A process for producing cyclohexanone oxime is provided: (1) reacting cyclohexanone, hydrogen peroxide and ammonia in the presence of a titanosilicate catalyst to give a reaction solution containing cyclohexanone oxime, water, unreacted ammonia and unreacted cyclohexanone, (2) distilling off ammonia, (3) an extraction step, (4) mixing the organic layer obtained in step (3) with water followed by separating into an organic aqueous layers, (5) distilling off organic solvent and water to obtain a bottom product containing cyclohexanone oxime and cyclohexanone oxime, and (6) distilling off cyclohexanone and obtain a bottom product containing cyclohexanone oxime; wherein a compound selected from an oxide, an oxo acid, an oxo acid salt, an oxo acid ester and an oxo acid amide of boron or phosphorous is added to at least one of the water used in step (4) and the organic layer obtained in step (4) to be subjected to step (5).
Abstract:
Methods are disclosed of producing and purifying at least one amide. In accordance with one of the methods disclosed herein, the at least one amide is produced by providing an organic liquid comprising at least one oxime, providing at least one catalyst, adding the at least one catalyst to the organic liquid to form a rearrangement mass, wherein the rearrangement mass comprises at least one amide, at least one impurity, and the at least one catalyst, and heating the rearrangement mass to a temperature of at least about 115° C. for a period of time in order to sulfonate, break down and/or reduce the concentration of some of the at least one impurity in the rearrangement mass.
Abstract:
The present invention provides a method for manufacturing a zeolite comprising following steps of: (1): calcining crystals obtained by hydrothermal synthesis reaction of a silicon compound; (2): contact treating a calcined product obtained by the step (1) with an aqueous solution including an amine and/or a quaternary ammonium compound; (3): calcining a treated product obtained by the step (2); and (4): contact treating the calcined product obtained by the step (3) with an aqueous solution including ammonia and/or an ammonium salt. According to the present invention, a method is also provided wherein ε-caprolactam is manufactured by Beckmann rearrangement reaction of cyclohexanone oxime in a gaseous phase in the presence of the zeolite manufactured by the above-described method.
Abstract:
The present invention relates to a process for the preparation of zeolitic catalysts of the MFI type in spheroidal form. The process consists in emulsifying and consolidating in paraffinic hydrocarbons, in the presence of a non-ionic surface-active agent or a suitable combination of a non-ionic surface-active agent and a cationic surface-active agent, a dispersion of particles of zeolitic material of the MFI type in a silica sol.
Abstract:
In the production of null-caprolactam by contacting cyclohexanone oxime with a solid acid catalyst in the gaseous phase to effect a rearrangement reaction of the cyclohexanone oxime, wherein the solid acid catalyst is produced by calcining a dried catalyst precursor: in a first aspect, the catalyst precursor comprises a zeolite, a crystalline clay mineral and at least one substance selected from the group consisting of an inorganic oxide and a compound which forms the inorganic oxide by calcination, wherein the inorganic oxide comprises an oxide of at least one element selected from the group consisting of elements belonging to Groups 4, 13 and 14 of the Periodic Table and wherein the inorganic oxide is other than oxides contained in a crystalline form in the zeolite and the crystalline clay mineral; or in a second aspect, the rearrangement reaction is effected in the presence of a polyhydric alcohol derivative represented by the following formula: R1nullOnullR2nullOH (wherein: R1 represents a C1-C5 alkyl group or a phenyl group, and R2 represents a C2-C5 alkylene group).
Abstract:
The present invention relates to a process for the preparation of zeolitic catalysts of the MFI type in spheroidal form. The process consists in emulsifying and consolidating in paraffinic hydrocarbons, in the presence of a non-ionic surface-active agent or a suitable combination of a non-ionic surface-active agent and a cationic surface-active agent, a dispersion of particles of zeolitic material of the MFI type in a silica sol.
Abstract:
A method for producing a lactam by using an organic solvent as a substrate solution, which makes it possible to introduce a high-concentration oxime into flowing high-temperature and high-pressure water, thereby allowing the high-concentration lactam to be synthesized with a high efficiency. With this method, the lactam is continuously synthesized at a high rate from the oxime under high-temperature and high-pressure water mixture conditions within a temperature range of no less than 250null C. and a pressure range of no less than 15 MPa.
Abstract:
The subject-matter of the invention is a process for the preparation of cyclododecanone oxime by photonitrosation of cyclododecane in the presence of hydrochloric acid, characterized in that the nitrosing agent is trichloronitrosomethane.
Abstract:
A process for producing a high purity caprolactam is disclosed in which a crude caprolactam obtained by a catalytic rearrangement of cyclohexanone oxime is subjected(1) to mixing, while stirring, with at least one hydrocarbon selected from the group consisting of aliphatic hydrocarbons and alicyclic hydrocarbons to form a liquid-liquid, two-layer liquid mixture, and then crystallizing caprolactam out of the liquid mixture;(2) to mixing with both at least one hydrocarbon selected from the group consisting of aliphatic hydrocarbons and alicyclic hydrocarbons, and water to form a liquid mixture, separating the liquid mixture into a hydrocarbon layer and a water layer, and then recovering caprolactam from the water layer; or(3) to distillation in the co-presence of at least one aliphatic saturated hydrocarbon of 10 to 18 carbon atoms.
Abstract:
.epsilon.-Caprolactam is prepared by bringing cyclohexanone oxime into contact in gas phase with solid catalysts such as a zeolite catalyst in the presence of at least one nitrogen-containing compound selected from the group consisting of ammonia, methylamines and .epsilon.-caprolactam.