C07D201/06

Ammonium Sulphate Production on Industrial Scale

The invention provides a process for the production of crystalline ammonium sulfate, wherein the process comprises performing a Beckmann rearrangement reaction, neutralizing the Beckmann rearrangement reaction mixture, separating a first aqueous ammonium sulfate phase and an aqueous ε-caprolactam phase, charging the first ammonium sulfate phase to a first evaporative type crystallization section wherein crystalline ammonium sulfate is obtained, discharging from the first evaporative type crystallization section mother liquor enriched in organic components, extracting the aqueous ε-caprolactam phase to obtain an extracted ε-caprolactam phase and a second aqueous ammonium sulfate phase, discharging the mother liquor that is discharged from the first evaporative type crystallization section and/or the second aqueous ammonium sulfate phase to a second evaporative type crystallization section wherein evaporative type crystallization is performed so that a three-phase system occurs. At least a liquid oily phase is recovered from the three-phase system. The invention further provides a plant suitable to carry out the process of the invention, crystalline ammonium sulfate and a liquid oily phase obtained by the process of the invention.

Ammonium Sulphate Production on Industrial Scale

The invention provides a process for the production of crystalline ammonium sulfate, wherein the process comprises performing a Beckmann rearrangement reaction, neutralizing the Beckmann rearrangement reaction mixture, separating a first aqueous ammonium sulfate phase and an aqueous ε-caprolactam phase, charging the first ammonium sulfate phase to a first evaporative type crystallization section wherein crystalline ammonium sulfate is obtained, discharging from the first evaporative type crystallization section mother liquor enriched in organic components, extracting the aqueous ε-caprolactam phase to obtain an extracted ε-caprolactam phase and a second aqueous ammonium sulfate phase, discharging the mother liquor that is discharged from the first evaporative type crystallization section and/or the second aqueous ammonium sulfate phase to a second evaporative type crystallization section wherein evaporative type crystallization is performed so that a three-phase system occurs. At least a liquid oily phase is recovered from the three-phase system. The invention further provides a plant suitable to carry out the process of the invention, crystalline ammonium sulfate and a liquid oily phase obtained by the process of the invention.

Process for the purification of caprolactam from a solution of crude caprolactam without organic solvent extraction

The present invention relates to a process for purifying caprolactam from solutions of crude caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process. A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

Process for the purification of caprolactam from a solution of crude caprolactam without organic solvent extraction

The present invention relates to a process for purifying caprolactam from solutions of crude caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process. A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

Refining process and refining system of caprolactam

A refining process includes steps of subjecting crude caprolactam to a first evaporative crystallization and a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor; washing the first caprolactam crystal to obtain a second caprolactam crystal; optionally concentrating the first crystallization mother liquor to perform a second evaporative crystallization and a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor; subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam; optionally concentrating the second crystallization mother liquor to perform thermostatic crystallization, performing separation to obtain a fifth caprolactam crystal and a third crystallization mother liquor; washing the fifth caprolactam crystal to obtain a sixth caprolactam crystal; and subjecting the second caprolactam crystal to a hydrogenation reaction.

PROCESS FOR THE PURIFICATION OF CAPROLACTAM FROM A SOLUTION OF CRUDE CAPROLACTAM WITHOUT ORGANIC SOLVENT EXTRACTION
20210040036 · 2021-02-11 ·

The present invention relates to a process for purifying caprolactam from solutions of crude caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process.

A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

PROCESS FOR THE PURIFICATION OF CAPROLACTAM FROM A SOLUTION OF CRUDE CAPROLACTAM WITHOUT ORGANIC SOLVENT EXTRACTION
20210040036 · 2021-02-11 ·

The present invention relates to a process for purifying caprolactam from solutions of crude caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process.

A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

Preparation method of caprolactam

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.

Process for the purification of caprolactam from a solution of crude caprolactam without organic solvent extraction
20190382339 · 2019-12-19 ·

The present invention relates to a process for purifying caprolactam from solutions of cmde caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process. A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

Process for the purification of caprolactam from a solution of crude caprolactam without organic solvent extraction
20190382339 · 2019-12-19 ·

The present invention relates to a process for purifying caprolactam from solutions of cmde caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process. A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.