Abstract:
A process is disclosed in which the heat generated, during neutralization,y ammonium sulfate of a solution of .xi.-caprolactam in sulfuric acid, is used to effect evaporation of water present, and the temperature is kept at about 40.degree.C to 50.degree.C, under subatmospheric pressure, so that substantial hydrolysis of the caprolactam is avoided while a substantial portion of the water present in the neutralization mixture is evaporated at the subatmospheric pressure, and the ammonium sulfate is crystallized substantially free from entrained caprolactam. The caprolactam is then separated from the aqueous phase.
Abstract:
1. IN A PROCESS FOR THE RECOVERY PURE E-CAPROLACTAM CONTAINING LESS THAN 5 MEQ. OF IONOGENIC SUBSTANCES PER KG. OF LACTAM, OBTAINED BY INTRAMOLECULAR CONVERSION OF CYCLOHEXANONE OXIME WITH THE AID OF AN ACID CATALYST FROM THE GROUP CONSISTING OF SULFURIC ACID, OLEUM AND SULPHUR TRIOXIDE, AND EXTRACTION OF THE REACTION MIXTURE AFTER DILUTION WITH WATER AND, OPTIONALLY AFTER PARTIAL NEUTRALIZATION OF THE SULPHURIC ACID, WITH A WATER-IMMISCIBLE ORGANIC SOLVENT FOR THE LACTAM, THE IMPROVEMENT COMPRISING NEUTRALIZING THE RESULTING SOLVENT OF LACTAM IN THE ORGANIC SOLVENT WITH AQUEOUS AMMONIA TO A PH OF AT LEAST 4.5 (MEASURED AT 20* C.), THEREBY FORMING AN EMULSION OF AN AQUEOUS 15-40% WT. AMMONIUM SULPHATE SOLUTION EMULSIFIED IN THE ORGANIC SOLVENT, WASHING THE EMULSION WITH A COUNTERFLOW OF DEMINERALIZED WATER IN A WEIGHT RATIO OF 4-20 PARTS THEREBY REESTRACTING THE LACTAM FROM THE ORGANIC SOLVENT TO PRODUCE AN ECAPROLACTAM SOLUTION WITH LESS THAN 5 MEQ. OF IONOGENIC SUBSTANCES PER KG. OF LACTAM, WHILE THE RESULTING AQUEOUS LACTAM SOLUTION IS EVAPORATED, OPTIONALLY AFTER HAVING BEEN FREED OF ORGANIC IONGENIC COMPOUNDS ON CATION AND ANION EXCHANGERS.
Abstract:
A method of dehydrating gases using N-alkyllactams is described. Included are steps for the recovery of any entrained vapors of the N-alkyllactams from the dehydrated gas streams and the recirculation of the recovered lactams thus reducing the operating cost of such process.