Abstract:
Process the recovering caprolactam from the residue remaining following the distillation, under reduced pressure, of impure caprolactam obtained by rearrangement of cyclohexanone oxime with sulphuric acid or oleum, by distilling the residue under reduced pressure whereby a caprolactam-containing distillate is obtained; hydrogenating the caprolactam containing distillate in an aqueous medium to obtain a hydrogenation product; and recovering caprolactam from the resulting hydrogenation product.
Abstract:
A process for rapidly cooling gases which contain caprolactam vapor and which have been obtained by catalytic rearrangement of cyclohexanone-oxime in the gas phase in the presence of a supported catalyst containing boric acid, wherein a finely divided coolant at from 90.degree. to 200.degree. C. is fed into a cooling zone from above, gases which are at 330.degree.-400.degree. C. and contain caprolactam vapor are introduced radially at high speed through nozzle orifices over the downstream portion of the cooling zone, and are cooled to 100.degree.-200.degree. C. by thorough mixing with the finely divided coolant, and the cooled mixture is discharged.
Abstract:
Treatment of process waste waters to be discharged from a lactam manufacturing plant by stepwise concentration in two steps under suitable conditions, extraction of lactam from the concentrate with an organic solvent, oxidative combustion of the extract residue and conversion of sulfur dioxide formed into sulfuric acid can save losses of lactams, organic solvents and sulfur containing compounds to a considerable extent and render the waste waters no longer harmful.
Abstract:
In a process for manufacturing a lactam which includes rearranging a cycloalkanone-oxime with sulfuric acid to form the lactam, neutralizing the rearrangement mixture with ammonia to form ammonium sulfate, and separating the lactam and the ammonium sulfate, the improvement which comprises:A. heating at least a portion of the ammonium sulfate to a temperature of 240.degree. - 460.degree. C to form ammonia and ammonium bisulfate;B. separating the ammonia from the ammonium bisulfate;C. recycling the ammonia to neutralize the rearrangement mixture;D. burning the ammonium bisulfate at a temperature of 850.degree. - 1250.degree. C to form an SO.sub.2 -containing gas;E. oxidizing the SO.sub.2 -containing gas to form sulfuric acid; andF. recycling the sulfuric acid to the rearrangement stage.
Abstract:
In a process for the preparation of lactam from cycloalkanone comprising reacting said alkanone with hydroxylamine sulfate to form the corresponding cycloalkanone oxime followed by Beckman rearrangement to yield said lactam and neutralization of the sulfuric acid formed by ammonia whereby ammonium sulfate is formed as a byproduct, the improvement which comprises reacting said ammonium sulfate with an alkaline-earth metal oxide or hydroxide to form an alkaline earth metal sulfate and ammonia, heating said alkaline-earth metal sulfate to decompose it into said alkaline-earth metal oxide and sulfur dioxide and/or sulfur trioxide, converting said sulfur dioxide and/or sulfur trioxide into sulfuric acid, whereby said sulfuric acid and said ammonia are capable of reuse in said process.
Abstract:
A PROCESS FOR REARRANGING CYCLODODECANONEOXIME INTO PURE CYCLODODECALACTAME, CHARACTERIZED BY THE FACT THAT THE OXIME, CONVERTED INTO OXIME CHLORHYDRATE, IS MADE INTO A SOLUTION WITH A SELECTIVE SOLVENT, IN THE PRESENCE OF A SMALL QUANTITY OF CATALYST, CHOSEN FROM THE GROUP OF ACID HALIDES AND OXYHALIDES, AND THEN HEATED TO A TEMPERATURE OF BETWEEN 65 AND 110* C. FOR ONE TO TWO HOURS, THE RESULTING HYDROCHLORIC ACID IS DRAWN OFF BY MEANS OF A FLOW OF GAS WHILE MAINTAINING THE REFLUX TEMPERATURE OF THE SOLVENT, THE REACTION MIXTURE IS WASHED WHILE HOT WITH AN ALKALINE AQUEOUS SOLUTION, THE ORGANIC PHASE CONTAINING THE LACTAME IS WASHED IN HOT WATER UNTIL BECOMES NEUTRAL, AND THE LACTAME IS RECOVERED BY CRYSTALLIZATION OR DISTILLATION OF THE SOLVENT. THE QUANTITY OF CATALYST USED RANGES FROM 0.5 TO 5%, AND PREFERABLY 1 TO 2%, OF THE WEIGHT OF OXIME. THE SOLVENT IS PREFERABLY SELECTED FROM ALKANES, CYCLOALKANES, SUBSTITUTED ALKANE AND CYCLOALKANE DERIVATIVES, AND HALOGENATED ALKANE AND CYCLOALKANE DERIVATIVES.
Abstract:
BORON TRIOXIDE SUPPORTED ON THORIA HAVING A SURFACE AREA OF AT LEAST ABOUT 100 SQUARE METERS PER GRAM PROVIDES A CATALYST PARTICULARLY USEFUL INTHE VAPOR PHASE, CATALYTIC REARRANGEMENT OF CYCLIC KETOXIMES TO THE CORRESPONDING LACTAMS; FOR EXAMPLE, IN THE VAPOR PHASE PROCESS FOR THE REARRANGEMENT OF CYCLOTHEXANONE OXIME TO CAPROLACTAM.