Abstract:
In a process for manufacturing a lactam which includes rearranging a cycloalkanone-oxime with sulfuric acid to form said lactam, neutralizing the rearrangement mixture with ammonia to form ammonium sulfate, and separating said lactam and said ammonium sulfate, the improvement which comprises:A. forming the ammonium sulfate into finely divided particles;B. burning the particles at a temperature of 850.degree. - 1250.degree. C. to form an SO.sub.2 -containing gas;C. oxidizing the SO.sub.2 -containing gas to form sulfuric acid; andD. recycling at least a portion of the sulfuric acid to the cycloalkanone-oxime rearrangement step.No external source of sulfuric acid is required. A portion of the SO.sub.2 -containing gas can be used for the manufacture of hydroxylamine sulfate, in which case no external source of SO.sub.2 need be required.
Abstract:
In commercial processes for producing epsilon-caprolactam, the caprolactam product is in admixture with sulfuric acid. An improved process for removing sulfuric acid from the caprolactam results from treating the admixture with ammonia at superatmospheric pressure.
Abstract:
A process for preparing pure N-alkyl-lactams obtained by the reaction, in an organic solvent medium of, the corresponding lactamate of an alkali metal and an alkyl halide. This process consists of treating a reactive mixture of N-alkyl-lactam containing the corresponding cyclo-alkylene imine as an impurity with a current of carbon dioxide, until the cyclo-alkylene imine precipitates completely in the form of an insoluble carbonate, and then separating it from the precipitate.
Abstract:
A process for purifying a polymerisable monomer selected from the group consisting of cyclic ethers, hydrocarbon olefins, vinyl compounds, aldehydes, lactams of the formula: ##EQU1## wherein x is an integer from 3 to 13 and lactones of the formula: ##EQU2## wherein n is an integer of from 1 to 4 and wherein R represents an hydrogen atom, an alkyl group or an aryl group; said process comprising contacting a liquid consisting of said monomer at a temperature of not greater than 130.degree. centigrade and at a pressure sufficient to keep said monomer in liquid form, with a solid absorbent consisting essentially of a porous reticulated macromolecular alkali metal or alkaline earth metal salt of a cationic exchange resin containing carboxylic, sulfonic or phosphoric acid groups, said cationic exchange resin having a specific surface area of at least one square meter per gram and a pore diameter of from 10.sup.1.3 to 10.sup.5 angstroms and recovering the purified monomer.
Abstract:
The invention relates to a process for the purification of caprolactam which is obtained by rearrangement of cyclohexanone oxime in the gas phase in the presence of solid catalysts. The purification takes place by dissolving the crude lactam in benzene or in alkyl benzene with seven to eight carbon atoms and recrystallization whilst cooling.
Abstract:
A process for the recovery of lactams from a Beckmann rearrangement mixture of lactams and sulphuric acid or sulphur trioxide, with the production of a phosphate-containing fertilizer is disclosed. The Beckmann rearrangement mixture is partially neutralized by the addition of ammonium or alkali metal hydroxide, sulphate or carbonate in an amount such that the molar ratio between the sulphate formed and the sum of the sulphate formed and the free sulphuric acid is at least 1/8:1. Thereafter, the resulting partially neutralized solution is extracted by a substantially water-immiscible, organic lactam solvent to separate lactam from the remainder of said mixture, and the remainder of said mixture after such extraction is used for the decomposition of rock phosphate with formation of gypsum and of a free phosphoric acid-containing solution. This latter solution, after removal of gypsum and neutralization of the solution with ammonia or alkali liquor is converted into a dihydrogen phosphate-containing solution from which dihydrogen phosphate, suitable for use in fertilizers, is recovered after evaporative concentration. The process provides for the ready separation of lactams from a Beckmann rearrangement reaction mixture, while at the same time producing, as a by-product, dihydrogen phosphate or a valuable dihydrogen phosphate containing fertilizer.
Abstract:
A PROCESS FOR RECOVERING E-CAPROLATAM FRO SOLUTIONS OF E-CAPROLACTAM AND SULPHURIC ACID AND SO3 IS DISCLOSED WHEREIN AMMONIUM DIHYDROGEN PHOSPHATE OR ALKALI METAL DIHYDROGEN PHOSPHATE IS ADDED TO THE LACTAM, SULPHURIC ACID SOLUTION AND THE SOLUTION THEN SUBJECTED TO EXTRACTION BY A SUBSTANTIALLY WATER IMMISCIBLE SOLVENT FOR THE LACTAM WHEREBY THE LACTAM IS EXTRACTED FROM THE SULPHURIC ACID SOLUTION AND THE LACTAM FREE SULPHURIC ACID SOLUTION CAN BE USED TO PROCESS ROCK PHOSPHATE TO GYPSUM AND PHOSPHORIC ACID AND THE PHOSPHORIC ACID BEING CONVERTED TO AMMONIUM OR ALKALI METAL DIHYDROGEN PHOSPHATE TO BE USED IN TREATING FURTHER SOLUTIONS OF LACTAM AND SULPHURIC ACID.
Abstract:
BY EXTRACTING A LACTAM-CONTAINING REACTION MIXTURE OBTAINED FROM THE BECKMANN REARRANGEMENT REACTION OF A CYCLIC KETOXIME IN THE PRESENCE OF WATER WITH LIQUID SULFUR DIOXIDE, THE LACTAM CAN BE EFFECTIVELY SEPARATED IN THE PURE STATE.