Abstract:
A process for the continuous preparation of an oxime from cyclohexanone and an aqueous buffered solution of a hydroxylammonium salt together with free phosphoric acid, phosphates, nitrates, and optionally sulphates all in controlled amounts and without the use of an organic solvent is disclosed. The resulting aqueous reaction mixture contains a manageable amount of unreacted cyclohexanone which is subsequently recovered and recirculated.
Abstract:
Epsilon -CAPROLACTAM IS RECOVERED FROM A Beckmann rearrangement mixture of the lactam and aqueous sulfuric acid by simultaneously neutralizing the rearrangement mixture with ammonia at a pressure of 1-5 atmospheres and crystallizing out ammonium sulfate, the heat liberated by the neutralization reaction is removed from the system by evaporating a portion of the water from the solution. At the conditions employed hydrolysis of the lactam is substantially reduced if not entirely avoided.
Abstract:
epsilon -CAPROLACTAM IS RECOVERED FROM A Beckmann rearrangement mixture of the lactam and aqueous sulfuric acid by simultaneously neutralizing the rearrangement mixture with ammonia at a pressure of 1-5 atmospheres and crystallizing out ammonium sulfate, the heat liberated by the neutralization reaction is removed from the system by evaporating a portion of the water from the solution. At the conditions employed hydrolysis of the lactam is substantially reduced if not entirely avoided.
Abstract:
An aqueous solution containing both phosphoric and nitric acids is extracted with a poorly water-miscible aliphatic ketone or ether having from 4 to 13 carbon atoms, the concentration of the starting solution and the weight ratio of the starting solution to the extracting agent being selected so that at least 90% of the nitric acid but not more than 10% of the phosphoric acid passes into the organic phase. The starting solution preferably contains at least 40%, but not more than 75%, by weight of water. When the starting solution contains from 40% to 70% by weight of water, the weight ratio between the acid solution and the ketone or ether preferably is kept at from 1: 1 to 1: 3, a higher proportion of extracting agent being favoured for more dilute solutions. The extraction either may be performed batchwise in one or a plurality of stages or may be carried out continuously with countercurrent flow of extracting agent and acid solution. The ketone or ether may be diethyl ether, diisopropyl ether, dibutyl ether, diisoamyl ether, methyl-isobutyl ketone, methyl-isoamyl ketone, butyl-ethyl ketone, diisobutyl ketone or dibutyl carbitol; the preferred extracting agent is methyl-isobutyl ketone. The above separation process may be applied in the recovery of phosphoric acid from the liquor resulting from the decomposition of phosphate rock by concentrated nitric acid. Such a procedure, an example of which is fully described and illustrated in the Specification, may entail preparing an aqueous solution of phosphoric and nitric acids by decomposing phosphate rock with nitric acid having a concentration of at least 45% by weight acid, lowering the molar calcium oxide/phosphorus pentoxide ratio of the solution to below 1.5 by cooling to remove calcium nitrate, subjecting the solution to an extraction with a butyl or amyl alcohol, freeing the resulting acids-containing organic extract from residual calcium nitrate by washing with a solution containing phosphoric acid and possibly nitric acid and having a concentration of at least 25% by weight total acid(s), washing the acid-washed organic extract with water in an amount such that not more than three quarters of the total acids present passes from the organic extract to the water, and separating the phosphoric acid from the nitric acid in the resulting aqueous acid solution by the extraction process described previously.