Abstract:
In a process for obtaining caprolactam by cleaving caprolactam oligomers by passing them through an alumina catalyst bed at an elevated temperature, the improvement that the oligomers are introduced, as liquid or solid, into a fluidized bed of alumina and are cleaved at from 290.degree. to 400.degree. C. in the presence of steam.
Abstract:
In a process for the preparation of .epsilon.-caprolactam by catalytic rearrangement of cyclohexanone-oxime in the gas phase at from 230.degree. to 450.degree. C. over a supported catalyst, containing boron trioxide, in a fluidized bed, wherein the catalyst is removed from the fluidized bed at the rate at which it becomes spent and is treated, in a fluidized state, with gases containing molecular oxygen at from 600.degree. to 900.degree. C., after which boron trioxide or boric acid is added to the fluidized catalyst, at from 300.degree. to 900.degree. C., before the catalyst is returned to the fluidized bed, the improvement that boron trioxide or boric acid of particle size from 0.05 to 1.5 mm is fed to the fluidized catalyst at one or more points.
Abstract:
In a process for the continuous extraction of caprolactam from crude lactam by means of benzene in counter-current, in which crude lactam is fed into the upper part of an extraction zone and benzene into the lower part, a solution of caprolactam in benzene is taken off at the top and an aqueous solution containing impurities is taken off at the bottom, the improvement that water is additionally fed into the upper part of the extraction zone and a part of the aqueous solution, containing impurities, obtained at the bottom of the extraction zone is recycled into the extraction zone. Caprolactam is used for the manufacture of nylon.
Abstract:
An improved process for the manufacture of cyclohexanone oxime by reacting cyclohexanone with an aqueous hydroxylammonium-ammonium sulfate solution at temperatures above the melting point of cyclohexanone oxime by the countercurrent process, the improvement consisting in that the reaction is carried out in the absence of solvents and neutralizing and/or buffer salts at pHs of up to 0.5 until equilibrium is reached, the oximes resulting during the reaction being separated from the aqueous phase and the aqueous phase being extracted with cyclohexanone and then subjected to steam distillation.
Abstract:
A process for processing polycaprolactam extraction liquors by evaporation of water and distillation of the residue in which the evaporation of water is carried out in a plurality of stages and the evaporation energy for the removal of the bulk of the water is taken from the heat liberated in the rearrangement of cyclohexanone oxime to caprolactam in oleum or sulfuric acid by using the extraction water for cooling the rearrangement mixture and utilizing the heat absorbed by the extraction water for the concentration of this extraction water by evaporation of water.
Abstract:
A hydrogenation catalyst, obtainable by carrying out essentially the following steps:(a) treatment of a platinum metal salt with finely divided sulfur followed by(b) reduction of the platinum metal salt to metallic platinum metal.
Abstract:
Caprolactam is purified continuously by passing a 75-95% strength by weight aqueous caprolactam solution together with hydrogen at 50.degree.-95.degree. C. and 1.5-100 bar upward through a fixed-bed supported palladium or nickel catalyst in a tubular zone while maintaining a residence time of from 10 to 100 min.
Abstract:
Distillation residues from the purification of caprolactam are worked up by heating in the presence of sodium hydroxide or potassium hydroxide and in the presence of a high-boiling hydrocarbon at from 250.degree. to 500.degree. C. and continuously removing the caprolactam.
Abstract:
Reaction mixtures obtained by Beckmann rearrangement of cyclohexanone oxime with sulfuric acid or oleum are neutralized by a process which comprises the following steps:(a) mixing the reaction mixture with recycled ammonium sulfate mother liquor whose concentration is chosen so that no solid ammonium sulfate is precipitated during the neutralization,(b) neutralization by feeding gaseous ammonia which contains water or an aqueous ammonium sulfate solution in finely divided liquid form through a plurality of nozzle orifices into the solution of the reaction mixture in the ammonium sulfate mother liquor at elevated temperatures,(c) separation of crude lactam from the aqueous ammonium sulfate solution,(d) evaporation of the ammonium sulfate solution under reduced pressure and with separation of the crystalline ammonium sulfate from the ammonium sulfate mother liquor and(e) recycling of the ammonium sulfate mother liquor to stage a).