Basf Aktiengesellschaft

Klaus Kartte

Hugo Fuchs

Uwe Brand

Gerald Neubauer

Rudolph Hans Gath

Franz-Josef Weiss

Erwin Thomas

Otto-Alfred Grosskinsky

Elmar Frommer

Otto Hofstadt

Ruediger Schmitz

Werner Biffar

Ernst Deuker

Kurt Kahr

Gerard Van Wauwe

Jozef Oostvogels

Josef Beullens

Emile DeDecker

Water-immiscible solvents are removed from offgases containing same by washing with water-containing caprolactam.

Removal of water-immiscible solvents from offgases containing same

Noble metal catalyst, in particular platinum catalysts, which are applied on carriers and have become poisoned by metals as a result of being used for many years in the preparation of hydroxyl-ammonium salts by catalytic reduction of nitric oxide with hydrogen in an aqueous mineral acid are regenerated by a process in which the metallic impurities are dissolved using nitric acid or aqua regia, the solution is neutralized, the troublesome metals are precipitated from the neutralized solution by means of a selective precipitating reagent, and the purified platinum solution is reused for the preparation of the catalyst. Organic complexing agents which form insoluble or sparingly soluble complexes with the metallic impurities are preferably used as precipitating reagents.

Regeneration of inactive and poisoned platinum catalysts

A process for purifying caprolactam, which has been obtained by a Beckmann rearrangement, by extracting crude caprolactam with solvents, distilling the extract in the presence of alkali, and isolating pure caprolactam, wherein, in a first stage, caprolactam is distilled from the alkaline distillation residue at a bottom temperature of 130.degree.-160.degree. C., and is recycled to the distillation stage, the residue thus obtained is distilled, in a second stage, at a bottom temperature of 140.degree.-180.degree. C., and the distillate is treated with strongly acidic agents in a third stage and is then recycled to the extraction stage.

Purification of caprolactam

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.

Continuous extraction of caprolactam from crude lactam

A process for obtaining coarsely crystalline pure ammonium sulfate from reaction mixtures which have been obtained by Beckmann rearrangement of cyclohexanone-oxime with sulfuric acid or oleum, by neutralizing the mixtures with ammonia at an elevated temperature, with the addition of recycled ammonium sulfate mother liquor, the concentration being so chosen that during the neutralization no solid ammonium sulfate precipitates, separating the crude caprolactam from the ammonium sulfate solution, crystallizing ammonium sulfate by evaporating the ammonium sulfate solution under reduced pressure, separating off the crystallized ammonium sulfate and recycling the mother liquor to the neutralization stage. The neutralization is carried out at from 80.degree. to 115.degree. C. under autogenous pressure and the ammonium sulfate solution obtained after separating off the crude lactam is evaporated under a pressure of from 200 to 600 mm Hg while cooling to from 72.degree. to 101.degree. C.

Process for obtaining coarsely crystalline pure ammonium sulfate

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.

Processing polycaprolactam extraction liquors

A process for the partial dehydration of cyclohexanone oxime by treatment with aqueous solutions of inorganic salts, wherein the crude cyclohexanone oxime is extracted, above its melting point, with a concentrated ammonium salt solution and/or hydroxylammonium salt solution in countercurrent in an extraction column and the salt solution is then separated from the partly dehydrated cyclohexanone oxime, reconcentrated by evaporation and recycled to the oxime dehydration process. The cyclohexanone oxime melt which has been dehydrated to water contents of about 4 to 6% by weight is treated with a heated inert gas above its melting point and the off-gas is washed to remove entrained cyclohexanone oxime.

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Beindersheim, Germany

Klaus Kartte