Abstract:
Caprolactam is recovered from caprolactam distillation low boilers or high boilers or mixtures thereof by the following steps:(a) crystallizing a low or high boiler or a mixture thereof to form purified capro-lactam crystals and a mother liquor,(b) separating off the purified caprolactam crystals to leave a mother liquor,(c) recycling from 5 to 90% by weight of the mother liquor of stage (b) into stage (a) and transferring the remainder of the mother liquor into the subsequent stage (d),(d) crystallizing the remaining mother liquor portion from stage (c) to form caprolactam crystals and a mother liquor, separating off the caprolactam crystals of stage(e) (d) and recycling the same into stage (a) to leave a mother liquor,(f) recycling from 20 to 99% by weight of mother liquor of stage (e) into stage (d) and channeling out the remainder of the impurity-containing mother liquor of stage (e).
Abstract:
Hydroxylamine-O-sulfonic acid is prepared by(a) reacting hydroxylammonium sulfate with oleum at elevated temperatures,(b) isolating sulfuric acid from the hydroxylamine-O-sulfonic acid formed,(c) diluting the sulfuric acid which was obtained in stage (b) and which still contains hydroxylamino-O-sulfonic acid with water to 2-6N and heating it to 30.degree.-80.degree. C. for 1-10 hours,(d) preparing hydroxylamine by catalytic reduction of nitrogen monoxide with hydrogen using the dilute sulfuric acid from stage (c) in the presence of a noble metal catalyst at elevated temperatures.
Abstract:
Wastewaters containing hydroxylamine or its salts are worked up by a process in which the said wastewaters are passed over a strongly acidic ion exchanger, after which a 5-15% strength by weight aqueous sulfuric acid is passed over the said ion exchanger and a solution of hydroxylammonium sulfate in aqueous sulfuric acid is obtained.
Abstract:
Caprolactam is obtained by treating .epsilon.-aminocaproic acid with steam at elevated temperatures in the presence of a catalyst by a process in whcih .epsilon.-aminocaproic acid is introduced into a fluidized alumina bed and treated in the presence of steam at from 290.degree. to 400.degree. C.
Abstract:
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.
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:
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.
Abstract:
Caprolactam is purified by oxidative treatment in which mixtures which essentially contain the caprolactam to be purified and unsaturated lactams are treated with oxygen or an oxygen-containing gas mixture in an alkaline medium.
Abstract:
Caprolactam is obtained from caprolactam-containing polymers in the presence of a base under reduced pressure by depolymerizing polymers which contain the repeating unit --[--N(H)--(CH.sub.2).sub.5 --C(O)--] or mixtures consisting essentially offrom 50 to 99.99% by weight of a polymer containing the repeating unit --[--N(H)--(CH.sub.2).sub.5 --C(O)--]--from 0.01 to 50% by weight of additives selected from the group consisting of inorganic fillers, organic and inorganic pigments and dyes,from 0 to 10% by weight of organic and/or inorganic additives,from 0 to 40% by weight of non-polyamide-containing polymers andfrom 0 to 20% by weight of polyamides, with the exception of polycaprolactam and copolyamides prepared from caprolactam,in at least two depolymerization reactors connected in series.
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.