Bayer Aktiengesellschaft

Bayer Materialscience Ag

Bernd Thelen

Karl-Werner Thiem

Wolfgang Auge

Rutger Neeff

Hans-Samuel Bien

Reinold Schmitz

Hans-Walter Brandt

Hans-Peter Schal

Bernd Schroeder

Ulrich Wolf

Norbert Majer

A mixture of isomeric diisocyanatodiphenylmethanes composed of at least 2,2'-diisocyanato-diphenylmethane, 2,4&#x2032;-diisocyanatodiphenylmethane and 4,4&#x2032;-diisocyanatodiphenyl-methane is distilled in at least one stage and a divided-wall column is used in at least one distillation stage.

Process for the distillation of a mixture of isomeric diisocyanatodiphenylmethanes

Process for working up aqueous nitric acid which is of a concentration above the azeotropic concentration and contains organic compounds in solution for suspension wherein said nitric acid of a concentration about the azeotropic concentration is distilled off in one or more rectification steps until the azeotropic nitric acid is obtained. In the process, certain specified ratios of nitric acid and water to organic constituents must be maintained.

Process for working up nitric acid

A process has been developed for isolating aromatic dinitro compounds by using nitric acid in specified concentrations in different portions of a rectifying column and separating off the mixture of aromatic dinitro compounds from the sump of the rectifying column.

Process for isolating aromatic dinitro compounds

A process for concentrating at least one of (a) individual halogenoanthraquinones (b) binary mixtures of di-halogenoanthraquinones and (c) binary mixtures of trihalogenoanthraquinones, from a mixture containing at least two halogenoanthraquinones, comprising subjecting said mixture containing at least two halogenoanthraquinones to fractional vacuum distillation in a heated rectification column having an efficiency corresponding to about 20 to 50 theoretical stages with an absolute pressure at the top of about 0.5 to 50 mm Hg and a reflux to take-off ratio of about 5/1 to 50/1. Advantageously, distillation is carried out continuously in a cascade of columns, the products withdrawn from the top of the first column being 2-chloroanthraquinone in the first stage, 1-chloroanthraquinone in the second stage, 1,6- and 1,7-dichloroanthraquinone in the third stage and 1,5- and 1,8-dichloroanthraquinone in the fourth stage, 1,4,5- and 1,4,6-trichloroanthraquinone being obtained in the sump of the 4th stage and being separated therefrom by film evaporation. The mixture of halogenoanthraquinones is advantageously a mixture of chloroanthraquinones such as is obtained by the action of chlorine, chloric acid or a chlorate on various industrial mixtures of nitro- or sulfo-anthraquinones.

Process for concentrating halogenoanthraquinones

The purification of high-melting organic products, such an anthraquinone and substituted anthraquinones, which is substantially free from lower-boiling impurities, by melting the product to be purified by heating, while mechanically conveying the same along a path with a screw conveyer, as for example, in a melting screw; degassing the melt at a reduced pressure in a column, as for example, at a pressure of 50 to 400 mm Hg; passing the degassed melt through a thin film evaporator at a reduced pressure of, for example, 5 to 250 mm Hg to evaporate the high-melting organic product and discharging the remaining high-boiling impurities and such impurities which are not capable of being distilled from the evaporator through a conically tapering sump, while mechanically scraping residue from the sump wall, preferably with the use of a rotating helical screw in the sump; the discharge from the sump being effected into and through an enclosed path at a rate sufficient to prevent liquid accumulating in the sump, while maintaining the central portion of the enclosed discharge path at a lower temperature than its end portion to form a crystal sludge in the central portion, which acts as a pressure seal; and solidifying and recovering the product discharging from the enclosed path. The enclosed path is preferably established through a screw-type pump which feeds into a crystallizing screw where the solidification takes place, the crystallizing screw being preferably maintained above the screw-type pump and is maintained filled with an amount of sump product which approximately corresponds to the amount of product in the sump take-off screw. The vapors produced in the thin film evaporator are passed via a heated rectifying column into a condenser, and a portion of the condensate is passed to the column as a reflux and another portion taken off and solidified in a crystallizing screw.

Process for the purification of high-melting organic products

Aromatic mononitro compounds are prepared by nitrating aromatic compounds with nitric acid having a concentration between 70 and 100% by weight, working up of the nitration mixture in a rectification column and separation of the aromatic mononitro compound. In the nitration mixture and in the rectification column, depending upon the concentration of the nitric acid present, the ratio by weight of nitric acid plus water is controlled and not lowered below defined figures. Optionally water or nitric acid is introduced into the rectification column.

Process for the production of aromatic mononitro compounds

Process for the manufacture of pure 1-nitroanthraquinone, characterised in that a nitroanthraquinone mixture obtained by nitration of anthraquinone in the presence of inorganic acids and, optionally, lowering the molar fraction of the acids in the reaction mixture after isolation of the reaction products which have precipitated and, optionally, further measures, is subjected to a rectification.

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Leverkusen, Germany

Bernd Thelen