Hoechst Aktiengesellschaft

Hilmar Roszinski

Bernd Lippsmeier

Reinhard Gradl

Hans-Werner Stephan

Werner Pieper

Heinz Harnisch

Gerhard Hartlapp

Wilhelm Giechau

Wilhelm P Doppelfeld

An apparatus is provided for fumigating waste waters in a fumigation tank with fumigation enclosures (gas manifolds which are situated in parallel next to one another and at a distance from one another and rest horizontally, in whose upper sides gas outlet openings are situated and whose undersides are open, wherein mobile rotation bodies rotated by gas flow are situated for cleaning purposes in the gas outlet openings 13 of the fumigation enclosures 14 and the gas outlet openings 13 each have, in a known manner, a central countersunk section 12 enclosing an angle .alpha. of, for example, 90 to 180.degree. underneath and the remaining wall thickness 15 of the gas outlet opening 13 of each countersunk section 12 amounts to 0.5 to 2 mm. The rotation body according to the invention may comprise a top section 1 and a base section 3 which are joined to a neck section 2.

Apparatus for fumigating waste waters

The disclosure relates to a process for purifying crude, concentrated wet-processed phosphoric acid. To this end, the disclosure provides:

Process for purifying wet-processed phosphoric acid

Production of O,O-dialkylthionophosphoric acid chlorides of the general formula: ##STR1## in which R is an alkyl radical having from 1 to 6 carbon atoms, by reacting a dialkyldithiophosphoric with chlorine. A reactor is supplied with O,O-dialkyldithiophosphoric acid and chlorine is added thereto at a temperature lower than about 75.degree. C.; following completion of the chlorine addition, the reactor is supplied with a further portion of O,O-dialkyldithiophosphoric acid at a temperature between 0.degree. and 75.degree. C., and the resulting reaction mixture is distilled to isolate O,O-dialkylthionophosphoric acid chloride therefrom.

Process for the purification of O,O-dialkylthionophosphoric acid

O,O-dialkylthionophosphoric acid chlorides are produced by chlorinating a dialkyldithiophosphoric acid in two stages. In the first stage, the acid is reacted with chlorine in a molar ratio of 1:1.15 to 1:1.50, resulting sulfur is separated, the liquid phase is admixed with a distilled product of a previous batch chlorinated in the second stage and with a further 0.25 to 0.7 mol of O,O-dialkyldithiophosphoric acid per mol of acid initially used, and desirable final product is distillatively separated from said mixture. In the second stage, the distillation residue of the first stage is reacted with a total proportion of 0.9 to 1.0 mol of chlorine per mole of acid initially used, precipitated sulfur is separated from the second stage chlorination product, the liquid phase is distilled off, and resulting distillate is recycled to the first chlorination stage.

Production of O,O-dialkylthionophosphoric acid chlorides

Production of pure dithiophosphoric acid O,O-diesters of the general formula ##STR1## in which the radicals R.sub.1 and R.sub.2, being identical or different, each stand for linear and/or branched alkyl, cycloalkyl, alkenyl, alkinyl, aralkyl or aryl radicals having from 1 to 18 carbon atoms, from their salts of the general formula: ##STR2## in which R.sub.1 and R.sub.2, respectively, have the meanings given hereinabove, M stands for a metal or ammonium cation, and n stands for the valency of the particular cation. The compounds are made by dissolving the salts in the quantity of one or more strong acids necessary to ensure reaction with the resultant formation of two separate liquid phases, and separating the two phases from one another.

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Erftstadt, Germany

Hilmar Roszinski