Hoechst Aktiengesellschaft

Alexander Ohorodnik

Klaus Gehrmann

Stefan Schafer

Eberhard Auer

Elmar Lohmar

Paul Stutzke

Hermann Vierling

Albert Mainski

Johannes Rosenthal

Karl Kaiser

Wernfried Riechmann

Karl-Heinz Steil

Hubert Neumaier

Udo Dettmeier

Ulrich Bollert

Gunter Legutke

Horst Semmler

Robert Willms

Rudolf Wesselmann

Joachim Hardel

Hans W Keuper

Heinz-Josef Berns

Friedhelm Bylsma

The disclosure relates to a process for the continuous production of 2-carboxyethyl-alkyl-phosphinic acid dialkylesters by reacting an alkanephosphonous acid monoalkylester with an acrylic acid ester in the presence of a metal alcoholate. To this end, the disclosure provides:

Process for the continuous production of 2-carboxyethyl-alkyl-phosphinic

The disclosure relates to an improved process for making alkanephosphonous acid esters which comprises: introducing a stoichiometric excess each of an alkyldihalogenophosphane and aliphatic alcohol into a reaction column and reacting them therein at a temperature higher than the boiling point of the reactants but lower than the boiling point of the resulting alkanephosphonous acid ester, this latter being obtained in the base portion of the reaction column and being removed therefrom; continuously expelling overhead of the reaction column a vaporous mixture consisting of by-products formed during the reaction, in the form of hydrogen halide and halide of the aliphatic alcohol, together with aliphatic alcohol in excess, and separating the mixture into its components in a series-connected distilling column, the aliphatic alcohol obtained in the base portion of the distilling column being removed therefrom and recycled into the reaction column, and selectively condensing the mixture issuing overhead with recovery of hydrogen halide gas and liquefied halide of the aliphatic alcohol.

Process for making alkanephosphonous acid esters

The disclosure relates to a process for making methyldichlorophosphane by reacting methane with phosphorus trichloride in the presence of 2 to 7 mol % carbon tetrachloride, based on the phosphorus trichloride used, at temperatures of 500.degree. to 650.degree. C. and over a period of time of 0.1 to 0.9 second. More particularly, the reaction is effected under a pressure of 2 to 10 bars, the proportion of carbon tetrachloride added being reduced at increasing pressure.

Process for making methyldichlorophosphane

The disclosure relates to a process for making fine particulate, non-agglomerating chloropolyethylene by subjecting pulverulent polyethylene to a chlorination reaction in aqueous or aqueous/hydrochloric acid-suspension with chlorine gas at a temperature of about 20.degree. to 140.degree. C. in the presence of silicic acid and silicon oil, separating, washing and drying the chloropolyethylene. More particularly, the disclosure provides for the chlorination to be terminated and for the aqueous hydrochloric acid-suspension of chloropolyethylene to be then intensively mixed with an aqueous or aqueous/hydrochloric acid-dispersion having talc as well as an orthophosphoric acid mono- and/or diester or a polysiloxane by means of an emulsifier dispersed in it, and for the chloropolyethylene to be separated from the mixture, to be washed and dried.

Process for making fine particulate non-agglomerating chloropolyethylene

Polyolefins which are made by subjecting .alpha.-olefins to catalytic polymerization are freed from residual liquid hydrocarbons by means of steam and water. To this end, the invention provides:

Continuous removal of residual hydrocarbons from polyolefins

The invention relates to a process for making 2-chloroformylethylmethylphosphinic acid chlorides of the general formula: ##STR1## in which R.sup.1 and R.sup.2 each stand for hydrogen or CH.sub.3. To this end, methyldichlorophosphane is reacted with acrylic acid, methacrylic acid or crotonic acid at elevated temperature. More particularly, a solution of methyldichlorophosphane in phosphorus trichloride, the solution originating from a reaction of phosphorus trichloride with methane at temperature higher than 500.degree. C., is used. The reaction is effected at temperatures ithin the range 50.degree. to 90.degree. C. in the presence of hydrogen chloride; and the phosphorus trichloride is distilled off.

Production of 2-chloroformylethylmethylphosphinic acid chlorides

The invention relates to a process permitting the deposition of solid matter in mixtures containing methyldichlorophosphane to be avoided. To this end, the mixture is stabilized by admixing it with phosphoric acid or a soluble compound containing at least one acid group selected from phosphoric acid, phosphonic acid, sulfonic acid, phosphonous acid, thiophosphoric acid or dithiophosphoric acid.

Process permitting the deposition of solid matter in mixtures containing

Pure acetyl chloride containing less than 1 ppm of phosphorus is produced. To this end, crude acetyl chloride containing phosphorus compounds is intimately contacted with 1 to 20 liters of gaseous chlorine per liter of liquid crude acetyl chloride and the acetyl chloride so contacted with chlorine is subjected to fractional distillation.

Production of pure acetyl chloride

Abrasion-resistant active carbon carriers or catalysts are made. To this end, an abrasion-resistant carrier is impregnated with an aqueous solution of a saccharide, the impregnated carrier is dried and the saccharide is thermally decomposed in the absence of air to active carbon which tenaciously adheres to the carrier.

Production of space abrasion-resistant active carbon carriers or

[2-(HALOGENOFORMYL)-VINYL]-ORGANYL-PHOSPHINIC ACID HALIDES OF THE GENERAL FORMULA ##STR1## in which R.sub.1 stands for an alkyl group having 1 to 8 carbon atoms, an aryl group or a substituted derivative of these groups, R.sub.2 stands for a hydrogen atom, an alkyl group having 1 to 8 carbon atoms, an aryl group or a substituted derivative of these groups, and X stands for a chlorine or bromine atom, are produced. To this end, a 2 halogenoacrylic acid or a substitution product thereof of the general formula ##STR2## in which R.sub.2 and X have the meanings given above, is reacted at 15.degree.-90.degree. C. with an organyldihalogenophosphane of the general formula

Production of [2-(halogenoformyl)-vinyl]-organyl phosphinic acid halides

Monomeric matter is removed from an aqueous dispersion of a polymer containing at least 50 weight % of polymerized vinyl chloride. To this end, the dispersion is introduced into the upper portion of a column provided with sieve plates and contacted therein for 10 seconds up to 20 minutes, under 600 up to 1200 mm Hg, with hot steam at 100.degree. up to 150.degree. C. flowing countercurrently with respect to the dispersion. The polymer dispersion so treated is removed from the column base portion; and a vaporous matter mixture issuing at the head of the column is condensed stagewise so as to recover an aqueous phase and the monomeric matter.

Process for continuously removing monomers from an aqueous dispersion of

Methyl-[2-(2,4,6-tribromophenylcarbamoyl-)ethyl-]phosphinic acid is made continuously. To this end, molten 2-methyl-2,5-dioxo-1-oxa-2-phospholane is reacted with molten 2,4,6-tribromoaniline at 210.degree. to 250.degree. C. in the absence of a solvent.

Production of

Production of N-substituted 2-carbamoyl phosphinic acids of the general formula: ##STR1## in which R.sup.1 stands for an alkyl group having 1 to 4 carbon atoms or an aryl group; R.sup.2 and R.sup.3 stand independently of each other for an alkyl group having 1 to 4 carbon atoms, an aryl group or a hydrogen atom; R.sup.4 stands for an alkyl group having 1 to 18 carbon atoms, an aryl group or a hydrogen atom; and R.sup.5 stands for an alkyl group having 1 to 18 carbon atoms or an aryl group. More specifically, a 2-chloroformyl phosphinic acid chloride of the general formula ##STR2## is reacted at 120.degree. to 170.degree. C with an amine of the general formula ##STR3## and resulting N-substituted 2-carbamoyl phosphinic acid chloride of the general formula ##STR4## the latter compound being obtained while hydrogen chloride is split off, is hydrolyzed with water.

Production of N-substituted 2-carbamoyl phosphinic acids

Production of methyldichlorophosphane. The compound is made by reacting methane and phosphorus trichloride in a reaction zone in which a temperature higher than 500.degree. C is maintained. More specifically, hot reaction gas coming from the reaction zone is mechanically freed from solid matter, and the reaction gas freed from solid matter is passed to a quenching zone in which it is quenched with liquefied reaction mixture having 0.3 to 5 weight % of an organic barium compound or a non-ionic surfactant dissolved therein.

Production of methyldichlorophosphane

Pure methyldichlorophosphane is recovered from a mixture containing phosphorus trichloride and methyldichlorophosphane as its principal constituents by distillation in two stages. Phosphorus trichloride and other low-boiling material are distilled off overhead in the first stage and methyldichlorophosphane is distilled off from high-boiling material in the second stage, the latter being fed with base product coming from the first stage. More specifically, there is dissolved in the said mixture, prior to admitting it to the first distillation stage, 0.01 to 1 weight % of an organic barium compound or 0.1 to 10 weight % of a non-ionic surfactant, and the base product coming from the first distillation stage is admixed, prior to admitting it to the second distillation stage, with 1 to 10 weight % of phosphorus oxychloride.

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Erftstadt, Germany

Alexander Ohorodnik