Hoechst Aktiengesellschaft

Hubert Neumaier

Hans-Jerg Kleiner

Wilhelm Vogt

Bernd Lippsmeier

Richard Schuller

Klaus Hestermann

Klaus Gehrmann

Horst Staendeke

Bernd Huber

Alexander Ohorodnik

Manfred Finke

Erich Schallus

Gunther Lenz

Gunter Peantek

Kurt Sennewald

The disclosure relates to a process for making aryldichlorophosphanes of the general formula ##STR1## in which R.sub.1, R.sub.2 and R.sub.3 being identical or different each stand for a hydrogen atom, an alkyl group having from 1 to 8 carbon atoms, a halogen atom, an aryl group of an aryloxy group by reacting an arene of the general formula ##STR2## in which R.sub.1, R.sub.2 and R.sub.3 have the meanings given above, with at least 4 mols phosphorus (III) chloride per mol arene in the presence of aluminum chloride, boiling the mixture over a period of several hours and subsequently precipitating the aluminum chloride by adding a complexing agent, filtering and distillatively working up the filtrate. More particularly, the disclosure provides for 0.05 to 0.9 mol aluminum chloride to be used per mol arene and for 1-3 mols finely ground alkali metal chloride to be used as the complexing agent per mol aluminum chloride.

Process for making aryldichlorophosphanes

Phosphonous acids are obtained by hydrolysis of dichlorophosphanes with water at temperatures of about 60.degree. to about 100.degree. C., preferably of about 80.degree. to about 95.degree. C.

Process for the preparation of phosphonous acids

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 for making halogenomethylphosphinic acid halides of the general formula:

Production of halogenomethylphosphinic acid halides

Production of dialkylphosphine oxides of the general formula: ##STR1## in which R.sup.1 and R.sup.2 each stand for an alkyl group having from 1 to 4 carbon atoms by subjecting a dialkylchlorophosphine of the general formula: ##STR2## in which R.sup.1 and R.sup.2 have the meanings given above, or an addition product thereof with hydrogen chloride, to alcoholysis with an aliphatic C.sub.1 - C.sub.4 alcohol in the presence of a protective gas at temperatures between -30.degree. and +30.degree. C, and subjecting the resulting alcoholysate to thermolysis. The compounds are more specifically produced by continuously adding the dialkylchlorophosphine component to the alcohol; subjecting the resulting alcoholysate to thermolysis in a heated separation zone; introducing into the separation zone, countercurrently to the alcoholysate, 10 to 150 l/h of a protective gas, per liter of alcoholysate; removing simultaneously from the separation zone the gaseous thermolysis products and, separately from said products, an alcoholic solutions containing desirable final product; neutralizing the alcoholic solution and recovering the final product from said solution in known manner.

Production of dialkylphosphine oxides

The invention relates to filaments and fibers the filament-forming substance of which is a copolymer of from 35 to 85 weight % of acrylonitrile, from 5 to 45 weight % of vinyl chloride, vinyl bromide and/or vinylidene chloride, from 5 to 30 weight % of carboxyphosphinic acid derivatives of the formula ##STR1## where R.sub.1 is lower alkyl having up to 8 carbon atoms, or CH.sub.2 Cl--, R.sub.2 is lower alkyl having up to 8 carbon atoms in which a hydrogen atom may be substituted by a halogen atom in case of R.sub.1 being CH.sub.2 Cl--, and R.sub.3 is hydrogen or methyl, and from 0 to 15 weight % of other unsaturated compounds having an activated double bond; the weight percentages being relative to the total amount of monomers, and a process for their manufacture. The filaments obtained are self-extinguishing and excel furthermore by their thermostability and their high degree of whiteness.

Flameproofed modacryl copolymers, fibers and filaments containing

Production of halogen-containing tertiary phosphine oxides of the general formula (I) ##STR1## in which R.sub.1 stands for an alkyl, halogenoalkyl, alkenyl, halogenoalkenyl, alkinyl or halogenoalkinyl radical, each of these radicals containing from 1 to 18 carbon atoms, or stands for a cycloalkyl, a halogenated cycloalkyl, an aryl, a halogenated aryl, an aralkyl or a halogenated aralkyl radical, and X stands for halogen. The oxides are made by subjecting a compound of the general formula (II) ##STR2## in which R has the same meaning as R.sub.1 and X stands for halogen, to thermal treatment in the presence of hydrogen halide at atmospheric or at elevated pressure so as to split off water and formaldehyde in vapor form therefrom; by continuously freeing the resulting reaction mixture from the said components in vapor form; by terminating the reaction and thereafter stripping off the hydrogen halide from the reaction mixture by introducing an inert gas thereinto; and by purifying the remaining crude product by distillation or recrystallization.

Production of halogen-containing tertiary phosphine oxides

Production of tertiary phosphine oxides of the general formula (I): ##STR1## in which the substituents R.sub.1 and R.sub.2, being identical or different, each stand for an alkyl, alkenyl, alkinyl, cycloalkyl, aralkyl or aryl radical having from 1 to 18 carbon atoms. The phosphine oxides are made by splitting off formaldehyde and hydrogen halide at temperatures within the range about 150.degree. and 350.degree. C, in the presence of hydrogen halide, from a molten compound of the general formula (II): ##STR2## in which R.sub.1 and R.sub.2 have the meanings given above and X stands for halogen; separating the formaldehyde and hydrogen split off from the reaction mixture, and treating the resulting crude product so as to separate the compound of general formula (I) therefrom.

Production of tertiary phosphine oxides

Production of alkali metal salts of amino polycarboxylic acids by reaction of a suitable carboxylic acid nitrile with aqueous alkali at elevated temperature. The salts are produced from an amino polycarboxylic acid nitrile suspension in an aqueous alkali metal hydroxide solution, which has a minimum strength of substantially 30 % by weight and contains at least stoichiometric proportions of alkali metal hydroxide; the suspension is introduced into a reactor heated to a temperature between 60.degree. and 150.degree. C, and salt formation is effected by thorough agitation.

Process for the manufacture of alkali metal salts of amino

Production of nitrilotriacetonitrile by reacting a salt of ammonia and a non-oxidizing acids with formaldehyde and hydrogen cyanide in an aqueous acid phase, at elevated temperature, completing the reaction and separating the reaction mixture into firstly crystalline nitrilotriacetonitrile and secondly an aqueous acid phase as the mother liquor. More particularly, a product obtained by primary reaction of an aqueous ammonium salt solution with an aqueous formaldehyde solution, the ammonium salt and formaldehyde being used in a ratio larger than 1:6, is reacted with a stoichiometric proportion of an aqueous hydrogen cyanide solution, the said stoichiometric proportion being based on the formaldehyde concentration of the primary reaction product.

Process for the manufacture of nitrilotriacetonitrile

Production of halogen-containing tertiary phosphine oxides of the general formula I ##EQU1## in which the substituents R.sub.1, R.sub.2 and R.sub.3, being identical or different, stand for an alkyl, alkenyl, aryl or aralkyl radical, at least one of those radicals containing at least one aliphatically combined halogen atom. The compounds are made by reacting one or more compounds of the general formula II ##EQU2## in which R.sub.4, R.sub.5 and R.sub.6, being identical or different, stand for an alkyl, alkenyl, aryl or aralkyl radical, at least one of those R.sub.4, R.sub.5 and R.sub.6 radicals containing an aliphatically combined hydroxyl group, with at least equivalent proportions, based on the number of hydroxyl groups, of gaseous hydrogen halide with agitation, if desired, at temperatures within the range about 100.degree. and 300.degree.C; freeing the reaction mixture, during the reaction or after termination thereof, from water originating from the reaction; and separating from the resulting reaction mixture the halogen-containing tertiary phosphine oxide by distillation or crystallization.

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Hubert Neumaier