Hoechst Aktiengesellschaft

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Hoechst Aktiengesellschaft Knapsack

Werner Klose

Franz-Josef Dany

Horst Staendeke

Joachim Kandler

Gero Heymer

Werner Krause

Gunther R Schimmel

Norbert Weferling

Jurgen Grosse

Georg Elsner

Hannsjorg Ulrich

Christian May

Theodor Auel

Lothar Westermann

Helmut Klemp

The present invention relates to 1-hydroxy-.omega.-(alkyl- or arylphosphinico)alkane-1,1-diphosphonic acids of the general formula I ##STR1## and to the salts of these acids of the general formula II ##STR2## where, in these formulae, R.sup.1 denotes an alkyl radical having 1 to 6 carbon atoms, a cycloalkyl radical having 5 to 7 carbon atoms or an aryl radical having 6 to 10 carbon atoms, R.sup.2 denotes a straight-chain or branched alkylene radical having 1 to 6 carbon atoms and A denotes a monovalent equivalent of a cation of an inorganic or organic base. In addition, processes are described for the preparation of these novel compounds.

1-Hydroxy-omega-(alkyl- or arylphosphinico)alkane-1,1-diphosphonic

Dimensionally stable alkaline cleansing agents of low density consist at least of 2 to 50% by weight of alkali metal phosphates, 2 to 50% by weight of silicates and 1 to 60% by weight of alkali metal hydroxides and/or alkali metal carbonates or bicarbonates and additionally contain 0.25 to 10% by weight of phosphoric acid partial esters. These cleansing agents are prepared by first foaming phosphoric acid partial esters with water in a weight ratio of (1:2) to (1:80), using intensive stirring. When the remaining components have been incorporated into the foam, using stirring or kneading, the resulting mixture is converted to moldings. The moldings are allowed to set for 0.5 to 15 hours.

Dimensionally stable alkaline cleansing agents of low density, and a

Chlorophosphines or thiophosphinic acid chlorides of the general formulae RPCl.sub.2, R.sub.2 PCl or R.sub.2 P(.dbd.S)Cl are made from feed materials selected from hydrogen-functional primary or secondary phosphines or secondary phosphine sulfides, where R stands for identical or different, linear or branched, substituted or unsubstituted alkyl radicals having from 1-16 carbon atoms, aryl radicals, aralkyl radicals or alkylaryl radicals having from 6-9 carbon atoms or cycloalkyl radicals having from 5-10 carbon atoms. To this end, the feed materials are reacted with phosphorus pentachloride, or with chlorine gas in the presence of phosphorus trichloride at temperatures within the range -78.degree. to +145.degree. C. It is possible for two radicals R to be linked together by one or two substituted or unsubstituted hydrocarbon chains having from 1-4 carbon atoms.

Process for making chlorophosphines and thiophosphinic acid chlorides,

The invention relates to a process for making 1-aminoalkane-1,1-diphosphonic acids of the general formula (I): ##STR1## in which R stands for an aliphatic hydrocarbon radical having from 1 to 12 carbon atoms. To this end, the invention provides:

Process for the manufacture of 1-aminoalkane-1,1-diphosphonic acids

The invention relates to a process for separating a mixture containing phosphoric acid monoalkylesters, phosphoric acid dialkylesters and minor proportions of diphosphoric acid dialkylesters, each with 6 to 12 carbon atoms in the alkyl radical, by extractively distributing them between an aliphatic or aromatic hydrocarbon as an unpolar solvent and a polar solvent. To this end, the invention provides: for the ester mixture to be admixed with the quantity of water stoichiometrically necessary for hydrolyzing the P-O-P-bond of the diphosphoric acid dialkylester with the resultant formation of the phosphoric acid monoalkylester; for the whole to be maintained for at least 1 hour at temperatures higher than 60.degree. C.; for the partially hydrolyzed ester mixture to be treated in a countercurrent apparatus comprising n-stages with the solvents immiscible or partially miscible with one another so as to ensure introduction of pure solvent into stage 1 and stage n, respectively, and the introduction of partially hydrolyzed mixture into one of the stages 2 to (n-1), n standing for a whole number of at least 3.

Process for extractively separating a mixture containing phosphoric acid

The invention relates to a process wherein an alcohol and/or phenol is reacted with phosphorus pentasulfide in the presence of a catalyst which is selected from

Process for reacting alcohols and/or phenols with phosphorus pentasulfide

The invention relates to the continuous production of phosphine. To this end, elemental phosphorus is reacted with an aqueous alkali metal hydroxide solution and at least one alcohol, the reactants being used in admixture with 0.01 to 2 weight % of a surfactant, the percentage being based on the alcohol.

Continuous production of phosphine

Orthophosphoric acid esters are made by reacting phosphorus(V)-oxide with an alcoholic component. More specifically, phosphorus(V)-oxide is reacted by mixing or kneading it with a blend consisting of a monohydric alcohol and an alkane polyol containing 2 to 12 carbon atoms and 2 to 6 hydroxyl groups, at approximately 0 to 120.degree. C. with the exclusion of moisture, in the presence of an inert gas, and over a period of approximately 1 to 6 hours. The resulting reaction product is cooled.

Production of acid orthophosphoric acid ester mixtures

Production of stabilized pulverulent red phosphorus. The phosphorus so stabilized comprises a homogeneous blend of red phosphorus particles with a size of at most about 2 mm and a metal compound of the second or third group of the Periodic System as an oxidation stabilizer, wherein the metal compound is the aluminum, calcium or zinc salt of a phosphinic acid of the general formula ##STR1## in which R.sub.1 and R.sub.2 each stand for an alkyl, cycloalkyl, aryl or aralkyl group having 1 to 20 carbon atoms, the metal compound being present in the homogeneous blend in a proportion of about 0.5 to 5 weight %.

Stabilized red phosphorus and process for making it

A product consisting essentially of an acid orthophosphoric acid ester salt and containing at most about 1 weight % of water is made. The ester group R contains 1 to 50 carbon atoms, and the salt-forming cation M is a mono- or bivalent metal ion or an ammonium ion. To make the product, molar proportions of P.sub.2 O.sub.5 and of a compound of the general formulae M.sub.2 O, M.sub.2 CO.sub.3, MO or MCO.sub.3 are reacted at about 0.degree. to 150.degree. C, with thorough agitation, with 2/m mol of an at least partially liquid or molten organic hydroxyl compound of the general formula R(OH).sub.m, in which formulae the substituents M and R have the meanings given above and m is a number of 1 to 4. The reaction is terminated and the reaction product is cooled.

Production of acid phosphoric acid ester salts

The invention provides stabilized pulverulent red phosphorus. It comprises a homogeneous blend of red phosphorus particles with a size of at most about 2 mm and a metal compound of the second or third group of the Periodic System as an oxidation stabilizer, wherein the metal compound is the aluminum, magnesium, calcium or zinc salt of an acid orthophosphoric acid ester of a long chain aliphatic alcohol, which may be ethoxylated, or phenol, the metal compound being present in the homogeneous blend in a proportion of about 0.25 to 5 weight %.

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