O.[PH2]([O-])=O.[Na+].S(=O)(=O)(O)O.C=C.C([O-])([O-])=O.C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[Al:31].[Al+3].[CH2:33]([P:35](CC)(=[O:37])[O-:36])[CH3:34].[CH2:40]([P:42](CC)(=[O:44])[O-:43])[CH3:41].[CH2:47]([P:49](CC)(=[O:51])[O-:50])[CH3:48]>O>[Al+3:31].[CH2:33]([P:35]([O-:37])[O-:36])[CH3:34].[CH2:40]([P:42]([O-:44])[O-:43])[CH3:41].[CH2:47]([P:49]([O-:51])[O-:50])[CH3:48].[Al+3:31]1500 g (14 mol) of sodium hypophosphite monohydrate and 14 g of concentrated sulfuric acid are dissolved in 7.5 kg of water and initially charged in a 16 l steel-enamel jacketed pressure reactor. After heating the reaction mixture to 100° C., a reducing valve set to 6 bar is used to introduce ethylene into the reactor up to saturation. While stirring constantly at an ethylene pressure of 6 bar and a temperature of 100-110° C., a solution of 22 g (1 mol %) of sodium percarbonate in 300 g of water is metered in homogeneously. At a conversion of ethylene of 83.5%, the metered addition of sodium percarbonate is stopped and the reactor is decompressed. After cooling to about 90° C., 3000 g (4.67 mol of aluminum) of a 46% aqueous solution of Al2(SO4)3.14H2O were added within 60 minutes. Subsequently, the resulting solid is filtered off, washed with 2 l of hot water and dried at 130° C. under reduced pressure. The resulting mixture comprises diethylphosphinic acid aluminum(III) salt and ethylphosphonous acid aluminum(III) salt in a ratio of 76.4% by weight of diethylphosphinic acid aluminum(III) salt and 23.6% by weight of ethylphosphonous acid aluminum(III) salt (95.0% yield).
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