O.[PH2]([O-])=O.[Na+].C=C.C([O-])([O-])=O.C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].C(N(C(=O)C)CCN(C(=O)C)C(=O)C)(=O)C.[Al:42].[Al+3].[CH2:44]([P:46](CC)(=[O:48])[O-:47])[CH3:45].[CH2:51]([P:53](CC)(=[O:55])[O-:54])[CH3:52].[CH2:58]([P:60](CC)(=[O:62])[O-:61])[CH3:59]>O>[Al+3:42].[CH2:44]([P:46]([O-:48])[O-:47])[CH3:45].[CH2:51]([P:53]([O-:55])[O-:54])[CH3:52].[CH2:58]([P:60]([O-:62])[O-:61])[CH3:59].[Al+3:42]
1500 g (14 mol) of sodium hypophosphite monohydrate 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 and 16 g of tetraacetylethylenediamine in 300 g of water is metered in homogeneously. At a conversion of ethylene of 85%, the metered addition of sodium percarbonate and tetraacetylethylenediamine 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)3.14 H2O is added within 60 minutes. Subsequently, the resulting solid was 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 79.5% by weight of diethylphosphinic acid aluminum(III) salt and 20.5% by weight of ethylphosphonous acid aluminum(III) salt (95.9% yield).
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