Reaktion #425228

Reaktionsgleichung

diethylphosphinic acid aluminum(III) salt

aluminum

ammonium peroxodisulfate

ethylene

ethylene

ethylene

ammonium peroxodisulfate

sodium hypophosphite monohydrate

→

ethylphosphonous acid aluminum(III) salt

Ausbeute 96.3%

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea reducing valve set to 20 bar
2. 2
   Sonstigea temperature of 100-110° C.
3. 3
   TemperaturAfter cooling to about 90° C.
4. 4
   FiltrationSubsequently, the resulting solid is filtered off
5. 5
   Waschenwashed with 2 l of hot water
6. 6
   Sonstigedried at 130° C. under reduced pressure

Vorschrift

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 20 bar is used to introduce ethylene into the reactor up to saturation. While stirring constantly at an ethylene pressure of 20 bar and a temperature of 100-110° C., a solution of 32 g (1 mol %) of ammonium peroxodisulfate in 300 g of water is metered in homogeneously. At a conversion of ethylene of 90%, the metered addition of ammonium peroxodisulfate 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 is 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 87.3% by weight of diethylphosphinic acid aluminum(III) salt and 12.7% by weight of ethylphosphonous acid aluminum(III) salt (96.3% yield).

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