Hydrogen Peroxide → Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)

Participants

Reaction Conditions

Reaction Steps

1500 g (14 mol) of sodium hypophosphite monohydrate and 35 g of concentrated sulfuric acid were dissolved in 7.5 kg of water and used as initial charge in a 16 l jacketed pressure reactor composed of enameled steel. Once the reaction mixture had been heated to 10° C., ethylene was introduced by way of a reducing valve set to 6 bar until saturation had been reached in the reactor. A solution of 80 g (5 mol %) of hydrogen peroxide (33% by weight) in 300 g of water was metered in uniformly over a period of 6 h with constant stirring at an ethylene pressure of 6 bar and a temperature of from 100 to 110° C. After a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C., 746 g (4.67 mol of aluminum) of aluminum acetate in 2254 g of water were added within a period of 60 min. The resultant solid was then filtered off, washed with 2 l of hot water, and vacuum-dried at 130° C. Yield: 1721 g (93.5% of theory).

Provenance & Evidence