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

Participants

Reaction Conditions

Reaction Steps

1500 g (14 mol) of sodium hypophosphite monohydrate 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 100° 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 19 g (0.5 mol %) of 2,2′-azobis(2-amidinopropane) hydrochloride (Wako Pure Chemical Industries, Ltd., grade V50 98.8%) in 300 g of water was uniformly metered in 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., 650 g (4.67 mol of aluminum) of aluminum chloride hexahydrate in 2350 g of water were added over 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.

Provenance & Evidence