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

HRID 1868564Notes

Reaction equation

O.[PH2:2]([O-:4])=[O:3].[Na+].S(=O)(=O)(O)O.C=C.OO.[C:15]([O-])(=O)[CH3:16].[Al+3:19].[C:20]([O-])(=O)[CH3:21].[C:24]([O-])(=O)[CH3:25]>O>[CH2:20]([P:2]([CH2:15][CH3:16])(=[O:4])[O-:3])[CH3:21].[Al+3:19].[CH2:24]([P:2]([CH2:15][CH3:16])(=[O:4])[O-:3])[CH3:25].[CH2:20]([P:2]([CH2:15][CH3:16])(=[O:4])[O-:3])[CH3:21]

Participants

Conditions

Temperature: 10 °C

Procedure

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).

Workup

additionas initial charge in a 16 l jacketed pressure reactor
customof 6 h
customof from 100 to 110° C
temperatureAfter a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C.
filtrationThe resultant solid was then filtered off
washwashed with 2 l of hot water
customvacuum-dried at 130° C

Sources & evidence

ORD record: ord-0fd26ff6192d4d04b329257773763100
Source dataset: uspto-grants-2009_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07635785B2

Reaction notes

Loading…