Use of low boiling diluent in hydrolysis of aluminum alcoholate
An olefin having 2-4 carbon atoms is reacted with an alkyl aluminium hydride or aluminium trialkyl in which the alkyl groups have 2-8 carbon atoms, the so-formed trialkyl is oxidised to an aluminium alcoholate and the alcoholate is hydrolysed in the presence of 10-90% of the total volume of diethyl...
Gespeichert in:
1. Verfasser: | |
---|---|
Format: | Patent |
Sprache: | eng |
Schlagworte: | |
Online-Zugang: | Volltext bestellen |
Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
Zusammenfassung: | An olefin having 2-4 carbon atoms is reacted with an alkyl aluminium hydride or aluminium trialkyl in which the alkyl groups have 2-8 carbon atoms, the so-formed trialkyl is oxidised to an aluminium alcoholate and the alcoholate is hydrolysed in the presence of 10-90% of the total volume of diethyl ether, ethylpropyl ether or diisopropyl ether or a C5 hydrocarbon whereby the alcohol may be readily recovered. Specified hydrocarbons are n-pentane, isopentane and pentenes. The hydrolysis may be performed by means of water (or steam), aqueous ammonia or an aqueous organic or inorganic acid; in Examples ammonia is used. The alcoholates prior to hydrolysis generally contain alkoxy groups having 2-20 carbon atoms and preferably contain at least 5 weight per cent of C2-C4 alkoxy alcoholates. In examples, the higher aluminium alkyl was prepared by reacting aluminium tri-n-butyl in the presence of aluminium diethyl chloride with ethylene at 115 DEG C. and 1500 p.s.i.g. for 250 minutes, the product was diluted with n-heptane and oxidised with air at 95 DEG C. and atmospheric pressure; the heptane and by-product olefins were removed by distillation, diethyl ether (or n-pentane) was added and the mixture hydrolysed with aqueous ammonia; the mixture was aged and the resulting aqueous and organic layers separated. The organic phase was distilled to recover ether and the remaining organic phase was fractionated into the corresponding alcohols. In comparative examples describing only a fractionation, mixtures of ethanol, n-butanol, n-hexanol and either ether or n-hexane were fractionated: azeotroping took place between ethanol and n-hexane when the latter was used. If pentane is employed, azeotroping with ethanol is much less. Specifications 667,145 and 844,637 are referred to.ALSO:Aluminium alcoholates are hydrolysed in the presence of 10-90% of the total volume of diethyl ether, ethylpropyl ether, diisopropyl ether or a C5 hydrocarbon as a solvent, the so-formed alcohols are recovered, preferably the alumina is then aged to the b -form and calcined to the c -form; said alcoholates having been prepared by reacting an olefin with an aluminium trialkyl or an alkyl aluminium hydride, and oxidising the so-formed higher molecular weight aluminium trialkyl. Specified C5 hydrocarbons are n-pentane, iso-pentane and pentenes. The hydrolysis may be performed by means of water (or steam), aqueous ammonia or an aqueous organic or inorganic acid. In examples, ammonia is used. Specific |
---|