M. Attou et al., PROMOTING ACTION OF POCL3 IN O-PHOSPHORIC ACID ESTERIFICATION BY N-BUTANOL, Bulletin des Societes chimiques belges, 102(10), 1993, pp. 673-678
The opportunity of tri-n-butylphosphate(TBP) synthesis via esterificat
ion of o-phosphoric acid with n-butanol, under special conditions, was
investigated. The reagents were contacted without solvent in an autoc
lave, in the presence of small amounts of phosphorus oxichloride(ca. 6
.10(-4) mole per gram of reaction mixture), under argon pressure, duri
ng 3 hours. A strong dependence is observed between all operating para
meters i.e. temperature, pressure, phosphorus oxichloride content and
the reagents mole. The results obtained show clearly the promoting act
ion of phosphorus oxichloride. It was also depicted that TBP synthesis
is the main reaction in such conditions. An additive optimization stu
dy allowed to confirm the previous observations. Compared to the class
ical TBP synthesis ways, the present procedure appears as being a very
interesting low cost alternative if one takes into account that the u
se of phosphorus oxichloride as reagent is avoided.