Vanadium oxy-trialcoholates from the pentoxide and alcohols - sepg. water as azeotrope forming two phases on cooling

摘要

Prior art process for prepn. of vanadium oxytrialcoholates VO(OR)3 (where R = 2-5C alkyl) by reaction of V2O5 with excess alcohol, ROH, under reflux and sepg. the water formed, is modified by using 1.5-10, pref. 2-5 times theoretical ROH, sepg. water as an azeotrope via a fractionating column, allowing the distillate to partition into a lower layer and an upper layer which is returned to the reaction vessel which opt. contains a known entrainment agent e.g., benzene. When R = Bu or iso-Bu no entrainer is required. When R = Et, n-Pr, iso-Pr, sec.-Bu or t.-Bu entrainer is benzene. Ratio of ROH to entrainer is pref. 1.5-50:1 and esp. 5-20:1. Prodts. are used for prepn. of Ziegler catalysts.