Attempts were made to isolate 1,2-epoxybutane-3-ol and 2,3-epoxybutane-1-ol from post-reaction mixtures left after the epoxidation of 1-butene-3-ol and 2-butene-1-ol with hydrogen peroxide by thin film distillation. From the raw mixture containing about 8.3 wt% of the epoxide at the first stage the concentration of epoxide is increased to 32 wt%. At the second stage of distillation the epoxide fraction is concentrated to about 76 wt%. After the third stage of thin film distillation the epoxide fraction of 99.6% purity can be obtained. The concentration of this fraction by azeotropic distillation with n-propanol as an azeotropic agent permits obtaining epoxide of 99.6 wt% purity.
The results of the epoxidation of 2-buten-1-ol with 30 wt% hydrogen peroxide have been presented. As a solvent methanol was used. The process was carried out over the titanium silicalite catalysts: Ti-MCM-41 and Ti-MCM-48. The influence of temperature (20 - 120°C), the molar ratio of CRA/H2O2 (5:1 - 5:1), methanol concentration (5 - 90 wt%), catalyst concentration (0.1 - 5.0 wt%) and the reaction time (30 - 300 min) was investigated. The obtained results were used for the determination of optimum conditions of running the epoxidation process of 2-buten-1-ol.
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