Abstract
A technological process of manufacturing glycidol designed for the production capacity of 10 thousand tons per year and consisting in the direct oxidation of allyl alcohol with an aqueous solution of hydrogen peroxide in the presence of nanostructured titanium silicate in methanol is proposed. Due to the exothermic process, the solvent is not only a homogenizer of the mixture of the initial reagents of the epoxy process - allyl alcohol and hydrogen peroxide ensuring their interaction on the surface of the solid catalyst: it also prevents overheating of the reaction mass. On the basis of the research trial of the process the optimal parameters of the process were determined: temperature 30-40 °C; pressure 0.25 MPa; the initial hydrogen peroxide : allyl alcohol ratio = 1:(3-4) mass., methanol concentration in the reaction mixture 12-13 mol/l. Hydrogen peroxide conversion is 98%, the yield of the glycidol - 94%, the selectivity is no less than 95%. The process includes three main stages: (1) raw materials preparation, (2) liquid-phase epoxidation of allyl alcohol, (3) distillation of the target product. The scheme involves recirculation of unreacted allyl alcohol and the solvent - methanol. The developed technological process provides the following indicators (per 1 t of commercial glycidol): consumption of allyl alcohol no more than 0.843 t; consumption of hydrogen peroxide no more than 0.50 t (calculated for 100% hydrogen peroxide); consumption of methanol is no more than 0.022 tons All the waste products correspond to the 3-rd or 4-th hazard class.
Highlights
A technological process of manufacturing glycidol designed for the production capacity of 10 thousand tons per year and consisting in the direct oxidation of allyl alcohol with an aqueous solution of hydrogen peroxide in the presence of nanostructured titanium silicate in methanol is proposed
Due to the exothermic process, the solvent is a homogenizer of the mixture of the initial reagents of the epoxy process – allyl alcohol and hydrogen peroxide ensuring their interaction on the surface of the solid catalyst: it prevents overheating of the reaction mass
The developed technological process provides the following indicators: consumption of allyl alcohol no more than 0.843 t; consumption of hydrogen peroxide no more than 0.50 t; consumption of methanol is no more than 0.022 tons All the waste products correspond to the 3-rd or 4-th hazard class
Summary
Тонн в год и заключающийся в прямом окислении аллилового спирта водным раствором пероксида водорода в присутствии наноструктурированного силикалита титана в среде метанола. Ввиду экзотермичности процесса растворитель является не только гомогенизатором смеси исходных реагентов процесса эпоксидирования – аллилового спирта и пероксида водорода, обеспечивая их взаимодействие на поверхности твердого катализатора, но и препятствует перегреву реакционной массы. На основании исследовательских испытаний жидкофазного эпоксидирования аллилового спирта определены оптимальные параметры проведения процесса: температура 30-40 0С; давление 0.25 МПа; начальное массовое соотношение пероксид водорода:аллиловый спирт = 1:(3-4), концентрация метанола в реакционной смеси 12-13 моль/л. Разработанный технологический процесс обеспечивает следующие показатели (в расчете на 1 т товарного глицидола): расход аллилового спирта – не более 0.843 т; расход пероксида водорода – не более 0.50 т (в пересчете на 100%-ый пероксид водорода); расход метанола – не более 0.022 т. Для цитирования: Леонтьева С.В., Флид М.Р., Трушечкина М.А., Баботина М.В., Флид В.Р., Сулимов А.В.
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