FIELD: chemistry.
SUBSTANCE: present invention relates to a method for producing cyclohexyl hydroperoxide by liquid-phase non-catalytic oxidation of cyclohexane with air at a temperature of 150-180°C and a pressure of 0.8-1.6 MPa in a cascade of mixing reactors in the presence of an initiating additive to obtain a reaction liquid containing cyclohexane, cyclohexyl hydroperoxide, cyclohexanone and cyclohexanol, and reaction gases; by separating unreacted cyclohexane from the reaction gases by absorption and returning it to the oxidation stage; treating the reaction liquid with alkali to obtain an aqueous-alkaline layer and an organic layer; by distillation of unreacted cyclohexane from the reaction liquid in a rectification column to obtain cyclohexane in the upper part of the column, return it to the oxidation stage and obtain a mixture of cyclohexyl hydroperoxide, cyclohexanone and cyclohexanol in the lower part of the column as the target product. In this case, a mixture of cyclohexyl hydroperoxide, cyclohexanone and cyclohexanol obtained in the lower part of the column after distilling off the organic layer in an amount of 0.01-0.1 wt% is used as an additional initiating additive in relation to the total amount of recycled cyclohexane; the treatment of the reaction liquid with alkali is carried out in the presence of radical scavengers selected from the group of m-cresol, a mixture of m- and p-cresols, hydroquinone, pyrocatechol, benzoquinone and bisphenol A, taken in an amount of 0.01-0.1% wt. of the content of cyclohexyl hydroperoxide in the reaction liquid; air heated to the temperature of the reaction medium is used, and the process is carried out with the amount of air supplied to the oxidation zones, in accordance with the dependence Q (N + 1) = (1.33 ± 0.05) x Q (N), where Q (N +1) and Q (N) show the amount of air supplied to the next and previous oxidation zones, respectively; N is the ordinal number of the oxidation zone, counting in the direction of movement of the process stream.
EFFECT: method allows carrying out the process with obtaining cyclohexyl hydroperoxide in oxidate stably at the level of 5.0-6.0% wt. while maintaining high cyclohexyl hydroperoxide selectivity of the process - 95-97%.
1 cl, 2 dwg, 2 tbl, 10 ex
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Authors
Dates
2021-05-05—Published
2020-10-27—Filed