FIELD: processing and recycling of waste.
SUBSTANCE: invention relates to processing of water-organic waste of organic synthesis molybdenum catalyst. Method involves distillation of hydrocarbons, treating the still residue of sulphuric acid, separation of product processing into water and organic phase, separation of water phase of molybdenum trioxide and decahydrate sodium sulphate, separation from the organic phase of phenol and benzoic acid. Distillation of hydrocarbon wide fraction is carried out by pungent water steam at temperature of 110-130 °C, bottoms are treated with concentrated sulphuric acid to pH 1-2 at temperature of 25-40 °C, stratification of the processes product into water and organic phases is carried out at 30-40 °C for 30-60 minutes, after which the phases are separated. Residues of phenol and benzoic acid are extracted from water phase cooled to 20-25 °C by methyl-tert-butyl ether in ratio of water and organic phases: O:W = 1:1. Water phase is separated from organic and treated with water solution of sodium hydrosulphide and/or sulphide in molar ratio Mo:S = 1:5 with extraction of molybdenum trisulphide precipitate by filtration followed by drying and oxidative firing molybdenum trisulphide to molybdenum trioxide at the temperature of 550-600 °C. Water filtrate after removal of molybdenum trisulfide cleaned from residues of organic phase by sorption on activated carbon with subsequent evaporation of water solution and crystallisation of evaporated solution decahydrate sodium sulphate. From the organic phase obtained after separation of the still residue, successively extracted phenol distillation with pungent water steam at temperature of 110-130 °C, followed by extraction of distillate methyl-tert-butyl ether in volume ratio of water and organic phase: aqueous phase = 1:1 and purification from impurities through distillation, and benzoic acid at a temperature of 105-110 °C refining°with extraction from the distillate is performed by filtration and removal of impurities-sublimation solid dried product at a temperature of 105-110 °C.
EFFECT: invention increases efficiency of extracting commercial liquid products from water-organic waste molybdenum catalyst of organic synthesis.
12 cl, 2 tbl
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Authors
Dates
2016-05-20—Published
2014-08-27—Filed