The Study Of1,3,5-Triisopropyl Benzene Oxidated And Descomposed To Prepare Phloroglucinol

Phloroglucinol is an important fine chemical products, the market value of up to500,000yuan/ton. Domestic use of trinitrotoluene, yield100tons/year or so, backward technology, environmental pollution, high costs, much-needed development of low-cost clean synthetic route.In this paper, to1,3,5-triisopropyl benzene as raw materials for synthetic Phloroglucinol the synthesis routes were studied. The whole process line is divided into three parts:three Cumene between the auto-oxidation (that is the first step oxidation), the second step acid oxidation and decomposition.First of all, a synthesis of the whole process of detection method suitable for intermediate products suitable response to the detection method is to use liquid chromatography to detect, monitor the absorption wavelength of257nm, the silica gel used InterSil, packing particles100A, Model4.6× 250mm hexane liquid mixed with isopropyl alcohol as the mobile phase, the choice of n-hexane and isopropyl alcohol mobile phase of the mixed-volume ratio of Vn-hexane:Visopropanol=97:3isopropanol, the velocity of flow=0.5ml/min. For Phloroglucinol product, the use of the silica gel used InterSil, packing particles100A, Model4.6x250mm optional n-hexane isopropanol mixed system, monitors the absorption of the selected270nm, the best conditions for the separation:Vn-hexane:Visopropanol=85:15isopropanol, mobile phase velocity=0.5ml/min.Furthermore, on a three Cumene the first step oxidation, identified in the loop reactor, as a solvent chlorobenzene (1,3,5-three Cumene mass ratio4:1), the reaction temperature is90℃, the air per100g isopropyl benzene three to80ml/min flow-income, three isopropyl benzene oxides do initiator, pH value maintained at9to10, intermittent operation, the response65hours, THPO and its derivatives to Rate82%.Then, inspected the first step of the separation method of using three percent concentration of NaOH solution in accordance with the three Cumene six times the quality of raw material extraction ratio, layered in and out after the lye, then with half the quality of NaOH solution The chlorobenzene extraction, the reaction of more than90percent in the THPO and its derivatives have been isolated from the extraction of chlorobenzene to.To be the first step of separation of chlorobenzene, the added alcohol (alcohol and chlorobenzene mass ratio of8:1), by adding benzyl alcohol Ji Moer15times the number of H2O2, H2O2phase concentration in the water are20%, By adding sulfuric acid to the water quality of15percent, the reaction temperature is50℃, for the second step of the reaction time of30min, will be THPO86%more selective.Finally, a comparison of two resin acid and sulfuric acid catalyst for the decomposition of hydrogen peroxide effect on the results showed that:acid resin Better decomposition, the amount of decomposition of the quality of0.1percent, temperature select60℃, reaction Time15-30min, depending on the quality of decomposition, but not more than30minutes. By phloroglucinol crude products, and then through activated carbon and decoloration recrystallization, refined by the end of the phloroglucinol products, the purity of96.3%.Overall, this study has1,3,5-triisopropyl benzene to phloroglucinol the transformation process, to find a more suitable for low-cost clean Synthesis of the line.