Phenol hydrogen peroxide hydroxylation reaction wastewater recovering and applying method
A technology of hydrogen peroxide and hydroxylation, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult treatment of wastewater, and achieve the effects of fast reaction speed, high safety factor, and easy operation.
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[0034] Preparation of wastewater
[0035] The waste water in the examples was prepared in the following manner. The phenolic hydrogen peroxide hydroxylation reaction solution was extracted with a ratio of 1.2:1 with MIBK, and the oil phase and the waste water phase were separated.
Embodiment 1
[0037] In a 2000mL four-necked bottle, add 1500mL of waste water after extraction and 6g of PEG1000 dispersant, and stir evenly. The reaction temperature was raised to 65°C, stirred at a rotational speed of 600 r / min for 2 hours, then the reaction temperature was lowered to 35°C and stirred for 1 hour, then allowed to stand for 1 hour, and then filtered to obtain 1.767g of powdery tar polymer microspheres (See image 3 ), the wastewater changes from black to reddish brown (see Figure 4 ) of the recyclable aqueous phase.
[0038] The recovered water phase, phenol and iron-based catalyst are prepared into a phenol raw material solution in a mass ratio of 5:1:0.01. When the temperature of the microchannel reactor rises to 65 °C, the phenol raw material solution and hydrogen peroxide are pumped into the microchannel for hydroxylation. In the reaction, the molar ratio of phenol to hydrogen peroxide was 1:0.8, and the residence time was 30 seconds. The test results are: the conv...
Embodiment 2
[0042] In a 2000mL four-necked bottle, add 1500mL of waste water after extraction and 9g of PEG1000 dispersant, and stir evenly. Raise the reaction temperature to 60°C, stir at a rotational speed of 800 r / min for 2 hours, then lower the reaction temperature to 35°C and stir for 1 hour, let stand for 1 hour, and then filter to obtain 1.785g of powdery tar polymer microspheres .
[0043] The recovered water phase, phenol and iron-based catalyst are prepared into a phenol raw material solution in a mass ratio of 5:1:0.01. When the temperature of the microchannel reactor rises to 65 °C, the phenol raw material solution and hydrogen peroxide are pumped into the microchannel for hydroxylation. In the reaction, the molar ratio of phenol to hydrogen peroxide was 1:0.8, and the residence time was 30 seconds. The test results are: the conversion rate of phenol is 39.3%, and the selectivity of diphenol is 94.1%.
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