A method for separating phenanthrene and fluorene
A filtration separation and fluorenone technology, applied in chemical instruments and methods, hydrocarbon purification/separation, distillation purification/separation, etc., can solve the problems of low separation efficiency, difficult separation of phenanthrene and fluorene, etc., and achieve the effect of efficient separation
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Embodiment 1
[0037]Add 5.4052g of 9-fluorenone and 20.0475g of phenanthrene into 75mL of anhydrous methanol, heat to 40°C, stir at constant temperature for 30min, then slowly lower to 20°C, and filter to obtain 17.83g of phenanthrene with a purity of 98.10%. The filtrate was distilled under reduced pressure to remove methanol, then dried naturally, then added 18mL of cyclohexane, heated to 40°C and stirred at constant temperature for 30min, then slowly lowered to 20°C, filtered to obtain 4.57g of 9-fluorenone with a purity of 95.58%; 6 mL of cyclohexane was added to the obtained 9-fluorenone, and after further purification, 3.94 g of 9-fluorenone was obtained with a purity of 98.57%. The calculated phenanthrene yield was 87.27%, and the 9-fluorenone yield was 71.85%.
Embodiment 2
[0039] Add 3.33g of fluorene, 13.33g of phenanthrene, and 40mL of xylene in sequence into a jacketed reactor equipped with a magnetic stirrer and a condensing tube, pass hot water into the jacket, reflux at 58°C, and stir at a rate of 300r / min. After the fluorene and phenanthrene are dissolved, add 6.55g KOH, 8mL water, 0.33g tetrabutylammonium chloride, and feed air (rate 400mL / min). After 2h, all the fluorenes were converted, and the reaction was terminated. After oil-water separation, the organic phase was distilled under reduced pressure to obtain a mixture of phenanthrene and 9-fluorenone. The product was quantified using the internal standard curve method of gas chromatography. It was found by gas chromatography that ( image 3 ), except for impurities in 9-fluorenone and fluorene and phenanthrene in the product, no oxidation product of phenanthrene was detected, indicating that under the liquid phase oxidation conditions used in the experiment, phenanthrene was not ox...
Embodiment 3
[0042] Add 5g fluorene, 20g phenanthrene, 50mL xylene, 8.18gKOH, 10mL water, 0.50g tetrabutylammonium chloride in sequence in a jacketed reactor equipped with a magnetic stirrer and a condenser, and the others are the same as in Example 2. 3.5h After the fluorene is completely converted, the reaction is terminated. Separation was carried out according to the process of Example 1 to obtain 17.07 g of phenanthrene, with a purity of 98.07%; 4.41 g of 9-fluorenone, with a purity of 95.23%, and then 6 mL of cyclohexane was added to the obtained 9-fluorenone, and 9-fluorene was obtained after further purification Ketone 3.85g, purity 98.18%. The calculated phenanthrene yield was 83.70%, and the 9-fluorenone yield was 70.00%.
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