Process for purifying industrial fluorene
An industrial fluorene and process technology, which is applied in the field of coal tar deep-processing products, can solve the problems of limited improvement of primary crystallization purity, increased equipment investment, and large safety hazards, and achieves the effects of reducing recycling trouble, good effect, and improving safety.
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Embodiment 1
[0028] Such as figure 1 As shown, in the fluorene crystallizer with a volume of 8m3, 4000kg of fluorene fraction containing 61.26% of fluorene and 1600kg of medium washing oil were successively added, and the temperature was raised to 110°C under stirring conditions to dissolve all the materials. The stirring speed was 24r / min, and then controlled Cool down to 22°C at a constant rate of 4°C / h, keep the temperature for 1h, and then centrifuge to obtain 1990kg of crude fluorene, containing 92.11% fluorene, and the yield of this process is 74.80%.
[0029] The filtrate directly enters the medium-quality washing oil tank for washing benzene.
[0030] Put the crude fluorene obtained above into the fluorene recrystallizer with a volume of 5m3, add 800kg of No. 200 solvent oil, stir and raise the temperature to 130°C, the stirring speed is 24r / min, and then control the temperature at a uniform rate of 10°C / h Centrifuge at 22°C for 1 hour to obtain 1610kg of industrial fluorene, cont...
Embodiment 2
[0033] Add 4000kg of fluorene fraction containing 64.28% fluorene and 1700kg of medium washing oil into the fluorene crystallizer with a volume of 8m3, and heat up to 110°C under stirring conditions to dissolve all the materials. The stirring speed is 24r / min, and then controlled at 4°C The temperature was lowered to 22°C at a constant rate of / h, and then kept at a constant temperature for 1h, and then centrifuged to obtain 2120kg of crude fluorene, containing 92.33% fluorene, and the yield of this process was 76.13%. The filtrate is used to wash benzene.
[0034] Put the crude fluorene obtained above into a fluorene recrystallizer with a volume of 5m3, add 850kg of No. 200 solvent oil, stir and raise the temperature to 130°C, the stirring speed is 24r / min, and then control the temperature at a uniform rate of 10°C / h Centrifuge at 22°C for 1 hour to obtain 1730kg of industrial fluorene, containing 97.26% fluorene. The yield of this process is 85.96%, and the total yield is 65...
Embodiment 3
[0037] Add 4000kg of fluorene fraction containing 67.35% fluorene and 1800kg of medium washing oil into the fluorene crystallizer with a volume of 8m3, and heat up to 120°C under stirring conditions to dissolve all the materials. The stirring speed is 24r / min, and then controlled at 5°C The temperature was lowered to 20°C at a constant speed at a rate of / h, and then kept at a constant temperature for 1 hour, and then centrifuged to obtain 2280 kg of crude fluorene, containing 92.03% fluorene, and the yield of this process was 77.89%.
[0038] Put the crude fluorene obtained above into the fluorene recrystallizer with a volume of 5m3, add 920kg of No. 200 solvent oil, stir and raise the temperature to 130°C, the stirring speed is 24r / min, and then control the temperature at a uniform rate of 10°C / h Centrifuge at 24°C for 1 hour to obtain 1835kg of industrial fluorene, containing 97.18% fluorene. The yield of this process is 85.00%, and the total yield is 66.19%.
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