A New Purification and Refining Process of Crude Fluorene
A crude fluorene and process technology, which is applied in the field of crude fluorene purification and refining new process, can solve the problems of high solvent toxicity, high cost, and low product purity, and achieve simple equipment and process, less production, and low operation and running costs Effect
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Embodiment 1
[0018] Take 1000.00g of crude fluorene containing 69.91% by mass of fluorene, add 1000.00g of n-butanol to the reactor, stir at room temperature for 40min at a stirring speed of 30r / min, then filter and dry to obtain industrial Fluorene 673.80g, wherein the yield of fluorene is 85.22%;
[0019] Then, according to the mass ratio of toluene, water and industrial fluorene at 0.5:0.5:1, add 673.80g of industrial fluorene obtained above into the reactor—"a new type of equipment for purifying refined fluorene from industrial fluorene" (patent number 2012205596915), Then add 336.89g of toluene and 336.89g of water, turn on the program heating and cooling control device to heat, turn on the mixer, the stirring speed is 30r / min, stir for 40min, and heat to 90°C until the above industrial fluorene is completely dissolved; turn off the mixer, pass the program The temperature rise and fall control device adjusts the temperature of the reactor to keep the temperature at a cooling rate of 5...
Embodiment 2
[0021] Take 1000.00g of crude fluorene containing 60.55% by mass of fluorene, add 1000.00g of ethyl acetate to the reaction kettle, stir at room temperature for 50min at a stirring speed of 60r / min, then filter and dry to obtain 588.68g of mass content with a purity of 85.70% The fluorene, wherein the yield of fluorene is 83.32%.
[0022] According to the mass ratio of cyclohexane, water and industrial fluorene of 0.5:0.5:1, 588.68g of industrial fluorene, 294.34g of cyclohexane and 294.34g of water obtained above are added to the reaction kettle——"a kind of purification from industrial fluorene In "New Equipment for Fluorene" (Patent No. 2012205596915), turn on the program heating and cooling control device to heat, turn on the mixer, stir at a speed of 60r / min, stir for 50 minutes, and heat to 90°C until the above-mentioned industrial fluorene is completely dissolved; turn off the mixer, The temperature of the reactor is adjusted by the programmed temperature rise and fall c...
Embodiment 3
[0024] Take 1000.00g of crude fluorene containing 65.82% by mass of fluorene, add 1000.00g of solvent dimethylformamide to the reaction kettle, stir at room temperature for 60min at a stirring speed of 90r / min, then filter and dry to obtain 649.95g of mass content Fluorene with a purity of 86.23%, wherein the yield of fluorene is 85.11%.
[0025] According to the mass ratio of cyclopentadiene, water and industrial fluorene of 0.5:0.5:1, 649.95g of industrial fluorene, 324.98g of cyclopentadiene and 324.98g of water obtained above are added to the reactor—"a kind of industrial fluorene In the new equipment for purifying refined fluorene" (Patent No. 2012205596915), turn on the program heating and cooling control device to heat, turn on the mixer, stir at a speed of 90r / min, stir for 60 minutes, and heat to 90°C until the above industrial fluorene is completely dissolved; close Stirrer, adjust the temperature of the reactor through the programmed temperature rise and fall contro...
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Abstract
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