Method for preparing coarse fluorene and fluorenone by taking wash oil as raw material
A technology for washing oil and crude fluorene, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc. It can solve the problems of high energy, difficulty in industrial fluorene, waste of materials, etc., and achieve the effect of reducing energy consumption
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Embodiment 1
[0020] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 275 ° C fraction, and then secondary rectification respectively cut 265 ° C, 270 ° C fractions, and then these fractions were put into the refrigerator to cool and crystallize to obtain crude fluorene.
[0021] (2) Weigh 2g of crude fluorene, 14g of N,N-dimethylformamide, and 0.050g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirring The fluorenone mixture was stirred by using a mixer, and air was blown to the reaction device at a blowing rate of 450ml / min. The reaction was carried out at room temperature...
Embodiment 2
[0025] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 260 ° C fraction, and then secondary rectification respectively cut 260 ° C, 265 ° C fractions, and then these fractions were put into the refrigerator to cool and crystallize to obtain crude fluorene.
[0026] (2) Weigh 2g of crude fluorene, 14g of N,N-dimethylformamide, and 0.050g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirrer Stir, and blow air to the reaction device, the air blow rate is 450ml / min, the reaction is carried out at room temperature, and the whole reaction process is detected by TLC u...
Embodiment 3
[0030] (1) Use an equal volume of 10% sulfuric acid solution (weight ratio) and 10% sodium hydroxide solution (weight ratio) to wash the washing oil with acid and alkali at room temperature in sequence, and wash with distilled water to remove residual alkali or salt and magnesium sulfate , drying to remove residual moisture, the obtained neutral washing oil rectification cut 270 ° C fractions, and then secondary rectification were cut 260 ° C, 270 ° C fractions, and then these fractions were placed in the refrigerator to cool and crystallize to obtain crude fluorene.
[0031] (2) Weigh 2g of crude fluorene, 16g of N,N-dimethylformamide, and 0.056g of potassium hydroxide into a round low flask equipped with a magnetic stirrer, reflux condenser, and air blowing device, and turn on the magnetic stirring Stir with a mixer, and blow air to the reaction device, the air blow rate is 450ml / min, the reaction is carried out at room temperature, the whole reaction process is detected by T...
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