The invention discloses a method for producing 9-fluorenone by oxidizing fluorine The method comprises the following steps of: dissolving industrial fluorine as a raw material in to a halogenated hydrocarbon solvent at the temperature of 30-80 DEG C, adding sodium hydroxide and a quaternary ammonium salt which are cheaper than potassium hydroxide for serving as catalysts, reacting in a reaction kettle for 05-5 hours, separating a liquid, and distilling an organic phase under reduced pressure for removing the solvent to obtain an intermediate substance; adding an intermediate and an alcohol solvent into the reaction kettle, heating to 40-80 DEG C for dissolving, introducing air at the speed of 1-10m /h into every kilogram of industrial fluorine, and reacting for 05-5 hours; and after the reaction, removing the solvent under reduced pressure, cooling and crystallizing simultaneously, and filtering a crystal product to obtain fluorenone The equipment investment is low, process operation is easy, the solvent can be recycled, and cost is effectively saved; an obtained fluorenone product has high purity and high yield; in an entire process, an industrial grade organic solvent is adopted, so that operation and running costs are low; and an entire device is controlled automatically, so that operation conditions are improved, and the product quality stability is ensured simultaneously

Method for producing 9-fluorenone by oxidizing fluorene

The invention provides a method for synthesizing 2,7-diaminofluorene from fluorene. The method has advantages of high yield, simple reaction operation, low cost and little environmental pollution. The method comprises the following key steps: carrying out a reaction between fluorene and tetrahydrofuran and inorganic base at room temperature, carrying out suction filtration on reaction products after the reaction, concentrating, mixing with alkaline water and stirring, and carrying out suction filtration to obtain fluorenone, carrying out a reaction between fluorenone and mixed acids of concentrated sulfuric acid and concentrated nitric acid and refluxing, adding water after the reaction, carrying out suction filtration to obtain 2,7-dinitrofluorenone, dissolving 2,7-dinitrofluorenone in an alcoholic solution, adding anhydrous calcium chloride and zinc dust, carrying out a reflux reaction, precipitating by adding water after the reaction, carrying out suction filtration to obtain 2,7-diaminofluorenone, dissolving 2,7-diaminofluorenone in an alcoholic solution, carrying out a reflux reaction, dropwisely adding concentrated hydrochloric acid and amalgam zinc in batches, cooling after the reaction, carrying out suction filtration, and carrying out recrystallization to obtain 2,7-diaminofluorene.

Synthetic method of 2,7-diaminofluorene

The invention relates to the technical field of the production of aromatic compound 2, 7-binitro fluorenone, particularly to a method for producing 2, 7-binitro fluorenone. The method for producing 2, 7-binitro fluorenone is characterized by comprising the following steps: (1), adding industrial 2, 7-binitro fluorenone, benzene series resolvent, sodium hydroxide and quaternary ammonium salt into four bottles; (2), carrying out air oxidation under the temperature of 90 to 100 DEGC, and reacting for 6 to 7 hours: (3), recovering solvent through reduced pressure distillation and crystallizing condensate; and (4), washing, alkali removing and drying so as to obtain the product of 2, 7-binitro fluorenone. The benzene series resolvent is toluene or xylene. Compared with the prior art, the invention has the benefits as follows: (1), the reaction temperature is low, the operation is simple and convenient, and the reaction conditions are moderate; (2), sodium hydroxide is taken as the catalyst, and the cost is low; (3), the benzene series resolvent can be depressurized, distilled, recovered and recycled, the wash water is easy to be treated, and pollutions to the environment are small; and (4), the purity of the gas phase chromatography of the product is higher than 99.1 percent, the yield is higher than 84.8 percent, and the production requirements are met.

Method for producing 2, 7-binitro fluorenone

The invention relates to a process for extracting high-purity carbazole from anthracene oil by a coupling separation method. The process comprises the following steps of (1) adding raw material anthracene oil fractions and catalysts into a high pressure hydrogenation kettle for hydrogenation reaction; (2) filtering reaction liquid; recycling catalysts; directly cooling filter liquid to obtain carbazole products; or performing reduced pressure distillation/normal pressure distillation on the filter liquid to separate out light fractions including anthracene hydride and hydrophenanthrene; performing heating dissolution after a first solvent is added into the rest kettle liquid; then, performing cooling and recrystallization to obtain the carbazole products; (3) performing vacuum drying on the obtained carbazole products to obtain high-purity carbazole with the purity being greater than 98.5 percent. The anthracene oil fractions are subjected to selective hydrogenation; the boiling pointand the melting point of the separation ingredients are effectively reduced; through the simple reduced pressure distillation/normal pressure distillation, hydrogenation products of anthracene and phenanthrene can be separated out; the rest carbazole enriched liquid is treated by a crystallization method to obtain the high-purity carbazole product. The problems of complicated technical flow process, high energy consumption, serious environmental pollution and the like in the conventional carbazole separation and extraction process are solved.

Guangxing Wang

Papers

Method for producing 2, 7-binitro fluorenone

Process for extracting high-purity carbazole from anthracene oil by coupling separation method