Method for producing 9-fluorenone by oxidizing fluorene

Abstract

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 0.5-5 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<3> / h into every kilogram of industrial fluorine, and reacting for 0.5-5 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.

Description

technical field [0001] The invention relates to the field of deep processing of coal tar products, in particular to a method for producing high-purity 9-fluorenone by oxidation of fluorene. Background technique [0002] Fluorenone is a light yellow orthorhombic crystal with a melting point of about 83-84°C and a boiling point of 342°C. Fluorenone is a raw material of important fine chemicals, often used as a synthetic intermediate material, and has extremely important applications in the fields of medicine, dyes, agriculture, chemicals, plastics industry and photoconductive materials. In recent years, with the development of material science, fluorenones have been widely used in the synthesis of organic polymer materials and optoelectronic materials. The most typical example is the manufacture of bisphenol fluorene. Polymer materials containing bisphenol fluorene have good thermal stability and strength. The 3M company of the United States was the first to develop a new ty...

AI Technical Summary

Problems solved by technology

These methods all use benzene, pyridine, etc. as solvents. The solvents are highly toxic and the reaction temperature is high, and the reaction is often carried out near the boiling point of the solvent used, mostly above 90°C. Even the reaction temperature using pyridine as the solvent is higher than 110°C. Long time, mostly more than 5-8 hours, not only high energy consumption but also easy to cause solvent dissipation

Images