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Preparation method of 9-fluorenone

A technology of fluorenone and industrial fluorene, which is applied in the field of preparation of 9-fluorenone, can solve the problems of difficult processing and unfavorable environmental protection, and achieve the effects of low reaction temperature, less environmental pollution and mild reaction conditions

Inactive Publication Date: 2012-03-28
SINOSTEEL ANSHAN RES INST OF THERMO ENERGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of waste lye is produced in the above two inventions, which is difficult to handle and is not conducive to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 33.2g of fluorene, 85g of xylene, 0.67g of quaternary ammonium salt, and 4.9g of sodium hydroxide in a 250ml four-neck flask equipped with heating, stirring, thermometer, and reflux condenser, then heat to 90°C for solid dissolution, and control The temperature is 90-100°C, the air flow rate is 400ml / min for oxidation, the reaction is carried out for 4 hours, the reaction is stopped, the kettle liquid is filtered, vacuum distillation is recovered, the xylene solvent is recycled, and the concentrate is crystallized to obtain yellow fluorenone crystals. Wash with a small amount of water to remove alkali once, and dry to obtain 33.2 g of 9-fluorenone product, with a yield of 92.2%, a gas chromatography purity of 99.5%, and a melting point of 83-84°C.

Embodiment 2

[0026] Add 33.2g of fluorene, 85g of xylene, 0.9g of quaternary ammonium salt, and 4g of sodium hydroxide into a 250ml four-neck flask equipped with heating, stirring, thermometer, and reflux condenser, then heat to 90°C to dissolve the solid, and control the temperature 90 ~ 100 ℃ into the air flow rate of 400ml / min for oxidation, the reaction is carried out for 4 hours, stop the reaction, filter the kettle liquid, distill under reduced pressure, recover the xylene solvent for recycling, and crystallize the concentrate to obtain yellow fluorenone crystals. Wash once with a small amount of water, and dry to obtain 32.4 g of 9-fluorenone product, with a yield of 90.2%, a gas chromatography purity of 99.2%, and a melting point of 83-84°C.

Embodiment 3

[0028] Add 33.2g of fluorene, 85g of xylene, 0.8g of quaternary ammonium salt, and 3.5g of sodium hydroxide into a 250ml four-necked flask equipped with heating, stirring, thermometer, and reflux condenser, then heat to 90°C to dissolve the solid, and control The temperature is 90-100°C, the air flow rate is 400ml / min for oxidation, the reaction is carried out for 4 hours, the reaction is stopped, the kettle liquid is filtered, vacuum distillation, and the xylene solvent is recovered for recycling, and the concentrate is crystallized to obtain yellow fluorenone crystals , washed once with a small amount of water, and dried to obtain 31.2 g of 9-fluorenone product, with a yield of 86.7%, a gas chromatography purity of 99.5%, and a melting point of 83-84°C.

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Abstract

The invention relates to the technical field of production of an aromatic compound 9-fluorenone, in particular to a preparation method of the 9-fluorenone. The preparation method includes the steps as follows: 1) taking industrial fluorene, benzene series solvent, sodium hydroxide and quaternary ammonium salt, and adding the four components in a four-mouth bottle; 2) stirring the mixture in normal pressure, increasing the temperature to above 90 DEG C, reacting, and introducing air for oxidization; 3) conducting reduced-pressure distillation and allowing concentrate to crystallize, thus obtaining yellow fluorenone crystals; and 4) washing the fluorenone crystals for one time and then drying the fluorenone crystals, thus obtaining the 9-fluorenone product. The benzene series solvent is toluene or dimethylbenzene. Compared with the prior art, the preparation method has the benefits as follows: 1) the reaction temperature is low, the operation is simple and convenient and the reaction conditions are moderate; 2) the cheap sodium hydroxide is taken as a catalyst, so the cost is low; 3) the benzene series solvent can be recycled by reduced-pressure distillation, washing water is little in quantity, treatment is easy and pollution to environment is small; and 4) the gas chromatographic purity of the product is higher than 99.2%, the yield is higher than 86.7% and the production requirements are met.

Description

technical field [0001] The invention relates to the technical field of production of aromatic compound 9-fluorenone, in particular to a preparation method of 9-fluorenone. Background technique [0002] 9-Fluorenone (9-Fluorenonge), alias benzophenone, molecular formula C 13 h 8 O is a yellow orthorhombic crystal with a melting point of 84°C and a boiling point of 341.5°C. It is an important fine chemical raw material and is widely used in the synthesis and preparation of fuels, photoconductive materials, medicines, and luminescent materials. [0003] The main technology of the method for preparing 9-fluorenone by fluorene oxidation at home and abroad is as follows: In 1996, Nippon Shokubai Co., Ltd. used Han metal vanadium, titanium and alkali metal catalysts to prepare 9-fluorenone by gas phase method, and the reaction temperature was above 400 ° C. The yield is lower than 95% [ZL.96123084.3]. The preparation of 9-fluorenone by gas-phase oxidation of fluorene requires co...

Claims

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Application Information

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IPC IPC(8): C07C49/675C07C45/36
Inventor 王广兴王守凯方田焦宾姜辉臧娜
Owner SINOSTEEL ANSHAN RES INST OF THERMO ENERGY CO LTD
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