Method for oxidizing fluorene to 9-fluorenone

A technology for the production of fluorenone by oxidation, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as high environmental requirements, unfavorable industrialization implementation, etc., and achieves reduction in production costs and convenience. The effect of industrialized implementation and low price

Active Publication Date: 2006-04-05
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technologies disclosed in the above-mentioned Japanese Patent Laying-Open No. 6-211729, 7-82207, and 7-82206 are all dangerous chemicals due to the use of aromatics (toluene, etc.) as solvents, and methanol, etc., for recrystallization. Inflammable and explosive unsafe hazards and high requirements for the environment are not conducive to industrial implementation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 31Kg dimethyl sulfoxide, 28Kg industrial fluorene with a content greater than 90% and 0.35Kg sodium hydroxide into a 100-liter dissolution kettle, heat and stir to dissolve, and then put it into a tower-type packing reactor with a jacket for heat preservation. Under the condition of a temperature of 50°C, 22 L / min of industrial oxygen was introduced from the bottom of the reactor for 3 hours. The reaction liquid was cooled and separated to obtain crude fluorenone with a purity of 93%, and the liquid was distilled to recover 94% of the solvent to obtain part of the crude fluorenone (conversion rate 99.5-100%, yield 96%). The crude fluorenone is pumped into the crystallization tank of the first section by the raw material pump, and each fraction pump is respectively pumping the material of each fraction tank into the corresponding crystallization box, and each fraction is respectively obtained through cooling, heating, heat preservation, and melting operation and put i...

Embodiment 2

[0039] name

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Abstract

The invention discloses a method to prepare 9-fluorenone with fluorene. Wherein, using dimethyl sulfoxide as solvent, sodium hydroxide as catalyst, oxygen as oxidant and tower filling reactor; cooling and filtering the reacted liquid to obtain 93% coarse fluorenone; distilling liquid and recycling 94% solvent and some coarse fluorenone; refining with oriented crystallization method and obtaining yellow piece 99.8% fluorenone. This method is simple, needs short reaction time, produces no waste water, and convenient to produce in industry.

Description

technical field [0001] The invention relates to a preparation method of 9-fluorenone, in particular to a method for preparing 9-fluorenone by oxidation of fluorene. Background technique [0002] 9-Fluorenone (9-Fluorenone), alias benzophenone, molecular formula C 13 H 8 O, structural formula: Molecular weight 180.21, yellow orthorhombic crystal, melting point 84°C, boiling point 341.5°C, is an important fine chemical raw material. As early as the 1930s and 1950s, foreign countries have studied fluorenone in dyes, medicines, and pesticides. Its preparation method mainly uses fluorenone as raw material to synthesize monomers or derivatives containing fluorene structure, which are used for modification or synthesis of polymer materials with unique properties (such as epoxy resin, polyester, polycarbonate containing fluorene structure, etc.) and polyimide), non-silver-based photosensitive materials for synthetic electrophotography, intermediates for medicine and pesticides (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/453C07C45/36
Inventor 周建荣胡红
Owner SHANGHAI HUAYI ENERGY CHEM
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