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Preparation method for bisphenol fluorene

A technology of bisphenol fluorene and fluorenone, which is applied in the field of preparation of bisphenol fluorene, can solve the problems of co-catalysts with foul odor, air pollution, and worker poisoning, and achieve the effects of good product quality, simple process, and mild reaction conditions

Inactive Publication Date: 2014-05-28
常州市正锋光电新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention overcomes the deficiencies in the prior art that the cocatalyst used in the preparation method of bisphenol fluorene has a foul smell and is highly toxic, pollutes the air and causes poisoning of workers, and provides a preparation method of bisphenol fluorene

Method used

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  • Preparation method for bisphenol fluorene

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Embodiment

[0011] Add 100g of 9-fluorenone, 350g of phenol, and 0.5g of cysteamine into a 1000ml four-neck flask, heat up to 50°C under stirring and dissolve completely, cool to below 30°C, slowly add 28g of 98% sulfuric acid dropwise, and heat up to 55°C after dropping Keep stirring at ℃ for 6 hours, add 150ml of water, neutralize with liquid caustic soda to pH 6-7, separate the desalinated layer, recover phenol from the oil layer under reduced pressure, and recrystallize with ethanol and water mixed solvent to obtain white crystals, which can be obtained after drying. Phenolfluorene 175g, yield 90%, content 98.9%. The final product 1 HNMR spectrum as figure 1 Shown, show that the product finally obtained by this method is bisphenol fluorene.

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Abstract

A technical solution adopted by the invention is a preparation method for bisphenol fluorine. The preparation method comprises the following steps of adding phenol, 9-fluorenone and cysteamine into a container, a molar ratio of phenol to 9-fluorenone being 4-10 :1; dropwise adding concentrated sulfuric acid with stirring at a temperature of 30 DEG C; reacting for 3-12 hours with stirring under a temperature of 50-60 DEG C after the concentrated sulfuric acid is completely added; adding a proper amount of water after the reaction; neutralizing with liquid caustic soda; separating an oil layer for recovering phenol; and then recrystallizing with a mixed solvent of ethanol and water. The preparation method is mild in reaction conditions and simple in process; cysteamine is safe and has no smell during the use process, and can not cause worker poisoning or air pollution; a product has high quality and high yield; and the preparation method has high economical efficiency and is suitable for large-scale production. The product is determined by nuclear magnetic resonance.

Description

technical field [0001] The invention belongs to the field of chemical preparation, in particular to a preparation method of bisphenol fluorene. Background technique [0002] Bisphenol fluorene is a bisphenol compound with a Cardo skeleton structure prepared by condensation reaction of fluorenone and phenol as raw materials in the presence of an acidic catalyst. According to the different catalysts used, the methods for preparing bisphenol fluorene in the prior art can be mainly divided into sulfuric acid method, hydrogen chloride method and mercaptosulfonic acid method. [0003] Among them, the sulfuric acid method is relatively simple in process flow and high in yield. However, mercaptocarboxylic acid is commonly used as a cocatalyst, and mercaptocarboxylic acid has a foul smell and is highly toxic, which brings a lot of discomfort and air pollution to production personnel, threatens the health of production personnel, and seriously causes poisoning of workers. Contents ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/17C07C37/20
CPCC07C37/20C07C2603/18
Inventor 徐小虎
Owner 常州市正锋光电新材料有限公司
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