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Bisphenol fluorene synthesizing process catalyzed with solid magnetic super acid

A solid superacid and bisphenol fluorene technology, which is applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as large mass transfer resistance, small reaction interface, and difficult separation of catalysts and products , to achieve the effect of reducing pollution, mild reaction conditions, and reasonable and feasible synthesis process

Inactive Publication Date: 2007-06-27
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the application of solid superacid catalysts has disadvantages such as difficult separation of catalyst and product, small reaction interface, and large mass transfer resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix 2 g of fluorenone, 8.355 g of phenol, 0.2 ml of β-mercaptopropionic acid, and 1.15 g of magnetic solid superacid SO 4 2- / Fe 3 o 4 -ZrO 2 The catalyst is added in turn to a three-necked flask with a reflux condenser and a thermometer and stirred. The reaction temperature is 100°C and the reaction time is 11.5 hours. The magnetic solid superacid is deposited at the bottom of the flask by magnetic separation, and the reaction mixture is poured into the flask while it is hot. In the beaker, rinse the three-necked flask with 50 milliliters of hot methanol, and transfer it to the beaker, then add 300 milliliters of distilled water, cool to room temperature, precipitate crystals, filter, recrystallize the filter cake with acetone, filter, dry, and finally obtain white crystals, bis The yield of phenol fluorene is 93.4%, and the purity reaches 99.2%.

Embodiment 2

[0017] Mix 2 g of fluorenone, 10.44 g of phenol, 0.2 ml of β-mercaptopropionic acid, and 1.15 g of magnetic solid superacid SO 4 2- / Fe 3 o 4 -TiO 2 The catalyst was sequentially added into a three-necked flask with a reflux condenser and a thermometer. The reaction process and conditions were the same as in Example 1, except that the solvent used for recrystallization was changed to toluene. The final yield of bisphenol fluorene was 90.7%, and the purity reached 99.1%.

[0018] According to the method disclosed in the invention, the synthesis process flow of bisphenol fluorene is reasonable and feasible, the aftertreatment is simple, the catalyst is convenient to recover, the product yield is high, and the problems of metal corrosion and environmental pollution are solved.

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Abstract

The bisphenol fluorine synthesizing process includes mixing phenol, 9-fluorenone, solid magnetic super acid and mercapto carboxylic acid, with phenol / 9-fluorenone molar ratio of 6-12 to 1, mercapto carboxylic acid / 9-fluorenone weight ratio of 0.02-0.50 to 1 and solid magnetic super acid accounting for 5-15.0 % of total reactant weight, to react at 80-110 deg.c via stirring for 6-16 hr; magnetically separating after reaction to adsorb solid magnetic super acid to the bottom of reactor, transferring the hot reaction product to some container, washing the reactor with hot water solution of methanol, transferring the washed liquid to the container, cooling the container to separate out crystal, filtering, drying, recrystallizing the filter cake in organic solvent and stoving to obtain bisphenol fluorine crystal. The present invention has mild reaction condition and product purity as high as 99.2 %, and may be used widely in the phenol and 9-fluorenone condensation reaction.

Description

(1) Technical field [0001] The invention relates to the field of organic synthesis and materials, in particular to a method for catalytically synthesizing bisphenol fluorene with a magnetic solid superacid. (2) Background technology [0002] Bisphenol fluorene is a kind of fluorenyl compound containing phenolic hydroxyl structure. It is an important monomer for the synthesis of polycondensation products such as polycarbonate, epoxy resin, polyester or polyether. It is a new type of heat-resistant material synthesized from bisphenol fluorene Epoxy resin, polycarbonate and other materials have good thermal stability, high transparency, high refractive index and easy solubility, and can be used to prepare transparent conductive films, alignment films, gas separation films, photoreceptors with photoelectric properties, high Performance polymers, photoconductors, heat transfer materials, flame retardant thermoplastic resins, optical discs, radiation-resistant polymers with high t...

Claims

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Application Information

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IPC IPC(8): C07C37/20C07C39/17B01J27/055C08G8/02
CPCY02P20/52
Inventor 刘文彬王军嵇雷邱祺浩
Owner HARBIN ENG UNIV
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