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Bisphenol fluorene synthesizing process catalyzed with solid supported heteropolyacid

A technology for immobilizing heteropolyacids and bisphenol fluorene, applied in chemical instruments and methods, preparation of organic compounds, catalyst carriers, etc., can solve problems such as expensive corrosion-resistant materials, equipment corrosion, environmental hazards, etc., and achieve product yield High efficiency, mild process reaction conditions, and convenient recovery

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

Since hydrochloric acid is used as a catalyst in the reaction process, the biggest disadvantage is that the equipment is severely corroded, and the production equipment requires expensive corrosion-resistant materials. The production process produces a large amount of waste acid, which needs to be neutralized, and the large amount of waste water produced is also harmful to the environment. harm

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 2 grams of fluorenone, 10.44 grams of phenol, 0.2ml of β-mercaptopropionic acid, 2.19 grams of immobilized 12-phosphotungstic acid (molecular formula is H 3 PW 12 o 40 ) catalysts were added in turn to a three-necked flask with a reflux condenser and a thermometer and stirred, the carrier was activated carbon, the mass ratio of 12-phosphotungstic acid to activated carbon was 0.6:1, the reaction temperature was 95°C, and the reaction time was 12 hours. The mixture was filtered while it was hot, washed with aqueous methanol to precipitate crystals, filtered, dried, recrystallized with acetone, and dried in vacuo to obtain bisphenol fluorene crystals. The yield of bisphenol fluorene was 72.5%, and the purity could reach 99.8%.

Embodiment 2

[0018] The heteropolyacid in the immobilized catalyst of this embodiment is 12-phosphomolybdic acid (molecular formula is H 3 PMo 12 o 40 ), other conditions are the same as Example 1, and the yield of bisphenol fluorene is 51.5%, and the purity reaches 99.4%.

Embodiment 3

[0020] The carrier of this example is ZSM-5 molecular sieve, other conditions are the same as Example 1, the yield of bisphenol fluorene is 66.8%, and the purity reaches 99.5%.

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PUM

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Abstract

The bisphenol fluorine synthesizing process includes mixing phenol, 9-fluorenone, solid supported heteropoly acid and mercapto carboxylic acid, with phenol / 9-fluorenone molar ratio of 6-14 to 1, solid supported heteropoly acid accounting for 5.0-20.0 % of total reactant weight, heteropoly acid / solid carrier weight ratio of 0.3-1 to 1 and mercapto carboxylic acid / 9-fluorenone weight ratio of 0.02-0.50 to 1, to react at 60-130 deg.c via stirring for 6-14 hr; filtering the reacted product while it is still hot, and recovering the catalyst; washing the catalyst, merging the washed liquid with the filtrate, crystallizing, filtering, drying, recrystallizing in organic solvent and vacuum drying to obtain bisphenol fluorine crystal. The present invention has product purity as high as 99.8 %, simple post-treatment, less metal corrosion and environmental pollution and recovery of catalyst, 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 solid-loaded heteropolyacid. (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 hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/20C07C39/17B01J27/188B01J23/24B01J32/00B01J29/06C08G8/02
CPCY02P20/52
Inventor 刘文彬王军嵇雷邱祺浩王承洋闵龙吴明清
Owner HARBIN ENG UNIV
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