Method for synthesizing bisphenol fluorine by catalysis of highly acidic cation exchange resin

A strong acid cation, cation exchange technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as equipment corrosion, expensive corrosion-resistant materials, environmental hazards, etc. Simple and effective in solving metal corrosion problems and environmental pollution problems

Inactive Publication Date: 2007-07-25
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] Add 4.5 grams of fluorenone, 18.8 grams of phenol, 0.2 ml of β-mercaptopropionic acid, and 3.5 grams of DOWEX DR 2030 type strongly acidic cation exchange resin into a three-necked flask with a stirrer and a thermometer in sequence, start stirring, and the reaction temperature is 100°C , the reaction time was 6 hours, the reaction mixture was filtered while it was hot, the catalyst was recovered, the filtrate was washed with aqueous methanol, crystallization was precipitated, filtered with suction, dried, and recrystallized with toluene, filtered, and vacuum-dried to obtain 6.50 g of bisphenol fluorene, with a yield of 76.6% , purity 99.8%, elemental analysis results: carbon content is 85.51% (theoretical value 85.61%), hydrogen content is 5.21% (theoretical value 5.18%).

Embodiment 2

[0018] Except that the catalyzer is changed to NKC-9 type strongly acidic cation exchange resin, the reaction time is 9 hours, and recrystallization adopts isopropanol as a solvent, and other conditions are the same as in Example 1, and finally 6.3 grams of bisphenol fluorene are obtained, with a yield of 74.2%. 99.3% purity.

Embodiment 3

[0020] The catalyst recovered in Example 1 is activated with 5% hydrochloric acid solution, then reacted according to the reaction conditions and operation process of Example 1, and finally obtains 6.38 grams of bisphenol fluorene product, with a purity of 99.7%, and the yield of bisphenol fluorene was 75.2%. Repeat the test for 4 more times according to the above process, and the test results are listed in Table 1.

[0021] Table 1 Catalyst repeatability test result

[0022] repeat times

[0023] It can be seen from the results in the table that the cation exchange resin has high catalytic activity and can be reused many times. Therefore, the cost of the catalyst can be greatly reduced, the serious corrosion of equipment and the neutralization treatment steps of waste acid can be solved, and the impact on the environment can be reduced. pollute.

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PUM

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Abstract

This invention discloses a method for synthesizing biphenol fluorine by using strongly acidic cation exchange resin as catalyst. The method comprises: adding phenol, 9-fluorenone, strongly acidic cation exchange resin, and mercapto carboxylic acid into a container, reacting at 80-120 deg.C under stirring for 4-15 h, filtering after reaction, recovering the catalyst, adding methanol aqueous solution into the filtrate, precipitating the crystals, vacuum-filtering to obtain crude biphenol fluorene, recrystallizing with organic solvent, filtering, and vacuum-drying to obtain white biphenol fluorene crystals with a purity up to 99.8%. The phenol/9-fluorenone mol ratio is (6-15):1. The cation exchange resin is 5-30 wt. % of the reactants. The post-treatment is simple, thus solving the problems of metal corrosion and environmental pollution. Besides, the catalyst can be recycled.

Description

(1) Technical field [0001] The invention relates to the field of organic synthesis and materials, in particular to a technical method for synthesizing bisphenol fluorene. (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 temperature resistance, thermoplastic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/20C07C39/17B01J31/08
CPCY02P20/584
Inventor 王军刘文彬邱琪浩高庆平稽雷
Owner HARBIN ENG UNIV
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