Preparation method of dihydroxy oxethyl fluorene

A technology of bishydroxyethoxyfluorene and fluorenone, which is applied in the field of preparation of bishydroxyethoxyfluorene, can solve the problems of long reaction time, high reaction temperature, and increased cost, and achieve improved crystal form, fluidity, and process Simplified operation and beneficial effect of recycling

Inactive Publication Date: 2013-04-24
常州市正锋光电新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Concentrated sulfuric acid method is the traditional production method of bisphenol fluorene; the highest yield can reach 70% when heteropoly acid is used as catalyst, and 82.6% for ion exchange resin. Secondly, the reaction of commonly used catalysts is more than 10 hours, so that bisphenol The production cycle of fluorene is quite long, thus adding more cost
Finally, the reaction temperature is relatively high. The temperatur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Synthesis of BPEF.

[0021] Add 18g of fluorenone (0.1mol) with a content of 99% or more (HPLC), 50g of ethylene glycol monophenyl ether (0.36mol) with a content of 99% or more (GC), and 1g of mercaptoethanol (0.0128mol) in a 250ml flask. Stir for 0.5 hours, then add 35g of concentrated sulfuric acid with a content of 98% dropwise at 65-70°C within 3 hours. The combined organic layers were extracted twice with hydrocarbons, cooled to 0-5°C, crystallized, filtered and dried to obtain 41g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a yield of 93.5%, and a content of 98.2 %about.

Embodiment 2

[0022] Example 2: Synthesis of BPEF.

[0023] Add 18g of fluorenone (0.1mol) with a content of 99% or more (HPLC), 45g of ethylene glycol monophenyl ether (0.36mol) with a content of 99% or more (GC), and 0.9g of mercaptoethanol in a 250ml flask. Stir for 0.5-2 hours, then add 37g of concentrated sulfuric acid with a content of 98% dropwise at 60-70°C within 2.5 hours. The combined organic layer was extracted twice with alkanes and other halogenated hydrocarbons, cooled to 0-5°C, crystallized, filtered and dried to obtain 42g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a yield of 95.7% , the content is about 98.4%.

Embodiment 3

[0024] Example 3: Purification of BPEF.

[0025] Get 20g of the product obtained in Example 2, recrystallize twice with 60ml of ethylene dichloride, and filter and dry to obtain 18.8g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a purity of 99.8%.

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PUM

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Abstract

The invention belongs to the field of chemical synthesis, and relates to a preparation method of dihydroxy oxethyl fluorine. The method comprises the following steps of: executing condensation reaction of ethylene glycol monophenyl ether and 9-fluorenone in the presence of catalyst mercaptoethanol, extracting and purifying the reaction liquid by water-organic solvent, and then, obtaining the target product after recrystallization. With the preparation method provided by the invention, the reaction time is reduced, the yield is improved, the crystal form and the liquidity of products are improved, the solvent of a single type is more beneficial for recycling, and the technical operation is simplified, so that the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of bishydroxyethoxyfluorene. Background technique [0002] In the modern polymerization processing industry, bisphenol compounds are widely used in condensation reactions, especially for the preparation of epoxy resins, polyurethanes, polycarbonates, Polycondensation products such as polyester, polyarylate, polyether or polyether, bisphenol fluorene compound and its substituted derivatives such as bishydroxyethoxy fluorene are important monomers for the synthesis of the above polymers. Bisphenol fluorene compounds and their substituted derivatives are widely used in military, aerospace, electronics, and automotive industries such as aircraft structural materials, missile warheads, engine nozzles, and housings. The resulting polymers can be used as heat-resistant materials , separation membrane materials and optical materials, etc. [0003] Elec...

Claims

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Application Information

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IPC IPC(8): C07C41/30C07C43/23C07C41/38C07C41/40
Inventor 徐小虎唐华
Owner 常州市正锋光电新材料有限公司
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