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Synthesis method of 9, 9-di [4-(2-hydroxyethoxy) phenyl] fluorene

A technology of hydroxyethoxy and synthesis method, which is applied in the field of synthesis of 9,9-bis[4-phenyl]fluorene, can solve problems such as high pressure on environmental protection, achieve good product quality, improve atom economy and atom economy good effect

Active Publication Date: 2020-12-29
ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This synthetic route has the advantages of cheap and easy-to-obtain raw materials, simple reaction, and high synthesis yield. Acidic waste, environmental pressure is high

Method used

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  • Synthesis method of 9, 9-di [4-(2-hydroxyethoxy) phenyl] fluorene
  • Synthesis method of 9, 9-di [4-(2-hydroxyethoxy) phenyl] fluorene
  • Synthesis method of 9, 9-di [4-(2-hydroxyethoxy) phenyl] fluorene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]Add 180 grams of 9-fluorenone, 415 grams of phenoxyethanol, 1.8 grams of 3-mercaptopropionic acid, and 540 grams of cyclohexane into a 2-liter reaction bottle, start stirring, add 27 grams of concentrated sulfuric acid dropwise, after the dropwise addition, heat up To reflux, reflux and divide water for 24 hours while reacting, stop the reaction. Add 360 grams of water, cool down and crystallize, stir at 20-30°C for 2 hours, filter, rinse the filter cake with pure water until the pH of the rinse solution is neutral, and dry the filter cake to obtain 9,9-bis[4-( 2-hydroxyethoxy)phenyl]fluorene 412.2 g, yield 94.1%, content 99.2%.

[0038] The crystalline mother liquor obtained by filtration was left standing to separate the water phase, and the organic phase was distilled under normal pressure to obtain 492 g of cyclohexane with a content of 99.7% and a recovery rate of 91.1%. The concentrate was rectified under reduced pressure to obtain 127.1 g of phenoxyethanol with a...

Embodiment 2

[0040] Add 90 grams of 9-fluorenone, 173 grams of phenoxyethanol, 1.8 grams of mercaptoacetic acid, 315 grams of n-heptane, and 9 grams of methanesulfonic acid into a 1-liter reaction bottle, stir and heat up to reflux, and reflux and divide water for 18 hours while reacting. Hours, stopped responding. Add 135 grams of water, cool down and crystallize, stir at 0-10°C for 2 hours, filter, rinse the filter cake with pure water until the pH of the rinse solution is neutral, and dry the filter cake to obtain 9,9-bis[4-( 203.2 g of 2-hydroxyethoxy)phenyl]fluorene, yield 92.8%, content 99.1%.

[0041] The crystalline mother liquor obtained by filtration was left standing to separate the water phase, and the organic phase was distilled under normal pressure to obtain 291.4 g of n-heptane with a content of 99.8% and a recovery rate of 92.5%. The concentrate was rectified under reduced pressure to obtain 31.6 g of phenoxyethanol with a content of 99.1%. After deducting the theoretical...

Embodiment 3

[0043] Add 135 grams of 9-fluorenone, 465 grams of phenoxyethanol, 0.7 grams of 8-mercaptooctanol, 200 grams of methylcyclohexane, and 7 grams of concentrated sulfuric acid into a 2-liter reaction flask, stir and heat up to reflux, and reflux while reacting Divide water for 20 hours, stop the reaction. Add 135 grams of water, cool down and crystallize, stir at 10-15°C for 3 hours, filter, rinse the filter cake with pure water until the pH of the rinse solution is neutral, and dry the filter cake to obtain 9,9-bis[4-( 2-hydroxyethoxy)phenyl]fluorene 310.1 g, yield 94.4%, content 99.2%.

[0044] The crystalline mother liquor obtained by filtration was left standing to separate the water phase, and the organic phase was distilled under normal pressure to obtain 181.8 g of methylcyclohexane with a content of 99.6% and a recovery rate of 90.9%. The concentrate was rectified under reduced pressure to obtain 242.7 g of phenoxyethanol with a content of 99.6%. After deducting the theo...

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Abstract

The invention discloses a synthesis method of 9, 9di [4 -(2-hydroxy ethoxy) phenyl] fluorene, and belongs to the technical field of chemical synthesis. 9-fluorenone, phenoxyethanol, a catalyst and a cocatalyst are stirred and heated to reflux in an alkane solvent, generated water is removed from a reaction solution in an azeotropic manner while reaction is performed, water is added for dilution after the reaction is finished, the mixture is stirred uniformly, cooled, crystallized and filtered, a filter cake is rinsed and dried, and a 9, 9-di [4- (2-hydroxy ethoxy) phenyl] fluorene finished product is obtained; standing and layering the crystallized mother liquor obtained by filtering, removing a water phase, distilling an organic phase to recover the alkane solvent, and rectifying a concentrate to recover phenoxyethanol. The method has the advantages of cheap and easily available raw materials, simple operation, good atom economy, high synthesis yield, good product quality, environmental friendliness and the like, and is suitable for industrial application.

Description

Technical field: [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene. Background technique: [0002] 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene is a very important bisphenol compound. As a functional polymer material monomer, it is mainly used to manufacture High molecular materials such as epoxy resin, polycarbonate, polyarylate, polyether, etc. with excellent optical properties and excellent flame retardancy are widely used in aerospace, electronic appliances, automobile manufacturing and other fields. For example, polycarbonate synthesized with 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene as a monomer has excellent optical properties and is used to manufacture high-end resin lenses; 9,9- Bis[4-(2-hydroxyethoxy)phenyl]fluorene is an epoxy resin synthesized as a monomer. As a packaging material, it is widely used in the fields of display screen production and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/30C07C41/40C07C43/23
CPCC07C41/30C07C41/40C07C2603/18C07C43/23
Inventor 袁其亮蒋栋栋万应石永根徐鹏飞陈海峰
Owner ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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