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Method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene

A technology of hydroxyethoxy and phenyl, which is applied in the field of preparation of 9,9-bis[phenyl]fluorene, can solve the problem of high cost and achieve the effects of less waste, high reaction yield and convenient recycling

Active Publication Date: 2014-09-10
ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Although this synthetic route has better reaction yield and fewer wastes, the cost is higher due to the use of triphenylphosphine

Method used

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  • Method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene
  • Method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene
  • Method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 18 grams of 9-fluorenone, 31 grams of ethylene glycol monophenyl ether, and 0.1 grams of 3-mercaptopropionic acid into a 500 ml stainless steel reaction kettle, seal the reaction kettle, test the pressure with nitrogen, and replace it with nitrogen after confirming that the reaction kettle is well sealed System twice, cool the reactor to -40~-50°C, slowly feed anhydrous hydrogen fluoride gas to condense hydrogen fluoride into liquid in the reactor, until the weight of the reactor increases by 180 grams, stop feeding hydrogen fluoride. The temperature of the reaction kettle was raised to 60-70° C. for 20 hours. Cool the reaction system to 40-50°C, slowly open the exhaust valve to discharge the hydrogen fluoride gas, the hydrogen fluoride gas is condensed by the condenser and then recovered, after the hydrogen fluoride in the system is basically discharged, nitrogen gas is introduced into the reaction kettle to drive the remaining hydrogen fluoride out, stop nitrogen....

Embodiment 2

[0028] Add 25 grams of 9-fluorenone, 57.5 grams of ethylene glycol monophenyl ether, and 0.7 grams of 2-mercaptopropionic acid into a 500 ml stainless steel reactor, seal the reactor, test the pressure with nitrogen, and replace it with nitrogen after confirming that the reactor is well sealed System twice, cool the reactor to -20~-30°C, slowly feed anhydrous hydrogen fluoride gas to condense the hydrogen fluoride into a liquid in the reactor, until the weight of the reactor increases by 150 grams, stop feeding hydrogen fluoride. The temperature of the reaction kettle was raised to 80-90° C. for 15 hours. Cool the reaction system to 30-40°C, slowly open the exhaust valve to discharge the hydrogen fluoride gas, the hydrogen fluoride gas is condensed by the condenser and then recovered, after the hydrogen fluoride in the system is basically discharged, argon gas is introduced into the reaction kettle to remove the remaining hydrogen fluoride Drive out, stop argon. Slowly add 60...

Embodiment 3

[0030] Add 10 grams of 9-fluorenone, 30.7 grams of ethylene glycol monophenyl ether, and 0.5 grams of mercaptoacetic acid into a 250 ml stainless steel reactor, seal the reactor, test the pressure with nitrogen, and replace the system twice with nitrogen after confirming that the reactor is well sealed , Cool the reactor to -50~-60°C, slowly feed anhydrous hydrogen fluoride gas to condense hydrogen fluoride into a liquid in the reactor, and stop feeding hydrogen fluoride until the reactor increases in weight by 150 grams. The temperature of the reaction kettle was raised to 110-120° C. for 10 hours. Cool the reaction system to 50-60°C, slowly open the exhaust valve to discharge the hydrogen fluoride gas, the hydrogen fluoride gas is condensed by the condenser and then recovered, after the hydrogen fluoride in the system is basically discharged, nitrogen gas is introduced into the reaction kettle to drive out the remaining hydrogen fluoride out, stop nitrogen. Slowly add 50 gr...

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Abstract

The invention discloses a method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene and belongs to the technical field of chemical synthesis. The method is characterized by comprising the following steps: reacting 9-fluorenone and ethylene glycol monophenyl ether in hydrogen fluoride in the presence of a promoter to obtain 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene; at the end of the reaction, evaporating to reclaim hydrogen fluoride from the reaction system, diluting residues with alkaline liquid; extracting, washing and re-crystallizing to obtain 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene. The method has the advantages of use of low-price and easily available raw materials, high reaction yield, convenience in acid catalyst reclamation, generation of less 'three waste', environmental friendliness and the like, and has a high industrial application value.

Description

Technical field: [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of 9,9-bis[(4-hydroxyethoxy)phenyl]fluorene. Background technique: [0002] 9,9-bis[(4-hydroxyethoxy)phenyl]fluorene is an important bisphenol compound, which can be used to prepare epoxy resins, polyurethanes with high heat resistance, excellent optical properties and excellent flame retardancy Polycondensation products such as polycarbonate, polyester, polyarylate, polyether or polyether are widely used in military, aerospace, electronics, automobile industries and other fields such as aircraft structural materials, missile warheads, engine nozzles and housings. In recent years, resin materials prepared from 9,9-bis[(4-hydroxyethoxy)phenyl]fluorene have been widely used in the manufacture of high-end mobile phone displays, and are developing towards high-end liquid crystal displays. With the widespread use of smart phones, the marke...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/30
CPCY02P20/584C07C41/30C07C2603/18
Inventor 袁其亮鲍张丰张佳炳施正军陈寅镐王超
Owner ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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