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Preparing method of dihydroxyethyl bisphenol fluorene ether

A technology of bishydroxyethyl bisphenol fluorene ether and bisphenol fluorene, which is applied in the field of fine chemical synthesis, can solve the problems of high toxicity of solvents, and achieve the effects of increased reaction yield, less by-products, and easy recovery

Active Publication Date: 2019-04-19
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process can obtain bisphenol A polyether with higher purity and better color, the solvent it uses is more toxic

Method used

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  • Preparing method of dihydroxyethyl bisphenol fluorene ether
  • Preparing method of dihydroxyethyl bisphenol fluorene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 350g of bisphenol fluorene, 0.219g of triisopropylphosphine catalyst (the mass of the catalyst is 0.5‰ of the sum of the mass of bisphenol fluorene and ethylene oxide, the same below) and 140g Cyclohexane (40% of bisphenol fluorene mass), start stirring, vacuumize with vacuum pump, use N 2 Replace the air in the reactor. After three replacements, when the vacuum degree is ≥-0.095MPa, turn off the vacuum and start

[0038] Raise the temperature to dissolve the bisphenol fluorene and the catalyst in the solvent. When the temperature rises to 100°C, a small amount of ethylene oxide begins to pass through, and when the temperature rises to the reaction temperature of 120°C, the ethylene oxide begins to pass through stably, and continues to pass through the epoxy 88g of ethane, the reaction temperature is controlled at 120~125°C, the pressure of the reactor is controlled below 0.4MPa, after adding ethylene oxide, heat preservation and aging until the pressure in the reac...

Embodiment 2

[0041] Add 350g of bisphenol fluorene, 0.438g of triisopropylphosphine catalyst (1‰ catalyst) and 140g of cyclohexane (40% of the mass of bisphenol fluorene) in sequence in a stirring 2.5L reactor, and start stirring. Evacuate with a vacuum pump, using N 2Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up when the vacuum degree is ≥-0.095MPa, so that the bisphenol fluorene and the catalyst are dissolved in the solvent. When the temperature rises to 100°C, start to pass a small amount of ethylene oxide Alkanes, when the temperature rises to the reaction temperature of 120°C, start to pass ethylene oxide stably, continue to feed 88g of ethylene oxide, control the reaction temperature at 120~125°C, control the pressure of the reactor below 0.4MPa, and finish adding epoxy After heating with ethane, heat preservation and aging until the pressure in the reactor no longer drops. Then the temperature drops to about 105°C and starts nega...

Embodiment 3

[0044] Add 350g of bisphenol fluorene, 1.341g of triisopropylphosphine catalyst (3‰ catalyst) and 140g of cyclohexane (40% of the mass of bisphenol fluorene) in sequence in a stirring 2.5L reactor, and start stirring. Evacuate with a vacuum pump, using N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up when the vacuum degree is ≥-0.095MPa, so that the bisphenol fluorene and the catalyst are dissolved in the solvent. When the temperature rises to 100°C, start to pass a small amount of ethylene oxide Alkanes, when the temperature rises to the reaction temperature of 120°C, start to pass ethylene oxide stably, continue to feed 97g of ethylene oxide, control the reaction temperature at 120~125°C, control the pressure of the reactor below 0.4MPa, and finish adding epoxy After heating with ethane, heat preservation and aging until the pressure in the reactor no longer drops. Then the temperature drops to about 105°C and starts neg...

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Abstract

The invention belongs to the technical field of fine chemical synthesis, and particularly relates to a preparing method of dihydroxyethyl bisphenol fluorene ether. The preparing method of dihydroxyethyl bisphenol fluorene ether comprises the following steps of 1, putting and replacement of nitrogen, wherein bisphenol fluorene, a triisopropylphosphine catalyst and a solvent are added into a reaction still in sequence, stirring is started, vacuumizing is conducted under N2 protection, and after replacement is repeatedly conducted several times until the vacuum degree is larger than or equal to minus 0.095 MPa, temperature rise begins; 2, reactions, wherein when the temperature in the reaction still is increased to 100 DEG C, a small amount of oxirane begins to be introduced, after the temperature rises to the reaction temperature, oxirane begins to be stably introduced, the pressure of the reaction still is controlled to be within 0.4 MPa, after adding of oxirane is finished, and the reactions continue at preserved temperature and preserved temperature and are finished until the pressure is not reduced; 3, desorption of the solvent, wherein after curing is finished, cooling is conducted for solvent desorption at negative pressure; 4, discharging, wherein the temperature is reduced to 80 DEG C, 30 min after degassing, discharging begins to obtain a dihydroxyethyl bisphenol fluorene ether product with the content larger than 98%.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a preparation method of bishydroxyethyl bisphenol fluorene ether. Background technique [0002] Bisphenol fluorene is a bisphenol compound with Cardo skeleton structure prepared by condensation reaction of pentanone and phenol as raw materials under the action of a catalyst. The structural formula is as follows: [0003] [0004] Bisphenol fluorene is a new type of organic chemical raw material with high stability. Due to its unique Cardo ring, it can improve the heat resistance of the polymer and has good optical properties and formability, excellent transparency and high refractive index. Therefore, it has become a raw material or modifier for the synthesis of new polycarbonates, epoxy resins, polyesters, and polyethers, and is widely used in military, aerospace, electronics, and automotive industries such as aircraft structural materials and miss...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/23
CPCC07C41/03C07C2603/18C07C43/23
Inventor 张雨金一丰马定连余江
Owner ZHEJIANG HUANGMA TECH
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