Method for synthesizing dihydroxypropyl bisphenol A ether through one-step process

A technology of bishydroxypropyl bisphenol and step method, applied in the field of organic compound synthesis, can solve the problems of poor quality, high content of by-products, isomerization of propylene oxide and the like

Active Publication Date: 2014-03-19
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the method of the patent "201210003017.3 (application number)" is not suitable for the synthesis of bisphenol A propoxylation because: firstly, the catalytic activity of the catalyst trialkylamine is low, and the reactivity of propylene oxide is weaker than that of ethylene oxide. The amount of catalyst required is large, the reaction cycle is too long, and propylene oxide is prone to isomerization into propylene alcohol or other by-products; secondly, the temperature required for the reaction is too high, and propylene oxide is also prone to isomerization in

Method used

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  • Method for synthesizing dihydroxypropyl bisphenol A ether through one-step process
  • Method for synthesizing dihydroxypropyl bisphenol A ether through one-step process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 684g of bisphenol A and 1.0g of 1,1'-bis(diphenylphosphino)ferrocene into the reaction kettle, vacuumize with a vacuum pump, and use N 2 Replace the air in the reactor. After three replacements, the vacuum degree ≥ -0.096MPa, N 2 Under protection, turn off the vacuum and heat up the material; when the bisphenol A is completely melted, vacuumize at this temperature for 20 minutes, after removing the low boiling point substances, continue to add 348g of propylene oxide, and control the reaction temperature at 160-165°C , The pressure inside the reactor is -0.04~0.3Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops; after the reaction is completed, cool down to 100°C and use vacuum degassing for 20 minutes, then discharge to obtain the finished product.

[0027] The product was analyzed by liquid chromatography: the content of propylene alcohol by-products was 0.003%, and the bishydroxypropyl bisphenol A ether was 99.5%. The...

Embodiment 2

[0029] Add 684g of bisphenol A and 0.5g of 1,1'-bis(diphenylphosphino)ferrocene into the reaction kettle, vacuumize with a vacuum pump, and use N 2 Replace the air in the reactor. After three replacements, the vacuum degree ≥ -0.096MPa, N 2 Under protection, turn off the vacuum, and raise the temperature to carry out the compounding; when the bisphenol A is completely melted, vacuumize at this temperature for 20 minutes, after removing the low boiling point substances, continue to add 355g of propylene oxide, and control the reaction temperature at 165-170°C , The pressure inside the reactor is -0.04~0.3Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops; after the reaction is completed, cool down to 100°C and use vacuum degassing for 20 minutes, then discharge to obtain the finished product.

[0030]The product was analyzed by liquid chromatography: the by-product content of propylene alcohol was 0.004%, and the bishydroxypropyl bis...

Embodiment 3

[0032] Add 684g of bisphenol A and 0.3g of 1,1'-bis(diphenylphosphino)ferrocene into the reaction kettle, vacuumize with a vacuum pump, use N 2 Replace the air in the reactor. After three replacements, the vacuum degree ≥ -0.096MPa, N 2 Under protection, turn off the vacuum, and heat up the material; when the bisphenol A is completely melted, vacuumize at this temperature for 20 minutes, after removing the low boiling point substances, continue to add 420g of propylene oxide, and control the reaction temperature at 170-175°C , The pressure inside the reactor is -0.04~0.3Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops; after the reaction is completed, cool down to 100°C and use vacuum degassing for 20 minutes, then discharge to obtain the finished product.

[0033] The product was analyzed by liquid chromatography: the content of propylene alcohol by-products was 0.005%, and the bishydroxypropyl bisphenol A ether was 99.2%; the co...

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Abstract

The invention relates to a method for synthesizing dihydroxypropyl bisphenol A ether through a one-step process, and belongs to the technical field of organic compound synthesis. The method comprises the steps of: by taking bisphenol A as the raw material, orderly carrying out material melting and synthesis by adding a chain extension agent, and finally obtaining the dihydroxypropyl bisphenol A ether, wherein the hydroxyl value of the dihydroxypropyl bisphenol A ether is 325-330mgKOH/g, and the color of the dihydroxypropyl bisphenol A ether is smaller than No.30. The technical scheme of the method is used for synthesizing the product through the one-step process, and the problems of complex preparation process, many process steps, high energy consumption, high composite cost, poor product quality and so on in the conventional technology are solved; the obtained product is rational in distribution, low in product color; and the content of the by-product allyl alcohol matters is low.

Description

technical field [0001] The invention relates to a method for synthesizing bishydroxypropyl bisphenol A ether in one step, and belongs to the technical field of organic compound synthesis. Background technique [0002] Bishydroxypropyl bisphenol A ether is a white solid, which can be applied to UV coatings with 5E characteristics, 5E are 1.Efficient (high efficiency), 2.Enabling (wide adaptability), 3.Economical (economical), 4.Energy Saving (energy saving), 5.Environmental Friendly (environmentally friendly), known as a new green industrial technology for the 21st century. It reacts with acrylic acid or methacrylic acid and is used as a functional diluent for UV coatings. It not only dissolves and dilutes oligomers, adjusts the viscosity of the system, but also participates in photopolymerization, affecting the photocuring speed of the coating and various properties of the cured film. Various properties, such as hardness, wear resistance, adhesion, flexibility and other phy...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/03
CPCC07C41/03C07C43/23
Inventor 马定连金一丰王胜利张敏张月江黄远远
Owner ZHEJIANG HUANGMA TECH
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