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Method for preparing bis(hydroxyethyl) bisphenol A ether

A bis-hydroxyethyl bisphenol and a certain amount of technology are applied in the field of organic compound synthesis, and can solve the problems of easy isomerization of propylene oxide, weak reaction activity, long reaction period and the like, and achieve light product color and reaction period. Short, reduced by-product formation effect

Inactive Publication Date: 2015-03-04
ZHEJIANG LYUKEAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent is not applicable to the synthesis of bisphenol A propoxylation: firstly, the catalyst trialkylamine has low catalytic activity, and propylene oxide is weaker than ethylene oxide in reactivity, the amount of catalyst required is large, and the reaction cycle is too long. Propylene oxide is prone to isomerization into propylene alcohol or other by-products; secondly, if the temperature required for the reaction is too high, propylene oxide is also prone to isomerization reaction into by-product propylene alcohol or allyl alcohol, and the product propylene alcohol The content is above 0.1%

Method used

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  • Method for preparing bis(hydroxyethyl) bisphenol A ether
  • Method for preparing bis(hydroxyethyl) bisphenol A ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 700g of bisphenol A, 2.0g of composite catalyst (1.8g of 1,1'-bis(diphenylphosphine) ferrocene, 0.2g of solid NaOH) into the reaction kettle, vacuumize with a vacuum pump, and use N 2 After replacing the air in the reactor for three times, turn off the vacuum and start to heat up at a vacuum degree ≥ -0.096MPa. The temperature rises to 160°C, and after vacuum degassing for 10 minutes, continue to add 300g of ethylene oxide, control the reaction temperature at 165°C-170°C, and the pressure in the reactor at -0.04 MPa-0.3MPa. After the addition, keep warm and continue the reaction. until the pressure no longer drops. After the reaction is completed, the temperature is lowered to 100°C and vacuum degassed for 20 minutes, then neutralized by adding 0.2g of glacial acetic acid, then cooled to 80°C and discharged to obtain the finished product. The product was analyzed by liquid chromatography: the residual bisphenol A was <1ppm, the content of monohydroxyethyl bisphenol...

Embodiment 2

[0039] Add 700g of bisphenol A, 5.0g of composite catalyst (4.7g of 1,1'-bis(diphenylphosphine) ferrocene, 0.3g of solid potassium carbonate) into the reaction kettle, vacuumize with a vacuum pump, and use N 2 After replacing the air in the reactor for three times, turn off the vacuum and start to heat up at a vacuum degree ≥ -0.096MPa. The temperature rises to 160°C, and after vacuum degassing for 10 minutes, continue to add 278g of ethylene oxide, control the reaction temperature at 155°C-165°C, and the pressure in the reactor at -0.02 MPa-0.2MPa. 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 vacuum degas for 20 minutes, then add 0.3g of glacial acetic acid for neutralization, then cool down to 80°C and discharge to obtain the finished product. The product was analyzed by liquid chromatography: the residual bisphenol A was <1ppm, the content of monohydroxyethyl bisphenol A...

Embodiment 3

[0041] Add 700g of bisphenol A, 1.5g of composite catalyst (1.35g of 1,1'-bis(diphenylphosphine)ferrocene, 0.15g of solid potassium methoxide) into the reaction kettle, vacuumize with a vacuum pump, and use N 2 After replacing the air in the reactor for three times, turn off the vacuum and start to heat up at a vacuum degree ≥ -0.096MPa. The temperature rises to 160°C, and after vacuum degassing for 10 minutes, continue to add 290g of ethylene oxide, control the reaction temperature at 160°C-165°C, and the pressure in the reactor at 0.0 MPa-0.4MPa. After the addition, keep warm and continue the reaction until until the pressure no longer drops. After the reaction is completed, the temperature is lowered to 100°C and vacuum degassed for 20 minutes, then neutralized by adding 0.15g of glacial acetic acid, then cooled to 80°C and discharged to obtain the finished product. The product was analyzed by liquid chromatography: the residual bisphenol A was <1ppm, the content of monohy...

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Abstract

The invention relates to a method for preparing bis(hydroxyethyl) bisphenol A ether. The method comprises the following steps: (1) washing a high-pressure reaction kettle with distilled water for several times, and cooling to room temperature for later use; (2) adding bisphenol A and a compound catalyst, vacuumizing to replace air, closing vacuum and beginning to warm when the vacuum degree is greater than or equal to -0.096MPa; (3) heating to 160 DEG C, carrying out vacuum degassing for 10 minutes, lastingly adding ethylene oxide, controlling the reaction temperature to be 150-175 DEG C and the pressure in the reaction kettle to be -0.05MPa to 0.5MPa, carrying out heat preservation after adding is ended, and further reacting until the pressure is not lowered more; and (4) cooling to 100 DEG C after reaction is ended, and carrying out vacuum degassing for 20 minutes, adding a certain amount of glacial acetic acid for neutralizing, cooling to 80 DEG C and emptying to obtain the finished product. The content of bis(hydroxyethyl) bisphenol A ether is greater than or equal to 95.0%; the content of mono-hydroxyethyl bisphenol A ether is smaller than or equal to 0.05%; the residual bisphenol A is smaller than or equal to 3ppm; the hydroxyl value is 350-355mgKOH / g; and the color and luster are 0-30# (Pt-Co unit).

Description

technical field [0001] The invention relates to a preparation method of bishydroxyethyl bisphenol A ether, which belongs to the technical field of organic compound synthesis. Background technique [0002] Bishydroxyethyl 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 physical and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/03
CPCC07C41/03C07C43/23
Inventor 金一丰马定连赵则亮张敏金洪财
Owner ZHEJIANG LYUKEAN CHEM
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