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Preparation method of hydroxyethyl p-cumylphenol ether

A technology of cumyl phenol ether and p-cumyl phenol, which is applied in the field of synthesis of organic compounds, can solve problems such as wide molecular weight distribution, and achieve the effects of short reaction cycle, high reactivity and low energy consumption

Active Publication Date: 2015-03-25
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The products synthesized are all products with high ethoxylation addition number and wide molecular weight distribution, so they are not suitable for use in the fields of UV coatings, epoxy resins, polycarbonate molecular weight regulators, end-capping agents, etc.

Method used

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  • Preparation method of hydroxyethyl p-cumylphenol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 650g of p-cumylphenol, 2.0g of composite catalyst (1.8g of 1,1'-bis(diphenylphosphine) ferrocene, 0.2g of solid sodium hydroxide) 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. After vacuum degassing for 10 minutes, continue to add 150g of ethylene oxide, control the reaction temperature at 165-170°C, and the pressure in the reactor at -0.04-0.3Mpa. After adding, keep warm and continue the reaction until the pressure No longer down. 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 is analyzed by liquid chromatography: residual p-cumylphenol is <10ppm, hydroxyethyl p-cumylphenol ether is 97.9%, and t...

Embodiment 2

[0036] Add 650g of p-cumylphenol, 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. After vacuum degassing for 10 minutes, continue to add 139g of ethylene oxide, control the reaction temperature at 155-165°C, and the pressure in the reactor at -0.02-0.2Mpa. After adding, keep warm and continue the reaction until the pressure No longer down. 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 is analyzed by liquid chromatography: residual p-cumylphenol is <10ppm, hydroxyethyl p-cumylphenol ether is 99.2%, and the content of p...

Embodiment 3

[0038] Add 650g of p-cumylphenol, 1.5g of composite catalyst (1.35g of 1,1'-bis(diphenylphosphine) ferrocene, 0.15g of solid potassium methylate) into the reaction kettle, vacuumize with a vacuum pump, and use N 2After 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 145g of ethylene oxide, control the reaction temperature at 160-165°C, and the pressure in the reactor at 0.0-0.4Mpa. until it drops again. 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 is analyzed by liquid chromatography: residual p-cumylphenol is <10ppm, hydroxyethyl p-cumylphenol ether is 99.4%, and the content of polymers above p-cumylphenol polyoxyethyle...

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Abstract

The invention relates to a preparation method of hydroxyethyl p-cumylphenol ether. The preparation method comprises the following steps: (1) adding a certain amount of p-cumylphenol and a composite catalyst into a reaction kettle, vacuumizing with a vacuum pump, replacing air in the reaction kettle with N2 for three times and when the degree of vacuum is equal to or greater than -0.096MPa, stopping vacuum and then heating; (2) heating the temperature to 160 DEG C, carrying out vacuum degassing for 10 minutes, further adding a certain amount of ethylene oxide, by controlling the reaction temperature at 150-175 DEG C and the pressure inside the reaction kettle at -0.05 to 0.5Mpa, after the addition is completed, carrying out heat preservation and further reacting until the pressure no longer drops; and (3) after the reaction is completed, cooling to 100 DEG C, carrying out vacuum degassing for 20 minutes, neutralizing by adding a certain amount of glacial acetic acid, cooling to 80 DEG C and discharging the material to obtain the finished product. The preparation method is easy to industrially implement and the obtained product has good and stable quality.

Description

Technical field [0001] The present invention involves a method of preparing a hydroxyethylene to prepare the dry phenolin. It is a synthetic technology field of organic compounds. Background technique [0002] The hydroxyethene can be applied to the dry -based phenol ether.(Energy -saving), 5. Environmental Friendly (environmentally friendly), known as a new green industry technology for the 21st century.It is used as a functional diluent that is used as a UV coating with acrylic acid or methyl acrylic acid. It not only has the effect of dissolving and diluted low pools, regulating the viscosity of the system, but also can participate in the optical agglomeration, affecting the light curing speed of the coating and the curing film of the coating film and the curing filmSpecies, such as hardness, abrasion resistance, adhesion, flexibility and other physics and machines. [0003] As a modified agent and additive for the polymer polymer chain: it can be used for epoxy resin, polycar...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/03
CPCB01J31/26B01J2231/48C07C41/03C07C43/23
Inventor 马定连金一丰金洪财张敏赵则亮
Owner ZHEJIANG HUANGMA TECH
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