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
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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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