"Place the four-necked flask in an oil bath, install a stirrer, thermometer and reflux condenser."
-Deshangchemical
The preparation method of octyl benzyl phthalate
(1) Place the four-necked flask in an oil bath, install a stirrer, thermometer and reflux condenser. Add phthalic anhydride, n-octanol and sulfuric acid to the flask. Gradually heat it to 138-140℃ while stirring continuously, allowing the phthalic anhydride to melt completely into a transparent liquid. Then raise the temperature to 100-110℃ and let the reaction proceed for 2 hours. A monooctyl phthalate is produced.
(2) Cool the reaction product to 60-80℃, drop in sodium hydroxide solution while stirring continuously. Complete the addition within 30 minutes and then adjust the pH of the reaction mixture to 8.0-8.5 using sodium carbonate solution.
(3) Heat the reaction product in step (2) to 80-90℃, add catalyst tri-n-butylamine and drop in benzyl chloride while controlling the dripping speed. Complete the addition in 20 minutes. Then raise the temperature to 100-105℃ and conduct a reflux reaction for 2-3 hours.
(4) After the reaction is complete, cool to room temperature, pour the reaction mixture into a separating funnel and let it stand to separate layers. The lower layer is the aqueous phase. The upper layer is the oil phase. Wash it with 200 milliliters of water three times until it becomes neutral. After removing the water layer, the crude ester is obtained.
(5) Distill the crude ester obtained in step (4) using steam distillation to remove low-boiling substances. Then conduct vacuum distillation to remove moisture and finally obtain a pale yellow transparent oily liquid, which is the finished product.
