Preparation method for styrenated phenol
A technology for styrenated phenol and styrene, applied in the field of preparation of styrenated phenol, can solve the problems of solid waste pollution, uneven pore distribution, low conversion rate, etc., and achieves pollution reduction, stable reaction process, and corrosion degree. little effect
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preparation example Construction
[0012] A preparation method of styrenated phenol, comprising the following steps:
[0013] Step 1: Take phenol and p-toluenesulfonic acid and put them into the container, pass nitrogen gas, and stir fully with the stirring device. The rotation speed of the stirring device is 300-350r / min, heat up to 85°C, and start to add styrene dropwise. The dropping time is less than 2.5 Hour;
[0014] Step 2: After the addition of styrene is completed, the temperature is raised to 120-130°C at a constant speed, and the temperature is kept for 2-2.5 hours;
[0015] Step 3: Stop heating, add triethylamine to the mixture, stir well and then filter, then suction filter and vacuum distill until no liquid evaporates, cool down to below 80°C, and discharge.
[0016] Further, the purity of phenol is greater than 99%, and the purity of styrene is greater than 99%.
[0017] Further, the mass ratio of styrene to phenol is 1.9:1˜2.3:1.
[0018] Further, in step 1, styrene is added dropwise, the dro...
Embodiment 1
[0022] Accurately weigh 200g of phenol and 2.0g of p-toluenesulfonic acid and put them into a dry and clean four-necked flask, fix and install the stirring paddle, and insert thermocouples, spherical condensing reflux tubes and nitrogen gas conduits into the remaining three ports of the four-necked flask. The phenol was melted by heating with nitrogen, and the stirring blade was turned on at a speed of 300 r / min. When the temperature rises to 85°C, 380g of styrene is added dropwise, the dropping rate is controlled to be 2.6g / min, the dropping time does not exceed 2.5h, and the temperature is maintained at 88-92°C. After dropping, the temperature was raised to 120°C at a constant speed, and the heat preservation was started. Stop heating after 2h, add 1.2g triethylamine to neutralize, stir well and filter. Start the vacuum pump, adjust the vacuum degree to 0.095Mpa, and keep the kettle temperature not exceeding 140°C until no liquid evaporates. Cool down to below 80°C and dis...
Embodiment 2
[0024] Accurately weigh 200g of phenol and 4.0g of p-toluenesulfonic acid and put them into a dry and clean four-necked flask, fix and install the stirring paddle, and insert thermocouples, spherical condensing reflux tubes and nitrogen gas conduits into the remaining three ports of the four-necked flask. The phenol was melted by heating with nitrogen, and the stirring paddle was turned on at a speed of 350 r / min. When the temperature rose to 85°C, 460g of styrene was added dropwise, the dropping rate was controlled to be 5g / min, the dropping time was not more than 2.5h, and the temperature was maintained at 92°C. After dropping, the temperature was raised to 120°C at a constant speed, and the heat preservation was started. Stop heating after 2.5h, add 2.4g triethylamine to neutralize, stir well and filter. Start the vacuum pump, adjust the vacuum degree to 0.095Mpa, and keep the kettle temperature not exceeding 140°C until no liquid evaporates. Cool down to below 80°C and d...
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