Preparation method of 2,6-diphenyl phenol
A diphenylphenol, tubular technology, applied in the preparation of organic compounds, chemical instruments and methods, bulk chemical production, etc., can solve the problems of difficult separation of products and catalysts, low mechanical strength of catalysts, difficult control of operating conditions, etc. , to achieve the effect of high mechanical strength, easy to control, and not easy to coke
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Embodiment 1
[0022] With reference to the method described in the article "Study on the Synthesis of 2,6-Diphenylphenol Intermediates" published on the 30th to 34th pages of the first phase of "Ship Defense Chemical" in 2009 by Xu Donghai, etc., using cyclohexanone as Raw materials for synthesis of tripolyketone. Connect a condenser to a 250mL three-neck flask, add 98.2g cyclohexanone and 40mL toluene, heat to 150°C, add 0.28g potassium hydroxide as a catalyst, and reflux at 150°C for 2.5 hours. After the reaction stops, use the reaction product 10% hydrochloric acid solution neutralization, separation of water layer, drying, vacuum distillation, collecting fractions at different temperatures, the mass fraction of the product obtained is 12.6% cyclohexanone, 35.6% dimer ketone, 50.6% trimer ketone, 1.2 % high boilers.
Embodiment 2
[0024] A tubular fixed-bed reactor with an aspect ratio of 10:1 is placed in a heating furnace, and the tubular fixed-bed reactor is filled with 5% Pd / Al 2 o 3 Catalyst, the reaction temperature is controlled at 290 ° C, protected by nitrogen, and after the temperature is stable, the trimerketone prepared in Example 1 is input from the lower port of the tubular fixed bed reactor with a pump, and the liquid hourly space velocity is 2.9h -1 , relying on the pressure of the pump, the trimeric ketone flows out from the upper port of the tubular fixed-bed reactor after being reacted by the catalyst, and collects the reactant flowing out; adopts the external standard method, analyzes the reactant with HPLC, and the analysis condition is: column Temperature is 30 ℃, mobile phase is 80% methanol aqueous solution, and mobile phase flow rate is 0.5ml / min, and analysis result is as follows: Based on the mass of described reactant as 100%, wherein tripolyketone is 6.9%, 2-cyclohexyl -6-p...
Embodiment 3
[0026] A tubular fixed-bed reactor with an aspect ratio of 5:1 is placed in a heating furnace, and alumina is loaded into the tubular fixed-bed reactor as a catalyst with a carrier palladium content of 5%, the reaction temperature is controlled at 290 ° C, and nitrogen gas Protection, after the temperature is stable, the trimerketone prepared in Example 1 is input from the lower port of the tubular fixed bed reactor with a pump, and the liquid hourly space velocity is 2.9h -1 , relying on the pressure of the pump, the trimeric ketone flows out from the upper port of the tubular fixed-bed reactor after being reacted by the catalyst, and collects the reactant flowing out; adopts the external standard method, analyzes the reactant with HPLC, and the analysis condition is: column Temperature is 30 ℃, mobile phase is 80% methanol aqueous solution, and mobile phase flow rate is 0.5ml / min, and analysis result is as follows: The mass of described reactant is 100%, and wherein, trimeron...
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