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Clean Technology To Produce2-ethoxy-5-prop-1-enylphenol By Eugenol

Posted on:2015-04-17Degree:MasterType:Thesis
Country:ChinaCandidate:Z H ZhangFull Text:PDF
GTID:2181330452958021Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
Vanitrope as a phenolic ether spice, due to its stable, strong and long-lasting aroma,so it is widely used in the perfume industry and the pharmaceutical industry. Highly toxicreagent diethyl sulfate was used in traditional process,with highly corrosive,bring seriouspollution to the environment. Isomerization reaction Use liquid alkali, the reactiontemperature is high, and required the high equipment requirements, multi-product, andlow yield. To solve these problems, we explore a cleaner production processes, with betterindustrial prospects.DEC as ethylation reagent. adopted distillation process, selected a variety of catalysts,finally established K2CO3as a catalyst to synthesize eugenol ethyl ether. UsingResponse Surface Design to optimize reaction, obtaining optimum conditions. Thereaction temperature is177.5℃, the amount of KOH is8.66%of the total material, n(eugenol): n (DEC)=1:4.64, the reaction time was6.38h. Eugenol ethyl etherl maximumyield was93.1%. studied with KF/γ-Al2O3catalyst preparation. Experimentally get thecatalyst KF/γ-Al2O3preparation conditions was: impregnating temperature50℃,concentration impregnating30%, impregnation time8h, drying under120℃, calcinationtemperature400℃. Under this condition, the yield of eugenol ethyl etherl reached81.7%.Using KOH and phase transfer catalyst (PTC) polyethylene glycol to isomerismeugenol ethyl ether, by selected and contrasted, choiced PEG-400as phase transfercatalyst. Studied optimum conditions of PEG-400as phase transfer to synthsizeIsoeugenol ethyl etherl. Optimum conditions are: the amount of KOH is40%, the amountof PEG-400is40%, the reaction temperature is90℃, reaction time is6h; under thisprocess conditions, the yield of Isoeugenol ethyl ether reach96.3%.Studied with eugenol as raw material. Though one step way to synthesize isoeugenolethyl ether. By selected and contrasted. determined K2CO3as catalyst, PEG-400as a phasetransfer catalyst; one step way of this catalytic system to synthesize isoeugenol ethyl etheroptimum conditions as follows: reaction temperature is175℃, the amount of K2CO3is50%, the amount of PEG-400is40%, the addition ratio of n (DEC): n (eugenol)=4:1,reaction time6h, under the process conditions, the yield of isoeugenol ethyl ether is90.3%.Isoeugenol ethyl ether as raw material to synthesis vanitrope through demethylationreaction. Judged the conversion rate of isoeugenol ethyl ether and the selective ofvanitrope as an indicator, selected a variety of catalysts, and ultimately established theAlCl3as catalyst, toluene as a solvent, the reaction was studied on the process to obtain the optimum is as follows: the reaction temperature is40℃, the amount of AlCl3catalystis20%, reaction time is7h. the yield of Vanitrope reach38.4%.
Keywords/Search Tags:diethyl carbonate, polyethylene glycol, γ-alumina, Vanitrope
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