Study on Synthsis of Cinnamic Acid from Styrene and Carbon Tetrachloride
|School||Zhejiang University of Technology|
|Keywords||Styrene Carbon tetrachloride Cinnamic acid Preparation Catalyst Dynamics|
Styrene and carbon tetrachloride as raw materials, through the addition and elimination reaction of cinnamic acid hydrolysis. Experimental The reaction temperature, reaction time, ratio of reactants, the catalyst type and amount of catalyst and other factors were studied. In the first step reaction, cuprous chloride, diethylamine is the preferred catalyst system conditions: a temperature of 70 ~ 75 ℃, reaction time 6h, the reaction molar ratio of 1:2, representing a catalyst material of styrene the amount of 5%, the yield was 91.0%. Experimental study of the preparation of supported catalysts, the catalyst carrier, the active component is filtered to obtain nano carbon tube as a carrier, cuprous oxide as active component preferred catalysts. Then the catalyst load condition and other factors, the amount of the active ingredient compared to obtain a dry mix prepared by the mass of the active ingredient content of 10% to 20% of the preferred catalysts. Examine the performance of the catalyst, at 70 ℃ after 5h reaction, the yield of up to 95%, after applying three times the yield still more than 80%. Hydrolytic elimination reaction in the second step, the use of different catalysts, the yield is very different. Acetic acid - ferric chloride system, acetic acid - ferric sulfate system, acetic acid - sulfuric acid system and acetate - zinc sulfate seven systems to inspect comparison, the acetic acid - zinc sulfate system most suitable for the hydrolysis reaction. The preferred reaction conditions: reaction time 12h, the catalyst intermediate accounted for 13.3 mole% acetic acid intermediates used in an amount of 1 to 1.3 times the yield of 91.2%. Addition reaction kinetics also studied. Through the derivation mechanism is established kinetic model: the experimental data by Polymath, to give a dissociation adsorption activation energy of a control procedure: 111kJ/mol. Regressed intrinsic kinetics equation: with 50 sets of data were fitted R2 = 0.93, each parameter at 95% confidence interval of the error is less than 1.8%. Parameters obtained reasonable and reliable. Also proposed a power function in the form of kinetic equations: The Polymath fit the experimental data obtained kinetic equation as follows: With 48 sets of data were fitted R2 = 0.93, each parameter at 95% confidence interval of the error is less than 1.5%. Its overall activation energy 108kJ/mol, with literature values. Intrinsic kinetics can better explain the reaction process, power function equations can better explain the reactant concentration and temperature on the impact of the experiment. Two model calculations and experimental values ??are in good agreement that the model is a reliable reference for engineering development.