Study On The Synthesis Of Tmpde And The Measurement Of Vapor-Liquid Equilibrium Of The Mixture

This dissertation focused on the synthesis of Trimethylol propane diallyl ether and Allyl Pentaerythritol.The vapor-liquid equilibrium (VLE) of binary system allyl alcohol-methanol, allyl alcohol-ethanol, allyl alcohol-water were studied, respectively.Trimethylolpropane diallyl ether was synthesized with trimethylolpropane, sodium hydroxide and allyl chloride as raw materials by Williamson etherification reaction. The effects of reaction temperature, concentration of NaOH, amount of catalyst and different catalyst on the yield were researched, which the reaction conditions were analyzed by Response Surface Methodology (RSM) with three factors and three levels, and a correlation model on the optimized synthesis yield of trimethylolpropane diallyl ether was presented. The optimal synthesis conditions of trimethylolpropane diallyl ether with the catalyst of tetrabutylammonium bromide were as follows:reaction temperature,75.2℃, concentration of NaOH,38.5%, amount of catalyst,14.5%, which the optimized yield was 91.2%.Allyl Pentaerythritol was synthesized with pentaerythritol, sodium hydroxide and allyl chloride as raw materials by Williamson etherification reaction. Response Surface Methodology (RSM) was used to analyze reaction temperature, concentration of NaOH, amount of catalyst on the yield of Allyl Pentaerythritol and a correlation model on the optimized synthesis yield of Allyl Pentaerythritol was presented. The analysis of variance showed that the interactions between reaction temperature and amount of catalyst, concentration of NaOH and amount of catalyst affected the response variables significantly. The optimaized synthesis conditions of Allyl Pentaerythritol with the catalyst of tetrabutylammonium bromide were as follows:reaction temperature,78.0℃, concentration of NaOH,54.9%, amount of catalyst,11.1%, which the optimized yield was 70.2%.The vapor-liquid equilibrium (VLE) of binary system allyl alcohol-methanol, allyl alcohol-ethanol, allyl alcohol-water at 101.33kPa were measured. The thermodynamic consistency of the VLE data was checked by Herrington method. For the binary system of allyl alcohol-methanol, calculated with Wilson equation, the maximum deviation of vapour phase composition and the average deviation were 0.0095,0.0318. The energy parameters g12-g11)and g21-g22 were -3572.51,-3543.27, respectively; Those calculated with NRTL equation, the maximum deviation of vapour phase composition was 0.0094, the average deviation,0.0459. The energy parameters g12-g11 and g21-g22 were -4423.03,-4591.73, respectively, and a12 was 0.3. Compared with the results from the two equations for this system, the fitting precision of the Wilson model was better. For the binary system of allyl alcohol-ethanol, calculated with Wilson equation, the maximum deviation of vapour phase composition was 1.7037, the average deviation,0.2129. The energy parameters g12-g11 and g21-g22 were -4790.92 and -2762.64, respectively; those calculated with NRTL equation, the maximum deviation of vapour phase composition was 1.0561, the average deviation,0.0587. The energy parameters g12-g11 and g21-g22 were -3474.24,-7761.92, respectively, andα12 was 0.3. Compared with the results from the two equations for this system, the fitting precision of the NRTL model was better. For the binary system of allyl alcohol-water, calculated with Wilson equation, the maximum deviation of vapour phase composition was 0.0516, the average deviation,0.1617. The energy parameters g12-g11 and g21-g22 were 12250.5,-2140.81, respectively; Those calculated with NRTL equation, the maximum deviation of vapour phase composition was 0.0582, the average deviation,0.1585. The energy parameters g12-g11 and g21-g22 were -7344.16,-4987.03, respectively, andα12 was 0.3. Compared with the results from the two equations for this system, the fitting precision of the NRTL model was better.