Add time:08/07/2019 Source:sciencedirect.com
Synthesis of rubber oil methyl ester (ROME) employing a two-step procedure, esterification using homogeneous catalyst followed by transesterification with heterogeneous catalyst was studied. The acid value of extracted RSO was reduced from 24 mg KOH/g to 2 mg KOH/g during esterification using 1.5 wt% catalyst loading (H2SO4) and 15:1 methanol to oil molar ratio for 2 h reaction time at 30 °C. Transesterification of esterified RSO with heterogeneous Barium hydroxide octahydrate (cas 12230-71-6) catalyst (Ba(OH)2·8H2O) was performed using conventional and ultrasonic techniques. Ultrasonic technique results in the increased yield of ROME compared to conventional process. The effect of catalyst Ba(OH)2·8H2O dehydration on the yield of ROME was also investigated in detail. The results showed that methyl ester conversion is not influenced by calcinations of catalyst. Highest transesterification yield was obtained with non-calcinated Ba(OH)2·8H2O compared to calcinated catalyst. But, within the studied calcinations temperature range, 400 °C showed significantly higher ROME conversion compared to 800 °C. BET analysis confirms lower surface area formation at 800 °C compared to other calcinated conditions. Central composite design (CCD) using response surface methodology (RSM) was adopted to design the experimental matrix and to optimize the combined effect of process parameters, reaction time (5–15min), catalyst loading (CL) (4–6wt%) and methanol to oil molar ratio (MR) (6:1–9:1) on ROME conversion. A second order model equation with p-value <0.05 was obtained to predict the conversion using the input parameters. Maximum conversion (∼97%) was achieved at CL of 5.38 wt% with MR of 8.09:1 in 13.20 min.
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