Abstract

The optimization of the epoxidation reaction of methyl esters obtained from Jatropha oil was appraised. Response surface methodology (RSM) based on a central composite rotatable design (CCRD) was employed for the experimental design. Four reaction variables namely hydrogen peroxide/ C=C mole ratio, formic acid/C=C mole ratio, reaction temperature and reaction time were evaluated. The optimum epoxidation conditions calculated by the quadratic model were 3.12 moles of hydrogen peroxide/C=C moles, 0.96 moles of formic acid/C=C moles, a reaction temperature of 70.0 °C and a reaction time of 277 minutes. A reaction optimized by the proposed process parameters provided a yield of 92.89 ± 1.29 wt.% with relatively improved reaction time. Hydrogen peroxide concentration and reaction temperature were found to be the most significant variables while reaction temperature and hydrogen peroxide showed strong interactions. The epoxidized methyl esters were analyzed using FT-IR, 1 H NMR and 13 C NMR techniques. This study suggested relatively higher molar ratio of formic acid required than was proposed in the literature.

Highlights

  • SUMMARYThe optimization of the epoxidation reaction of methyl esters obtained from Jatropha oil was appraised

  • The epoxidation reaction in natural oils and alkyl esters has gained prominence in recent years due to its multifarious usage in many industrial synthetic processes

  • Response surface methodology (RSM) based on central composite rotatable design (CCRD) was successfully applied for optimizing the reaction parameters for the epoxidation of methyl esters obtained from Jatropha oil using hydrogen peroxide and formic acid

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Summary

SUMMARY

The optimization of the epoxidation reaction of methyl esters obtained from Jatropha oil was appraised. Four reaction variables namely hydrogen peroxide/ C=C mole ratio, formic acid/C=C mole ratio, reaction temperature and reaction time were evaluated. The optimum epoxidation conditions calculated by the quadratic model were 3.12 moles of hydrogen peroxide/C=C moles, 0.96 moles of formic acid/C=C moles, a reaction temperature of 70.0 °C and a reaction time of 277 minutes. A reaction optimized by the proposed process parameters provided a yield of 92.89 ± 1.29 wt.% with relatively improved reaction time. The epoxidized methyl esters were analyzed using FT-IR, 1H NMR and 13C NMR techniques. This study suggested relatively higher molar ratio of formic acid required than was proposed in the literature. KEY-WORDS: Characterization – Epoxidised Jatropha oil – Optimization – Response surface methodology

INTRODUCTION
MATERIALS AND METHODS
Experimental design
Epoxidation process
Characterization of the product
Statistical analysis
Optimization of the reaction conditions by RSM
Effects of reaction parameters
Validation of the model
FT-IR analysis
NMR analysis
CONCLUSIONS
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