Separation of Vanillin from Oil Palm Empty Fruit Bunch Lignin

The separation of vanillin from the lignin of empty fruit bunch oil palm is presented in this study. The lignin was extracted from soda black liquor derived from oil palm empty fruit bunches (EFB) using 20% sulfuric acid. Nitrobenzene oxidation was carried out by adding 50 mg of dry EFB lignin into a mixture of 7 mL of 2 M NaOH and 4 mL of nitrobenzene in a 15 mL steel autoclave. The autoclave was sealed tightly with a screw cap fitted with a Teflon gasket and heated to 165°C for 3 h in a preheated thermostatic oil bath. High performance liquid chromatography (HPLC) was used to determine the concentration of each compound present in the lignin. There were eight compounds detected in the HPLC chromatogram. The crystallization process was then used as a method to separate vanillin from other compounds. Based on the solubility of vanillin in acetone, 15 mL of acetone was added to the residue of the oxidized products and heated to 60°C for 10 min. A yield of 1.6% vanillin was isolated from a 50 mg lignin sample. The isolated compound was analyzed with HPLC, Fourier transform infrared spectrophotometry (FT‐IR) and nuclear magnetic resonance (¹³C‐NMR) for structural verification. The results of the characterization studies proved that the isolated compound is vanillin.