Fractionation of phenolic aldehydes by liquid-liquid extraction and polymer resin adsorption

The extraction and adsorption characteristics of three phenolic aldehydes with high physicochemical similarity in lignocellulosic biomass hydrolyzate, which are fermentation inhibitors, were investigated. The extraction process considered both physical extraction with two organic solvents and reactive extraction with five basic extractants. In physical extraction, n-hexane was found to be the most suitable organic solvent for selectively separating 4-hydroxybenzaldehyde from the three phenolic aldehydes, and in reactive extraction, trioctylphosphine oxide was identified as the most suitable basic extractant for the selective separation of syringaldehyde. In the adsorption process, various neutral polymer resins and anion-exchange polymer resins were employed. Among them, the neutral polymer resin XAD16 was found to be the most suitable for selectively separating 4-hydroxybenzaldehyde. To efficiently separate and concentrate the three phenolic aldehydes with equal mass percentages, a proposed five-step fractionation process included the aforementioned extraction and adsorption techniques. By implementing n-hexane-based physical extraction in step 4 and NaOH solution-based back-extraction in step 5 of the fractionation process, the purities of 4-hydroxybenzaldehyde, vanillin, and syringaldehyde in the final solution increased from their initial 33.3% each to 67.6%, 69.8%, and 76.4%, respectively, at a volume ratio of the aqueous phase to the organic phase of 1:15.