Abstract:
Levulinic acid and methyl levulinate were synthesized from cellulose with using solid FePO
4 as catalyst in water/methanol medium. By comparing the catalytic results of liquid acid, metal chloride, metal sulfate and FePO
4, the results showed that FePO
4 displayed a nearly result in both conversion efficiency of cellulose and yields of levulinic acid and methyl levulinate as comparable to the catalytic effects of H
2SO
4 and Al
2(SO
4)
3.The catalytic effect of solid FePO
4 was mainly attributed to form Brønsted and Lewis acidic sites, which provide catalytic activity for cellulose hydrolysis, glucose isomerization and dehydration to form levulinic acid/ester. The total yield of levulinic acid and methyl levulinatewas 62.2% under optimal the best technological conditions of reaction temperature at 220℃, reaction time for 2 h, 2 g of microcrystalline cellulose, water/methanol volume ratio of 1:19 (total solvent volume 40 mL) and 1.5 g of catalyst dosage. The characterization of cellulose, solid residue and FePO
4 catalyst were conducted by FT-IR, XRD and TG/DTG techniques, and the results indicated that the cellulose was efficiently liquefied and then the catalyst was recycled by recrystallization. The formation of levulinates was conducted by the methanolysis and hydrolysis of cellulose, while methyl glucoside (MLG) was an important intermediate and its conversion was affected by the reaction time and the catalyst dosage. Further systematical research of this new technique is further required before the process could be industrialized considering the excellent catalytic activity and recycling characteristic of FePO
4.