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在150℃条件下,对以离子液体[BMIM]Cl和DMSO为溶剂,微晶纤维素为原料,金属氯化物和浓硫酸为催化剂制备5-羟甲基糠醛的反应过程进行了研究。通过改变作为溶剂的离子液体[BMIM]Cl与二甲基亚砜(DMSO)的质量比,以及Cr Cl3·6H2O和浓硫酸的加入量,考察较为优化的反应条件。反应产物由高效液相色谱进行分析。结果发现,在固液比(TS)为3.8%,m([BMIM]Cl)∶m(DMSO)=1∶1(IDR=1∶1),硫酸和氯化铬加入量分别3.3%和13.3%(相对于纤维素)等条件下反应60 min时,5-HMF得率较高,为74.4%。
The reaction of 5-hydroxymethylfurfural with ionic liquid [BMIM] Cl and DMSO as solvent, microcrystalline cellulose as raw material, metal chloride and concentrated sulfuric acid as catalyst was studied at 150 ℃. The optimized reaction conditions were investigated by changing the mass ratio of [BMIM] Cl to dimethylsulfoxide (DMSO) as a solvent and the amount of CrCl3 · 6H2O and concentrated sulfuric acid. The reaction product was analyzed by high performance liquid chromatography. As a result, it was found that the addition of sulfuric acid and chromium chloride was 3.3% and 13.3 respectively at a solid-liquid ratio (TS) of 3.8%, m ([BMIM] Cl) % (Relative to cellulose) and other conditions 60min reaction time, 5-HMF yield was high, 74.4%.