纤维素制备5-羟甲基糠醛技术研究

Preparation of 5-hydroxymethylfurfural from cellulose

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%。

5-HMF is prepared in a mixed solvent of the ionic liquid 1-butyl-3-methylimidazolium chloride （[ BMIM] C1） and dimethyl sulfoxide （DMSO） using metal chloride （CrCl3 6H20） and concentrated sulfuric acid （ H2SO4 ） as catalysts at the temperature of 150℃. The optimized reaction conditions are studied by changing the ratio of m（ [ BMIM] C1）：m （DMSO）, H2SO4 and CrCl3 6H2O loading. The eventually obtained products are determined by HPLC. The yield of 5-HMF can reach as high as 74. 4% under the following conditions ：3.8% of solid-liquid ratio, 1 ： 1 of [ BMIM] C1-DMSO ratio,3.3% of H2SO4 and 13.3% of CrC13 ＂6H20 （with respect to cellulose） and 60 minutes of time.