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纤维素制备5-羟甲基糠醛技术研究
Preparation of 5-hydroxymethylfurfural from cellulose
【摘要】 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%。
【Abstract】 5-HMF is prepared in a mixed solvent of the ionic liquid 1-butyl-3-methylimidazolium chloride( [BMIM]Cl) and dimethyl sulfoxide( DMSO) using metal chloride( Cr Cl3·6H2O) 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]Cl) ∶ m( DMSO),H2SO4 and Cr Cl3·6H2O 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∶ 1of [BMIM]Cl-DMSO ratio,3. 3% of H2SO4 and 13. 3% of Cr Cl3·6H2O( with respect to cellulose) and 60 minutes of time.
【Key words】 5-hydroxymethylfurfural; microcrystalline cellulose; ionic liquids; metal chlorides;
- 【文献出处】 现代化工 ,Modern Chemical Industry , 编辑部邮箱 ,2015年10期
- 【分类号】TQ251.11
- 【被引频次】2
- 【下载频次】248