通过γ-氯丙基三甲氧基硅烷将磺基功能化离子液体-N-磺丙基咪唑盐化学键合到微球硅胶上,制得微球硅胶固定化离子液体(IL3). 用FTIR、TG、~(13)C NMR、SEM、BET及酸度测定等测试技术对IL3进行了表征,并考察其在果糖脱水合成5-羟甲基糠醛(HMF)过程中的催化性能. 研究结果表明,氯丙基三甲氧基硅烷可以将磺基功能化咪唑型离子液体化学键合到微球硅胶上. 微球硅胶固定化磺基咪唑离子液体能有效催化果糖脱水生成HMF. 果糖在固载率45.4%的IL3催化下、乙二醇甲醚(EGME)溶剂中、115 ℃反应5 h,HMF收率可达82.1%. 催化剂循环使用4次后,HMF的收率下降为53.0%.
The sulfonic group functionalized ionic liquid-1-H-3-(3-sulfonic acid)propylimidazolium chloride was immobilized on micro-ball silica-gel with γ-chloropropyltrimethoxysilane as coupling agent to obtain the silica-gel immobilized ionic liquid(IL3). IL3 was characterized by SEM, FTIR, DSC-TG, ~(13)C NMR, BET, and acidity measurement. Its catalytic performance in the synthesis of 5-hydroxymethylfurfural(HMF) from fructose dehydration was investigated. The results indicate that 1-H-3-(3-sulfonic acid)propylimidazolium chloride could be immobilized on micro-ball silica-gel surface by chemical bonds, and IL3 is a good catalyst for the HMF synthesis from fructose dehydration. The yield of HMF was up to 82.1% with 45.4% loading of IL3 as the catalyst and ethylene glycol monomethyl ether(EGME) as solvent at 115 ℃ over 5 h. After IL3 reused four times, the yield of HMF decreased from 82.1% to 53.0%.
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