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Catalytic dehydration of fructose to 5-hydroxymethylfurfural over mesoporous Nb-W oxide solid acid catalyst
Biomass & Bioenergy ( IF 5.8 ) Pub Date : 2023-06-06 , DOI: 10.1016/j.biombioe.2023.106860
Qiuhe Ren , Hong Ma , Wenbo Wang , Chongchong Chen , Jinbin Xiao , Penghua Che , Xin Nie , Yizheng Huang , Kasanneni Tirumala Venkateswara Rao , Chunbao(Charles) Xu

In this study, a mesoporous Nb-W oxide solid acid catalyst was synthesized and characterized in detail by TEM, N2 physisorption, and Py-FTIR. Effects of the calcination temperature on the pore structure and acid properties were investigated. The results showed that increasing calcination temperature from 400 °C to 600 °C remarkably affected the characteristics of mesoporous Nb-W oxides, with a decrease in specific surface area, pore volume, and acid amount, but an increase in pore size from 5.1 nm to 10.4 nm. Furthermore, a notable decrease was found in both the fructose conversion and HMF yield in the dehydration of fructose to HMF over Nb-W oxides when increasing the calcination temperature, and the catalyst could keep high catalytic activity and selectivity after recycling 4 times. Solvents also played a key role in the fructose dehydration to HMF over the Nb-W oxides, and DMSO was the optimized solvent. 1H NMR and 13C NMR experiments revealed that the key intermediate, 4-hydroxy-5-hydroxymethyl-4,5-dihydrofuran-2-carbaldehyde, could generate in DMSO but not in other solvents including NMP, DMF, DMAC, and EG.



中文翻译:

介孔铌钨氧化物固体酸催化剂催化果糖脱水制5-羟甲基糠醛

在这项研究中,合成了一种介孔 Nb-W 氧化物固体酸催化剂,并通过 TEM、N 2物理吸附和 Py-FTIR对其进行了详细表征。研究了煅烧温度对孔结构和酸性质的影响。结果表明,将煅烧温度从 400 °C 提高到 600 °C 显着影响介孔 Nb-W 氧化物的特性,比表面积、孔体积和酸量降低,但孔径从 5.1 nm 增加到 10.4 纳米。此外,当焙烧温度升高时,Nb-W氧化物上果糖脱水制HMF的果糖转化率和HMF收率均显着降低,催化剂仍能保持较高的催化活性和选择性回收4次后。溶剂在 Nb-W 氧化物上的果糖脱水为 HMF 中也起着关键作用,DMSO 是优化的溶剂。1H NMR 和13C NMR 实验表明,关键中间体 4-hydroxy-5-hydroxymethyl-4,5-dihydrofuran-2-carbaldehyde 可以在 DMSO 中生成,但在 NMP、DMF、DMAC 和 EG 等其他溶剂中不能生成.

更新日期:2023-06-06
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