以超临界CO2为溶剂,以经磷酸浸渍碳化、浓H2SO4磺化制备的油茶壳炭磺酸为催化剂,将D-果糖脱水转化制备5-HMF.利用中和滴定、元素分析、红外光谱、Raman光谱对催化剂进行了表征.在220℃、浸渍10 h后再磺化3 h,-SO3H基团成功键合到无定形炭基体上,得到的油茶壳炭磺酸催化剂表面酸值最高可达1.8010 mmol·g-1.相比无溶剂或选取有机溶剂、浓硫酸为催化剂的反应体系而言,在超临界CO2中,D-果糖在120℃反应30 min,5-HMF的得率最高可达47%.实验结果为超临界CO2在生物质催化转化领域的应用及油茶壳的高附加值利用提供了理论和实验参考.%5-Hydroxymethyl furfural is made from fructose in supercritical carbon dioxide with Camellia oleifera nutshell sulfonic acid catalyst prepared by H3PO4 impregnation carbonization and sulfonation reaction with con-centrated H2SO4. Elemental analysis, ion exchange titration, FT-IR and Raman spectra are adopted for catalyst analysis. The results show that under the conditions of 220 ℃, 10 h immersing time and 3 h sulfonating time, -SO3H group is chemically bonded to the surface of the amorphous carbon material and the surface sulfonic acid value of the catalyst is up to 1.8010 mmol·g-1. Compared with non-solvent or organic solvent or concentrated H2SO4 reaction system, when the reaction temperature is 120 ℃ and the reaction time is 30 minutes, the highest yield of 5-HMF can be up to 47% in supercritical carbon dioxide solvent. The experimental results provide the-oretical and experimental reference for high-value added utilization of Camellia oleifera and utilization of super-critical carbon dioxide in biomass conversion.
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