催化学报 ›› 2009, Vol. 30 ›› Issue (12): 1203-1208.

• 研究论文 • 上一篇    下一篇

生物质炭基固体酸催化剂的制备

乌日娜1, 王同华1, 修志龙2, 郭 峰2, 潘艳秋1, 银建中3   

  1. 1 大连理工大学化工学院材料化工系精细化工国家重点实验室, 辽宁大连 116012 2 大连理工大学环境与生命学院生物科学与工程系, 辽宁大连 116023 3 大连理工大学化工学院化工机械系, 辽宁大连 116012
  • 收稿日期:2009-12-25 出版日期:2009-12-25 发布日期:2013-09-29

Preparation of a Biomass Carbon-Based Solid Acid Catalyst

WU Rina1, WANG Tonghua1,*, XIU Zhilong2, GUO Feng2, PAN Yanqiu1, YIN Jianzhong3   

  1. 1State Key Laboratory of Fine Chemicals, Department of Materials Science and Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Dalian 116012, Liaoning, China 2Department of Biological Science and Engineering, School of Environ-mental and Biological Science and Technology, Dalian University of Technology, Dalian 116023, Liaoning, China 3Department of Chemi-cal Machinery, School of Chemical Engineering, Dalian University of Technology, Dalian 116012, Liaoning, China
  • Received:2009-12-25 Online:2009-12-25 Published:2013-09-29

摘要: 以生物质木粉为原料, 采用炭化-磺化法制备了炭基固体酸催化剂, 并用于油酸与甲醇的酯化反应, 考察了制备条件对炭基固体酸催化剂活性的影响. 采用 X 射线衍射、红外光谱、热重分析、高分辨透射电子显微镜及元素分析等手段对催化剂进行了表征. 结果表明, 由生物质木粉制备的炭基固体酸催化剂具有较高催化酯化反应活性, 在 400 oC 下炭化 0.5 h, 135 oC 下磺化 1 h 制备的炭基固体酸催化剂在精馏分水连续酯化装置中催化油酸与甲醇的酯化反应 2 h 时, 酯化转化率达到 96%. 采用炭化-磺化法制备的生物质炭基固体酸催化剂具有蠕虫状的无序乱层炭结构, 磺酸基 (-SO3H) 含量高达 13.25%, 并且在 220 oC 以下时具有良好的热稳定性.

关键词: 生物质, 生物柴油, 炭基固体酸, 油酸, 甲醇, 酯化

Abstract: A carbon-based solid acid catalyst was prepared by a carbonization-sulphonation method from natural biomass wooden powder. The esterification of oleic acid and methanol was taken as the model reaction to investigate the impact of  preparation parameters on the catalyst activity. X-ray diffraction, Fourier transform infrared spectroscopy, Thermogravimetric analysis, high-resolution transmission electron microscopy, and elemental analysis were used to characterize the catalyst. The results showed that the carbon-based solid acid catalyst prepared under the optimal conditions of carbonization at 400 oC for 0.5 h and then sulphonation at 135 oC for 1 h exhibited higher catalytic activity. The conversion of oleic acid reached 96% after reaction for 2 h in an equipment of continuous esterification with a rectifying column for removing water from the system. The biomass carbon-based solid acid catalyst had turbostratic carbon structure, and the sulfuric acid group (–SO3H) content reached 13.25%. The catalyst showed considerable heat stability below 220 oC.

Key words: biomass, biodiesel, carbon-based solid acid, oleic acid, methanol, esterification