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介孔炭基固体酸催化高酸值油脂合成生物柴油的研究

—— 磺化介孔炭的表征及其催化性能初步研究. 介孔炭基固体酸催化高酸值油脂合成生物柴油的研究. 高振华 2012-12-4. 1. 2. 3. Contents. 磺化介孔炭的表征. 油酸甲 酯的合成. 试验计划. 磺化介孔炭的表征. 红外. a: OMC b: S-OMC(80 ℃ , 1:4:2) c: S-OMC(90 ℃ , 1:4:2). 磺化介孔炭的表征. TEM. OMC-800 ℃. OMC-400 ℃. S-OMC -80 ℃ , 1:4:2. S-OMC -80 ℃ , 1:4:4. S-OMC -90 ℃ , 1:4:2.

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介孔炭基固体酸催化高酸值油脂合成生物柴油的研究

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  1. ——磺化介孔炭的表征及其催化性能初步研究 介孔炭基固体酸催化高酸值油脂合成生物柴油的研究 高振华 2012-12-4

  2. 1 2 3 Contents 磺化介孔炭的表征 油酸甲酯的合成 试验计划

  3. 磺化介孔炭的表征 • 红外 a: OMC b: S-OMC(80℃, 1:4:2) c: S-OMC(90℃, 1:4:2)

  4. 磺化介孔炭的表征 • TEM OMC-800℃ OMC-400℃ S-OMC -80℃, 1:4:2 S-OMC -80℃, 1:4:4 S-OMC -90℃, 1:4:2 S-OMC -90℃, 1:4:4

  5. 磺化介孔炭的表征 • BET 1.OMC-800℃ N2吸附/脱附等温线和孔径分布曲线 BET Surface Area: 178.7m2/g Mesopore/micropore Area: 88.0/63.6m2/g Total Pore Volume: 0.11cm3/g Mesopore /micropore Volume: 0.061/0.029cm3/g Average pore diameter: 2.8nm

  6. 磺化介孔炭的表征 • BET 2.S-OMC -80℃, 1:4:2N2吸附/脱附等温线和孔径分布曲线 BET Surface Area: 97.8m2/g Mesopore/micropore Area: 34.3/47.5m2/g Total Pore Volume: 0.054cm3/g Mesopore /micropore Volume: 0.025/0.022cm3/g Average pore diameter: 2.9nm

  7. 磺化介孔炭的表征 • BET 3.S-OMC -90℃, 1:4:2N2吸附/脱附等温线和孔径分布曲线 BET Surface Area: 80.8m2/g Mesopore/micropore Area: 32.0/42.4m2/g Total Pore Volume: 0.044cm3/g Mesopore /micropore Volume: 0.026/0.019cm3/g Average pore diameter: 3.3nm

  8. 磺化介孔炭的表征 • BET 4.S-OMC -90℃, 1:4:4N2吸附/脱附等温线和孔径分布曲线 BET Surface Area: 58.6m2/g Mesopore/micropore Area: 28.5/22.1m2/g Total Pore Volume: 0.031cm3/g Mesopore /micropore Volume: 0.021/0.011cm3/g Average pore diameter: 2.7nm

  9. 磺化介孔炭的表征

  10. 旋蒸温度过高 N2吸附脱附 仪器问题 乙醇挥发温度 过低 磺化介孔炭的表征 原因分析 溶剂乙醇挥发自组装过程在室温下进行，挥发缓慢。而后直接转移至100℃进行热聚合，温度变化大，导致两者结合不充分。 甲阶酚醛树脂除水处理时，旋蒸温度超过了50℃，致使酚醛树脂发生固化，部分生成不溶的丙阶酚醛树脂，影响了其与F127的聚合，导致孔结构差。

  11. 油酸甲酯的合成 • 硫酸催化(5wt%硫酸) 1.m(甲醇):m(油酸)=5:1, 65℃, 6h 2.m(甲醇):m(油酸)=5:1, 65℃, 24h 3.m(甲醇):m(油酸)=2:1, 150℃, 6h 4.m(甲醇):m(油酸)=10:1, 120℃, 6h

  12. 油酸甲酯的合成 • S-OMC催化(10wt%S-OMC) 1.m(甲醇):m(油酸)=10:1, 65℃, 10h 1.m(甲醇):m(油酸)=2:1, 150℃, 6h 3.m(甲醇):m(油酸)=10:1, 120℃, 6h

  13. 实验计划 改正操作方法合成OMC，重新测试BET结果 用已确定的条件制得的S-OMC在反应釜中催化油酸酯化反应，摸索反应条件 磺化不同炭化温度的OMC，考察其催化效果

  14. Thank you

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