Soft-template synthesis of sulfonated mesoporous carbon with high catalytic activity for biodiesel production

Soft-template synthesis of sulfonated mesoporous carbon with high catalytic activity for biodiesel production
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软模板合成高催化活性磺化介孔碳用于生物柴油生产

DOI:
10.1039/c2ra21982d
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发表时间:
2013-01
期刊:
影响因子:
3.9
通讯作者:
Dong, Xiaoping
Dong, Xiaoping
中科院分区:
化学3区
文献类型:
--
作者:
Chang, Binbin;Fu, Jie;Tian, Yanlong;Dong, Xiaoping

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在此,我们报道了一种用于催化合成生物柴油的优异碳基固体酸催化剂,该催化剂通过介孔酚醛树脂碳化,然后用浓硫酸磺化而制备。研究了炭化温度对孔结构和酸度的影响。采用傅里叶变换红外光谱、能谱分析和间接滴定法证明了碳表面-SO3H基团的成功修饰并测定了催化剂的酸度。采用N2吸附-脱附和透射电子显微镜表征了介孔结构和孔结构参数。这些结果表明,在低温(400℃)下碳化的磺化催化剂表现出最高的酸度,为2.21 mmol H+ g−1,同时保留了介孔结构和较大的表面积。采用油酸与甲醇的酯化反应来评价催化剂的性能。磺化介孔碳催化剂表现出高效的活性,在 30: 1 甲醇/油酸的作用下,在 70 °C 下反应 3 h,油酸的转化率超过 95%。对反应物摩尔比、反应时间和反应温度等实验参数进行了优化,连续五个循环后表现出优异的回收性能。
Here, we reported an excellent carbon-based solid acid catalyst for the catalytic synthesis of biodiesel, which was prepared by carbonizing a mesoporous phenolic resin and then followed by sulfonation with concentrated sulfuric acid. The influence of carbonization temperature on the pore structure and acidity was studied. Fourier transform infrared spectroscopy, energy dispersive spectrum analysis and an indirect titration method were used to demonstrate the successful modification of –SO3H groups on the carbon surface and determine the acidities of catalysts. N2 adsorption–desorption and transmission electron microscopy were used to characterize the mesoporous structure and pore structure parameters. These results indicated that the sulfonated catalyst carbonized at a low temperature (400 °C) showed the highest acidity of 2.21 mmol H+ g−1, meanwhile, retaining a mesoporous structure and relatively large surface area. The esterification reaction of oleic acid with methanol was employed to evaluate the performance of catalysts. The sulfonated mesoporous carbon catalyst exhibited a highly efficient activity, above 95% conversion of oleic acid with a 30 : 1 methanol/oleic acid at 70 °C for 3 h. Experimental parameters, including the molar ratio of reactants, reaction time and reaction temperature, were optimized and a superior recycling property was presented after five consecutive cycles.
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