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Preparation, characterization and application of sulfonated mesoporous hollow carbon microspheres

机译:磺化介孔中空碳微球的制备,表征及应用

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Mesoporous hollow carbon microspheres (MHCM) with high specific surface area was prepared by using a core-shell structured mesoporous material of SiO2@SBA-15 as hard template, sucrose as carbon precursor via inverse replica method. Then, MHCM was sulfonated by diazonium coupling to synthesize sulfonated mesoporous hollow carbon microspheres (MHCM-DS). TEM images showed that hollow carbon microspheres were successfully formed. The small angle XRD patterns of SiO2@SBA-15 and MHCM confirmed these two materials were ordered mesoporous material. BET surface area and pore diameter distribution results indicated that MHCM had an area of 620m(2)/g and a double mesoporous with 2.7nm and 3.4nm pore diameter, respectively. After the MHCM being sulfonated, the area was reduced to 446m(2)/g. In addition, pore diameter distributions of 2.7nm and 3.4nm were weakened, and new pore diameter distributions in the range of 5-10nm were appeared meanwhile. Surface acid amount of sulfonated carbon microspheres (2.8mmol H+/g) was higher than unsulfonation carbon microspheres (2.2mmol H+/g). Besides, the FTIR result also demonstrated the existing of -SO3H. The catalytic activity of MHCM-DS was observed for transesterification and epoxidation reaction, respectively. For transesterification reaction, the highest yield of fatty acid methyl esters was 93wt% at 180 degrees C in 6h with 0.6g catalyst amount. For epoxidation reaction, when reaction temperature was 40 degrees C and reaction time was 6h, conversion and yield could both reach up to 50%.
机译:通过使用SiO 2 @ SBA-15作为硬模板的核心壳结构化介孔材料制备具有高比表面积的介孔中空碳微球(MHCM),通过反复制法作为碳前体。然后,将MHCM通过重氮偶联磺化以合成磺化的介孔中空碳微球(MHCM-DS)。 TEM图像显示成功形成中空碳微球。 SiO 2的小角度XRD图案SBA-15和MHCM确认了这两种材料是有序的介孔材料。 BET表面积和孔径分布结果表明,MHCM的面积为620米(2)/ g,分别为2.7nm和3.4nm孔径的双介孔。在磺化MHCM后,该面积降至446米(2)/ g。此外,削弱了2.7nm和3.4nm的孔径分布,同时出现了5-10nm的新孔径分布。表面酸量的磺化碳微球(2.8mmol H + / g)高于未熔融碳微球(2.2mmol H + / g)。此外,FTIR结果还证明了-SO3H的存在。观察到MHCM-DS的催化活性分别用于酯交换和环氧化反应。对于酯交换反应,脂肪酸甲酯的最高产率为93wt%,在6小时内为0.6g催化剂量为6小时。对于环氧化反应,当反应温度为40℃并反应时间为6小时,转化和产率均可达到50%。

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