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Organosulfonic acid-functionalized biomass-derived carbon as a catalyst for glycerol acetylation and optimization studies via response surface methodology
Journal of the Taiwan Institute of Chemical Engineers ( IF 5.5 ) Pub Date : 2021-01-11 , DOI: 10.1016/j.jtice.2020.12.021
Usman Idris Nda-Umar , Ramli Irmawati , Ernee Noryana Muhamad , Norsahida Azri , Nor Shafizah Ishak , Muhamad Yahaya , Yun Hin Taufiq‐Yap

Organosulfonic acid-functionalized biomass-derived carbon catalysts were developed using different aryl and alkyl sulfonating reagents at low concentrations. The catalysts were characterized using advanced analytical techniques and evaluated in glycerol acetylation in a batch reflux reactor. Results indicated that the catalyst obtained from the functionalization of palm kernel shell with ethanesulfonic acid (ESA) exhibited better performance in terms of glycerol conversion and triacetin selectivity. Response surface methodology (RSM) was used to develop empirical models to optimize the reaction conditions and subsequently validated. Average values of 99.03±0.14% GC, 6.91±0.56, 54.86±0.42, and 37.73±0.21% selectivity to monoacetin, diacetin and triacetin, respectively were achieved at the optimum conditions of temperature 120±2 °C, glycerol to acetic acid mole ratio of 1:8, catalyst load of 0.69 g and reaction time of 3 h. The models were statistically analyzed and exhibited a good fit with agreement between the predicted and the experimental data, the determination coefficient (R2) > 0.9500 and adequate signal-to-noise ratio >4. The effects of the reaction variables and their interaction were further explained using the models and the surface response plots. On the reusability test, the catalyst exhibited excellent performance in glycerol conversion and diacetin selectivity for the five reaction cycles but was inferior in the selectivity to triacetin, stabilizes only after the first reaction cycle at a reduced level, due to leaching of the acidic sites.



中文翻译:

有机磺酸官能化的生物质衍生碳作为甘油乙酰化和通过响应面法进行优化研究的催化剂

使用低浓度的不同芳基和烷基磺化试剂开发了有机磺酸官能化的生物质衍生碳催化剂。使用先进的分析技术对催化剂进行表征,并在间歇回流反应器中进行甘油乙酰化评估。结果表明,由棕榈磺酸壳用乙磺酸(ESA)官能化制得的催化剂在甘油转化率和三醋精选择性方面表现出更好的性能。响应面方法(RSM)用于建立经验模型以优化反应条件并随后进行验证。在120±2°C的最佳条件下,对单醋精,双醋精和三醋精的选择性分别达到99.03±0.14%GC,6.91±0.56、54.86±0.42和37.73±0.21%的平均值,甘油与乙酸的摩尔比为1:8,催化剂负载为0.69 g,反应时间为3 h。对模型进行统计分析,显示出与预测数据和实验数据,测定系数(R2)> 0.9500,并且适当的信噪比> 4。使用模型和表面响应图进一步解释了反应变量及其相互作用的影响。在可重复使用性测试中,该催化剂在五个反应循环中均表现出优异的甘油转化性能和双醋精选择性,但对甘油三醋精的选择性较差,仅在第一个反应循环后由于酸性位点的浸出而稳定在降低的水平。

更新日期:2021-02-05
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