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Design of an acidic sulfonated mesoporous carbon catalyst for the synthesis of butyl levulinate from levulinic acid
Environmental Progress & Sustainable Energy ( IF 2.1 ) Pub Date : 2021-07-22 , DOI: 10.1002/ep.13721
Behrokh Bakhtiari 1 , Alireza Najafi Chermahini 1 , Zahra Babaei 1
Affiliation  

In this work, the ordered mesoporous carbon CMK-8 which has some advantages, including large specific pore volume, high surface area, and also its tunable pore size, was synthesized, then functionalized with various sulfonic acid groups and utilized as a heterogeneous catalyst in the esterification reaction of levulinic acid (LA) into n-butyl levulinate (BL). The prepared catalysts were characterized using Fourier transformed-infrared spectroscopy, N2 adsorption–desorption, small-angle X-ray diffraction analysis, elemental analysis, transmission electron microscopy, field emission scanning electron microscope, thermal gravimetric analysis, energy dispersive X-ray spectroscopy, and elemental mapping. The important parameters such as reaction temperature, reaction time, catalyst amount, and LA to n-BuOH molar ratio were investigated by Taguchi experimental design. Maximum BL yield (75.1%) and LA conversion (95%) were obtained with CMK-8-SO3H catalyst under optimum reaction conditions: reaction temperature 130°C, reaction time 10 h, catalyst dosage 0.015 g, and LA to n-BuOH molar ratio 1:10. Among the entire parameters, LA to n-BuOH molar ratio followed by the reaction temperature, catalyst concentration, and reaction time have the most influence on BL yield. Finally, the regeneration and reusability of the CMK-8-SO3H catalyst were studied, and the recovered catalyst showed high stability and activity after four runs.

中文翻译:

乙酰丙酸合成乙酰丙酸丁酯的酸性磺化介孔碳催化剂的设计

在这项工作中,我们合成了有序介孔碳 CMK-8,它具有比孔体积大、比表面积大、孔径可调等优点,然后用各种磺酸基团进行功能​​化,并用作非均相催化剂。乙酰丙酸 (LA) 酯化反应生成乙酰丙酸丁酯 (BL)。使用傅立叶变换红外光谱、N 2对制备的催化剂进行表征吸附-解吸、小角度 X 射线衍射分析、元素分析、透射电子显微镜、场发射扫描电子显微镜、热重分析、能量色散 X 射线光谱和元素映射。通过田口实验设计研究了反应温度、反应时间、催化剂用量和LA与n- BuOH摩尔比等重要参数。在最佳反应条件下,CMK-8-SO 3 H 催化剂获得最大 BL 产率(75.1%)和 LA 转化率(95%):反应温度 130°C,反应时间 10 h,催化剂用量 0.015 g,LA to n -BuOH 摩尔比 1:10。在整个参数中,LA到n-BuOH 摩尔比、反应温度、催化剂浓度和反应时间对 BL 产率的影响最大。最后,研究了CMK-8-SO 3 H催化剂的再生和可重复使用性,回收的催化剂在四次运行后表现出较高的稳定性和活性。
更新日期:2021-07-22
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