Yusuff Adeyinka Sikiru, Gu Yanlong, Berdimurodov Elyor, Eliboev Ilyos
Department of Chemical and Petroleum Engineering, College of Engineering, Afe Babalola University Km 8.5, Afe Babalola Way Ado-Ekiti Ekiti State Nigeria
Institute of Physical Chemistry and Industrial Catalysis, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology 1037 Luoyu Road, Hongshan District Wuhan 430074 China.
RSC Adv. 2024 Sep 4;14(39):28308-28319. doi: 10.1039/d4ra04834b.
The grafting of metal-bipyridine (Bpy-M, M = Mn or Zn) on aminopropyl-modified montmorillonite K10 (NH-MK10) synthesized a functionalization-immobilization-metalation route was investigated. Formulated NH-MK10-Bpy-Mn and NH-MK10-Bpy-Zn were characterized using BET, FTIR, SEM, XRD, CHNS and NH-TPD techniques and tested for the synthesis of butyl acetoacetate (BAT) the transesterification of β-keto ethyl acetoacetate (EAA) with butanol (BTL). The influence of reaction parameters on the BAT yield was investigated using the Taguchi optimization approach. According to characterization data, the samples were mesoporous materials with a considerable number of acidic sites and diverse inorganic and organic functional groups, making them inorganic-organic hybrid catalysts. Optimization results showed that catalyst loading had the most significant impact on the BAT yield, followed by the BTL : EAA molar ratio and temperature, whereas the conversion time had the least impact on the reaction process. NH-MK10-Bpy-Mn outperformed NH-MK10-Bpy-Zn in the transesterification of β-keto EAA, achieving 96.1 ± 0.79% conversion compared to 87.3 ± 0.94% at 110 °C for 7 h with a BTL : EAA molar ratio of 1.4 : 1 and catalyst loading of 2.0 wt%. Both catalysts were reusable and maintained good stability, which indicate their great potential for catalyzing the transesterification of β-keto ester.
研究了在氨基丙基改性蒙脱石K10（NH-MK10）上接枝金属联吡啶（Bpy-M，M = Mn或Zn）合成功能化-固定化-金属化路线。使用BET、FTIR、SEM、XRD、CHNS和NH-TPD技术对配制的NH-MK10-Bpy-Mn和NH-MK10-Bpy-Zn进行了表征，并测试了它们用于乙酰乙酸丁酯（BAT）的合成，即β-酮基乙酰乙酸乙酯（EAA）与丁醇（BTL）的酯交换反应。采用田口优化方法研究了反应参数对BAT产率的影响。根据表征数据，这些样品是具有大量酸性位点以及多种无机和有机官能团的介孔材料，使其成为无机-有机杂化催化剂。优化结果表明，催化剂负载量对BAT产率的影响最为显著，其次是BTL : EAA摩尔比和温度，而转化时间对反应过程的影响最小。在β-酮基EAA的酯交换反应中，NH-MK10-Bpy-Mn的性能优于NH-MK10-Bpy-Zn，在110℃下反应7小时，BTL : EAA摩尔比为1.4 : 1，催化剂负载量为2.0 wt%时，转化率达到96.1±0.79%，而NH-MK10-Bpy-Zn的转化率为87.3±0.94%。两种催化剂均可重复使用并保持良好的稳定性，这表明它们在催化β-酮酯酯交换反应方面具有巨大潜力。
