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Ultrasonic-assisted green synthesis of beta-amino carbonyl compounds by copper oxide nanoparticles decorated phosphate functionalized graphene oxide via Mannich reaction

机译:通过甘料反应用氧化铜纳米粒子装饰磷化官能化石墨烯氧化物的超声波辅助绿色合成β-氨基羰基化合物

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facile chemical synthetic route has been demonstrated for the synthesis of copper oxide nanoparticles decorated phosphate functionalized graphene oxide (CuO/PGO). The synthesized nanocatalyst was used as an efficient and active candidate for the synthesis of beta-amino carbonyl compounds via a green synthetic ultrasonic route. The structural properties of the samples were investigated by means of a number of sophisticated techniques like X-ray diffraction (XRD), Fourier-transform Infrared (FTIR) spectroscopy, High Resolution Transmission Electron Microscope (HRTEM), N-2 adsorption-desorption measurements, X-ray photoelectron spectroscopy (XPS) analysis, Ammonia temperature programmed desorption analysis (NH3-TPD) and Raman spectroscopy. HRTEM analysis confirmed the presence of spherical CuO nanoparticles distributed uniformly throughout the PGO surface. XPS analysis demonstrated the presence of Cu2+ species and minor reduction of oxygen functional groups on GO. A higher surface area of 162 m(2)/g for CuO/PGO was found from N-2 adsorption-desorption isotherms. Later on, the presence of acidic groups on CuO/PGO that play an essential role in the catalytic activity was examined by NH3-TPD and pyridine adsorbed IR analysis. The total acidity on the surface of synthesized nanocatalyst was found to be of 0.59 mmol g(-1) which includes both Lewis as well as Bronsted acidic sites. A higher product yield of 95% in a shorter period of time of 15 min was achieved which is superior to many reported catalytic systems. A combined strategy involving greener and easier ultrasonic route and use of an efficient acidic graphene oxide-based catalyst resulted in higher catalytic activity and stability with good recyclability.
机译:已经证明了容易化学合成途径用于合成氧化铜纳米颗粒装饰磷酸官能化石墨烯氧化物(CUO / PGO)。合成的纳米催化剂通过绿色合成超声途径用作合成β-氨基羰基化合物的有效和活性候选者。通过X射线衍射(XRD),傅里叶变换红外(FTIR)光谱,高分辨率透射电子显微镜(HRTEM),N-2吸附 - 解吸测量等多种复杂技术来研究样品的结构性质,X射线光电子能谱(XPS)分析,氨温度编程解吸分析(NH3-TPD)和拉曼光谱。 HRTEM分析证实了在整个PGO表面均匀分布的球形CuO纳米颗粒的存在。 XPS分析证明了Cu2 +物种的存在,并在去上进行氧官能团的轻微减少。从N-2吸附 - 解吸等温线中发现了CuO / Pgo的162m(2)/ g的较高表面积。后来,通过NH 3 -TPD和吡啶吸附的红外线分析检查在催化活性中发挥基本作用的CuO / PGO上的酸性基团的存在。发现合成纳米催化剂表面上的总酸度为0.59mmol g(-1),其包括Lewis以及富棱镜酸性位点。实现了15分钟的较短时间的较高产量95%,其优于许多报道的催化系统。涉及更环保和更容易超声波途径的组合策略以及使用有效的酸性石墨烯氧化物基催化剂,导致催化活性较高,稳定性具有良好的再循环性。

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