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Role of (3-aminopropyl)tri alkoxysilanes in grafting of chlorosulphonic acid immobilized magnetic nanoparticles and their application as heterogeneous catalysts for the green synthesis of α-aminonitriles

机译:(3-氨基丙基)三烷基硅烷在氯膦酸固定化磁性纳米粒子接枝中的作用及其作为α-氨基腈的绿色合成的非均相催化剂的应用

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The surface modification of SiO _(2) coated Fe _(3) O _(4) nanoparticles by grafting silane coupling agents is a highly significant approach to enhancing the interface interaction between the inorganic magnetic core and the organic functionality to be anchored. However, the effect of the grafted molecular structure of silane, utilizing different silane alkoxy groups, has been seldom investigated on the organic–inorganic hybrid magnetic heterogeneous catalysts. The silanization was carried out on the surface of SiO _(2) coated Fe _(3) O _(4) nanoparticles using two different trialkoxy silanes, i.e. , 3-aminopropyltriethoxysilane (APTES) and 3-aminopropyltrimethoxysilane (APMES). The effect of the alkoxy silane structure anchored to the surface of silica functionalized Fe _(3) O _(4) nanoparticles on their surface area and pore volume has been analyzed by BET analyzer. The silane functionalization using APTES leads to higher surface area and pore volume than APTMS. Further, chlorosulphonic acid was immobilized on both the APTES and APTMS functionalized SiO _(2) @Fe _(3) O _(4) nanoparticles named (AE and AM), and their role as magnetically separable heterogeneous catalyst for the one pot synthesis of α-aminonitriles using water as solvent was successfully carried out. The chlorofunctionalized nanoparticles, which utilized APTES as the silanizing agent, showed better catalytic activity than APTMS in terms of reaction time and yield. The presented protocol is a water based synthesis involving room temperature conditions, along with reusability and recyclability of the catalyst. The characterization of the synthesized catalysts was carried out by using different techniques, such as FT-IR, XRD, TEM, BET, XPS, VSM and TGA-DTA.
机译:通过接枝硅烷偶联剂的SiO_(2)涂覆的Fe _(3)oα(4)α(4)纳米颗粒的表面改性是增强无机磁芯与待锚定的有机功能之间的界面相互作用的高度显着的方法。然而,利用不同的硅烷烷氧基的硅烷的接枝分子结构的效果很少研究有机 - 无机杂化磁性非均相催化剂。使用两种不同的三烷氧基硅烷,即3-氨基丙基三乙氧基硅烷(Aptes)和3-氨基丙基三甲氧基硅烷(APMES)在SiO _(2)涂覆的Fe _(3)Oα(4)α纳米颗粒表面上进行硅烷化。通过BET分析仪分析锚定在二氧化硅官能化Fe _(3)o_(3)α(4)纳米颗粒上的烷氧基硅烷结构的效果并进行了下注分析仪。使用APTES的硅烷官能化导致高度表面积和孔体积而不是APTMS。此外,将氯磺酸固定在APTES和APTMS官能化SiO _(2)@FE _(3)O _(4)纳米颗粒上(AE和AM)的纳米颗粒上,以及它们作为一个罐合成的磁性可分离的非均相催化剂的作用使用水作为溶剂的α-氨基腈进行成功进行。利用Aptes作为硅烷化剂的氯官能化纳米颗粒在反应时间和产率方面表现出比APTMS更好的催化活性。呈现的方案是涉及室温条件的基于水的合成,以及催化剂的可重用性和可再循环性。通过使用不同的技术进行合成催化剂的表征,例如FT-IR,XRD,TEM,BET,XPS,VSM和TGA-DTA。

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