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ε-Caprolactone polymerization using titanium complexes immobilized onto silica based materials functionalized with ionic liquids: insights into steric, electronic and support effects

机译:ε-己内酯聚合使用固定在用离子液体官能化的二氧化硅基材料上的钛配合物:洞察空间,电子和支持效应

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Heterogeneous catalysts comprised of titanium immobilized on silica imidazolium-based systems have been synthesized for the ring opening polymerization of ε-caprolactone. Titanium isopropoxide as a metallic precursor was grafted onto ionic liquid-functionalized silica surfaces or alternatively first grafted onto silica followed by reaction with 1-methyl-3-[(triethoxysilyl)propyl]imidazolium chloride. These materials have been characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), N _(2) adsorption–desorption, transmission electron microscopy (TEM) with microanalysis by energy-dispersive X-ray (EDX), ~(29) Si, ~(13) C and ~(49/47) Ti solid-state NMR spectroscopy (MAS NMR), Fourier-transform infrared spectroscopy (FT-IR), UV-vis diffuse reflectance spectroscopy (DRUV-vis), thermogravimetric analysis (TG-DTG) and solid state electrochemical techniques. Different ionic liquid compounds have been tested with different silica supports (mesoporous silica nanoparticles, SBA-15 and high surface area silica). Thus, the effect of the ionic liquid in the chemical environment of the anchored titanium complex has been determined. In addition, the stability and reusability of the catalysts have been studied.
机译:已经合成了由固定在基于二氧化硅咪唑鎓的系统上的钛的异质催化剂用于ε-己内酯的开环聚合。作为金属前体的钛异丙氧化物接枝到离子液体官能化的二氧化硅表面上或者首先接枝到二氧化硅上,然后与1-甲基-3 - [(三乙氧基甲硅烷基)丙基反应咪唑氯化物。这些材料的特征在于X射线衍射(XRD),X射线荧光(XRF),N _(2)吸附 - 解吸,透射电子显微镜(TEM)通过能量分散X射线(EDX), 〜(29)Si,〜(13)C和〜(49/47)TI固态NMR光谱(MAS NMR),傅立叶变换红外光谱(FT-IR),UV-VI扩散反射光谱(DRUV-Vis ),热重分析(TG-DTG)和固态电化学技术。已经用不同的二氧化硅载体(中孔二氧化硅纳米粒子,SBA-15和高表面积二氧化硅)测试了不同的离子液体化合物。因此,已经确定了离子液体在锚定钛络合物的化学环境中的影响。此外,已经研究了催化剂的稳定性和可重用性。

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