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Preparation of sol–gel hybrid materials from γ-methacryloxypropyltrimethoxysilane and tetramethyl orthosilicate: study of the hydrolysis and condensation reactions

机译:由γ-甲基丙烯酰氧基丙基三甲氧基硅烷和原硅酸四甲酯制备溶胶-凝胶杂化材料:水解和缩合反应的研究

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摘要

Organic–inorganic hybrid materials suitable for\udthe development of sol–gel coatings for metallic surfaces\udwere prepared by hydrolysis and condensation of γ-\udmethacryloxypropyltrimethoxysilane (MAPTMS) and tetramethyl\udorthosilicate (TMOS). The hydrolysis of MAPTMS/\udTMOS was carried out in an ethanol/water solution. The\udprehydrolysis stage of MAPTMS/TMOS system was\udmonitored by Fourier transform infrared spectroscopy\ud(FTIR) and liquid-state 29Si and 13C nuclear magnetic\udresonance (29Si and 13C NMR). FTIR analysis indicated\udthat the hydrolysis of MAPTMS/TMOS was accomplished\udas far as the (SiOMe) band corresponding to unhydrolyzed\udsilane disappeared. The concentration of the alkoxy groups\udand the extent of self-condensation of mono-, di-, and\udtrisubstituted siloxanes (T species) in the sol were estimated\udby using liquid-state 29Si NMR spectroscopy. The hydrolysis\udof the prepared sol was also evaluated by liquid-state\ud13C NMR spectroscopy. The results indicated that under the adopted synthesis strategy conditions, the hydrolysis\udprocess requires 4 h to be completed.
机译:通过对γ-二甲基丙烯酰氧基丙基三甲氧基硅烷(MAPTMS)和四甲基/原硅酸盐(TMOS)进行水解和缩合,制备适用于金属表面溶胶-凝胶涂层的有机-无机杂化材料。 MAPTMS / udTMOS的水解在乙醇/水溶液中进行。通过傅立叶变换红外光谱法(udir)和液态29Si和13C核磁共振(29Si和13C NMR)监测MAPTMS / TMOS系统的过水解阶段。 FTIR分析表明,只要与未水解\ ud硅烷对应的(SiOMe)带消失,就完成了MAPTMS / TMOS的水解。通过使用液态29Si NMR光谱估算溶胶中烷氧基的浓度和/或单,双和三取代硅氧烷(T物种)的自缩合程度。还通过液相\ ud13C NMR光谱法评估了所制备的溶胶的水解/ ud。结果表明,在所采用的合成策略条件下,水解\ ud过程需要4小时才能完成。

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