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Analytical assessment to develop innovative nanostructured BPA-free epoxy-silica resins as multifunctional stone conservation materials
Science of the Total Environment ( IF 9.8 ) Pub Date : 2018-07-19 , DOI: 10.1016/j.scitotenv.2018.07.188
Olivia Gómez-Laserna , Paola Lanzafame , Georgia Papanikolaou , María Ángeles Olazabal , Sandra Lo Schiavo , Paola Cardiano

Bisphenol A (BPA)-free epoxy resins, synthesized from low molecular weight cycloaliphatic compounds, may represents promising materials for stone conservation due to their very appealing and tunable physico-chemical properties, such as viscosity, curing rate and penetration ability, being also easy to apply and handle. Furthermore, alkoxysilanes have been widely employed as inorganic strengtheners since they are easily hydrolysed inside lithic substrates affording SiO linkages with the stone matrix. Taking into account the advantages of these two classes of materials, this work has been focused on the development of innovative conservation materials, based on hybrid epoxy-silica BPA-free resins obtained by reaction of 1,4-cycloexanedimethanol diglycidylether (CHDM-DGE) with various siloxane precursors, i.e. glycidoxypropylmethyldiethoxysilane (GPTMS), tetraethyl orthosilicate (TEOS) and isobutyltrimethoxysilane (iBuTMS), using the 1,8-diaminooctane (DAO) as epoxy hardener. Thanks to Raman spectroscopy the synthesis processes have been successfully monitored, allowing the identification of oxirane rings opening as well as the formation of the cross-linked organic-inorganic networks. In accordance with the spectroscopic data, the thermal studies carried out by TGA and DSC techniques have pointed that GPTMS is a suitable siloxane precursor to synthesize the most stable samples against temperature degradation. GPTMS-containing resins have also shown good performances in the dynamic mechanical analysis (DMA) and in contact angle investigations, with values indicating considerable hydrophobic properties. SEM analyses have highlighted a great homogeneity over the entire observed areas, without formations of clusters and/or aggregates bigger than 45 μm, for the cited materials, confirming the efficiency of GPTMS as coupling agent to enhance the organic/inorganic interphase bonding. The variations provided by the incorporation of nanostructured titania, specifically synthesized, inside the epoxy-silica hybrids have been also evaluated. According to all the collected results, the hybrid materials here reported have proven to be promising multifunctional products for potential application in the field of stone conservation.



中文翻译:

进行分析评估以开发创新的不含BPA的纳米结构环氧硅树脂作为多功能石材保护材料

低分子量脂环族化合物合成的不含双酚A(BPA)的环氧树脂,由于其极具吸引力和可调节的物理化学特性(例如粘度,固化速率和渗透能力)也很容易代表着石材保护的有希望的材料。申请和处理。此外,烷氧基硅烷由于容易在提供硅的硅酸盐基片内部水解而被广泛用作无机增强剂。O与石材基质的连接。考虑到这两类材料的优势,这项工作一直专注于开发创新的保护材料,该材料基于通过1,4-环己二甲醇二缩水甘油醚(CHDM-DGE)反应获得的无环氧-二氧化硅双BPA的杂化树脂。使用1,8-二氨基辛烷(DAO)作为环氧固化剂,可与各种硅氧烷前体(即环氧丙氧基丙基甲基二乙氧基硅烷(GPTMS),原硅酸四乙酯(TEOS)和异丁基三甲氧基硅烷(iBuTMS))结合使用。谢谢拉曼光谱法已经成功地监测了合成过程,从而可以识别环氧乙烷环的开环以及形成交联的有机-无机网络。根据光谱数据,通过TGA和DSC技术进行的热研究表明,GPTMS是合适的硅氧烷前体,可以合成最稳定的样品以防止温度下降。含GPTMS的树脂在动态力学分析(DMA)和接触角研究中也显示出良好的性能,其值表明具有相当大的疏水性。扫描电镜分析突出显示了极大的同质性对于所引用的材料,在整个观察区域中都没有形成大于45μm的簇和/或聚集体,这证实了GPTMS作为偶联剂增强有机/无机相间键合的效率。还评估了在环氧-二氧化硅杂化物内部掺入专门合成的纳米结构二氧化钛所产生的变化。根据所有收集到的结果,此处报道的杂化材料已被证明是有前途的多功能产品,有望在石材保护领域应用。

更新日期:2018-07-20
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