Synthesis of Hybrid Cellulose Acetate Membranes and Application of the Flynn-Wall-Ozawa Isoconversional Method

Gesiane Mendonça Ferreira, Daniella Herdi Cariello, Filipi França dos Santos, Kelly Cristine Da Silveira, Maria Clara Gonçalves, Mônica Calixto Andrade
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Abstract

The synthesis of hybrid materials is a promising alternative in the production of materials with optimized properties. In this context, the classic cellulose acetate membranes are being modified. It is worth mentioning that knowing the thermal stability of cellulosic materials is an essential factor in their use since organic polymers have low thermal resistance, limiting their applicability. This work evaluates the synthesis and the study of the thermal degradation kinetics of hybrid cellulose acetate membranes. The synthesis was carried out using the sol-gel process, with the phase inversion technique, through the reaction of cellulose acetate with organometallic precursors: tetraethyl orthosilicate, TEOS; 3-aminopropyl triethoxysilane, APTES, and titanium isopropoxide, TiPOT, in fixed composition. Thermal characterization was performed with thermogravimetric analysis at different heating rates under a nitrogen atmosphere. The kinetic parameter of thermal decomposition activation energy, Ea, was estimated with the isoconversional method proposed by Flynn-Wall-Ozawa (FWO). The degradation kinetics shows that the change in the chemical composition of the samples directly interferes with their thermal properties. Thus, it is possible to observe that the activation energy found for the reference sample, AC-Pure, in the first and second batches was 233.5 and 219.05 kJ/mol, respectively. The composition modification results in an increase in activation energy, in which sample B0//100-30 recorded 310.31 and 226.05 kJ/mol in the first and second batches; and sample B100//0-30 reached 452.73 and 424.74 kJ/mol. It is clear that the increase in the thermal resistance of the samples is associated with the change in the chemical composition and must be attributed to the increase in the TEOS content in the composition due to the formation and increase in the presence of siloxane groups in the material.
混合醋酸纤维素膜的合成及 Flynn-Wall-Ozawa 等转化法的应用
混合材料的合成是生产具有优化性能的材料的一种很有前途的替代方法。在这种情况下,传统的醋酸纤维素膜正在被改良。值得一提的是,了解纤维素材料的热稳定性是使用这些材料的一个重要因素,因为有机聚合物的热阻较低,限制了其适用性。本研究评估了混合醋酸纤维素膜的合成和热降解动力学研究。合成采用了溶胶-凝胶工艺和相反转技术,通过醋酸纤维素与有机金属前体(原硅酸四乙酯(TEOS)、3-氨基丙基三乙氧基硅烷(APTES)和异丙醇钛(TiPOT))在固定成分下的反应进行。在氮气环境下,以不同的加热速率通过热重分析进行了热表征。热分解活化能的动力学参数 Ea 是用 Flynn-Wall-Ozawa (FWO) 提出的等转化法估算的。降解动力学表明,样品化学成分的变化会直接影响其热学特性。因此,我们可以观察到,在第一批和第二批样品中,参考样品 AC-Pure 的活化能分别为 233.5 和 219.05 kJ/mol。成分改变导致活化能增加,其中样品 B0//100-30 在第一批和第二批中的活化能分别为 310.31 和 226.05 kJ/mol;样品 B100//0-30 的活化能分别为 452.73 和 424.74 kJ/mol。显然,样品热阻的增加与化学成分的变化有关,必须归因于材料中硅氧烷基团的形成和增加导致成分中 TEOS 含量的增加。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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