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Surface Modification of Cellulose Nanocrystals with Succinic Anhydride

机译:琥珀酸酐对纤维素纳米晶体的表面修饰

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摘要

The surface modification of cellulose nanocrystals (CNC) is a key intermediate step in the development of new functionalities and the tailoring of nanomaterial properties for specific applications. In the area of polymeric nanocomposites, apart from good interfacial adhesion, the high thermal stability of cellulose nanomaterial is vitally required for the stable processing and improvement of material properties. In this respect, the heterogeneous esterification of CNC with succinic anhydride was investigated in this work in order to obtain CNC with optimised surface and thermal properties. The influence of reaction parameters, such as time, temperature, and molar ratio of reagents, on the structure, morphology and thermal properties, were systematically studied over a wide range of values by DLS, FTIR, XPS, WAXD, SEM and TGA methods. It was found that the degree of surface substitution of CNC increased with the molar ratio of succinic anhydride to cellulose hydroxyl groups (SA:OH), as well as the reaction time, whilst the temperature of reaction showed a moderate effect on the degree of esterification in the range of 70–110 °C. The studies on the thermal stability of modified nanoparticles indicated that there is a critical extent of surface esterification below which only a slight decrease of the initial temperature of degradation was observed in pyrolytic and oxidative atmospheres. A significant reduction of CNC thermal stability was observed only for the longest reaction time (240 min) and the highest molar ratio of SA:OH. This illustrates the possibility of manufacturing thermally stable, succinylated, CNC by controlling the reaction conditions and the degree of esterification.
机译:纤维素纳米晶体(CNC)的表面改性是开发新功能以及针对特定应用定制纳米材料性能的关键中间步骤。在聚合物纳米复合材料领域,除了良好的界面粘合性,纤维素纳米材料的高热稳定性对于稳定加工和改善材料性能至关重要。在这方面,在这项工作中研究了CNC与琥珀酸酐的异质酯化,以获得具有最佳表面和热性能的CNC。通过DLS,FTIR,XPS,WAXD,SEM和TGA方法,系统地研究了反应参数(例如时间,温度和试剂的摩尔比)对结构,形态和热性能的影响,涉及的范围很广。发现随着琥珀酸酐与纤维素羟基的摩尔比(SA:OH)以及反应时间的增加,CNC的表面取代度增加,而反应温度对酯化度显示出适度的影响。温度范围为70–110°C。对改性纳米粒子的热稳定性的研究表明,存在表面酯化的临界程度,在此以下,在热解和氧化气氛中仅观察到降解的初始温度略有降低。仅在最长的反应时间(240分钟)和最高的SA:OH摩尔比下,才观察到CNC热稳定性的显着降低。这说明了通过控制反应条件和酯化程度来制造热稳定的琥珀酰化CNC的可能性。

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