Miao Yuanyuan, Wang Xiuya, Liu Yixing, Liu Zhenbo, Chen Wenshuai
Key Laboratory of Bio-Based Material Science & Technology, Northeast Forestry University, Ministry of Education, Harbin 150040, China.
Polymers (Basel). 2021 Dec 19;13(24):4453. doi: 10.3390/polym13244453.
The Hummers method is the most commonly used method to prepare graphene oxide (GO). However, many waste acids remain in the raw reaction mixture after the completion of this reaction. The aim of this study was to reuse these waste acids efficiently. In this study, microcrystalline cellulose (MCC) was directly dissolved in the mixture after the high-temperature reaction of the Hummers method. The residual acid was used to hydrolyze MCC, and the graphene oxide/microcrystalline cellulose (GO/MCC) composites were prepared, while the acid was reused. The effects of MCC addition (0.5 g, 1.0 g, and 1.5 g in 20 mL) on the properties of the composites were discussed. The structure, composition, thermal stability, and hydrophobicity of GO/MCC composites were characterized and tested by SEM, XRD, FTIR, TG, and contact angle tests. The results showed that MCC could be acid hydrolyzed into micron and nano-scale cellulose by using the strong acidity of waste liquid after GO preparation, and it interacted with the prepared GO to form GO/MCC composites. When the addition amount of MCC was 1 g, the thermal stability of the composite was the highest due to the interaction between acid-hydrolyzed MCC and GO sheets. At the same time, the hydrophobic property of the GO/MCC composite is better than that of the GO film. The freeze-dried GO/MCC composites are more easily dispersed in water and have stronger stability.
哈默斯法是制备氧化石墨烯(GO)最常用的方法。然而,该反应完成后,原始反应混合物中会残留许多废酸。本研究的目的是有效再利用这些废酸。在本研究中,微晶纤维素(MCC)在哈默斯法高温反应后的混合物中直接溶解。利用残留的酸水解MCC,制备了氧化石墨烯/微晶纤维素(GO/MCC)复合材料,同时实现了酸的再利用。讨论了MCC添加量(20 mL中分别添加0.5 g、1.0 g和1.5 g)对复合材料性能的影响。通过扫描电子显微镜(SEM)、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、热重分析(TG)和接触角测试对GO/MCC复合材料的结构、组成、热稳定性和疏水性进行了表征和测试。结果表明,利用制备GO后废液的强酸性可将MCC酸水解为微米级和纳米级纤维素,其与制备的GO相互作用形成GO/MCC复合材料。当MCC添加量为1 g时,由于酸水解的MCC与GO片层之间的相互作用,复合材料的热稳定性最高。同时,GO/MCC复合材料的疏水性能优于GO膜。冻干的GO/MCC复合材料更易分散于水中且具有更强的稳定性。