Influence on the structure and methylene blue adsorption of graphite oxide prepared by three modified Hummers methods
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摘要: 采用三种改性Hummers法制备氧化石墨（GO-1、GO-2和GO-3），利用X射线衍射（X-ray diffraction，XRD）、傅里叶变换红外光谱（Fourier transform infrared spectroscopy，FT-IR）、扫描电子显微镜（scanning electron microscopy，SEM）等多种分析手段对不同方法制备的氧化石墨的结构及性能进行表征，并研究了不同制备方法对氧化石墨吸附亚甲基蓝性能的影响。结果表明：氧化剂KMnO4用量的增加和低温氧化时间的增大有助于氧化石墨层间距的增大，其中氧化剂KMnO4用量对层间距的影响较大。氧化剂KMnO4用量的增多会导致含氧官能团的增多，导致氧化石墨表面形貌褶皱的增多，最终造成层间距的增大，但是当氧化剂KMnO4用量过多时，相邻表面的含氧官能团会发生交联，会造成氧化石墨的堆叠。GO-1对亚甲基蓝的去除效率比GO-2、GO-3分别高11.14%和23.21%，含氧官能团的增多有助于氧化石墨对亚甲基蓝的吸附。Abstract: Graphite oxide (GO) was prepared by three improved Hummers methods (GO-1, GO-2, and GO-3). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM), and the effects of different preparation methods on the adsorption of methylene blue by GO were studied. The results indicate that, with the increase of oxidant KMnO4dosage and the extension of low temperature oxidation time, GO interlayer spacing gradually increases, in which the dosage of oxidant KMnO4has a greater influence on the interlayer spacing. The increase of oxidant KMnO4dosage will lead to the increase of oxygen-bearing functional groups and GO surface wrinkle, eventually resulting in an enlarge in the interlayer spacing. However, when the oxidant KMnO4is overdosed, the adjacent surface of oxygen-bearing functional groups will be cross-linked, resulting in the stack of GO. Compared with GO-2 and GO-3, the removal efficiency of GO-1 to methylene blue is higher than that of GO-2 and GO-3 by 11.14% and 23.21%, respectively, indicating that the increase in oxygen-bearing functional groups will contribute to the adsorption of methylene blue on GO.
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Key words:
- graphite oxide /
- Hummers methods /
- KMnO4 /
- methylene blue
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图 1 不同方法制备的氧化石墨X射线衍射光谱
Figure 1. X-ray diffraction patterns of GO prepared by different methods
图 2 不同方法制备的氧化石墨傅里叶变换红外光谱图
Figure 2. FT–IR patterns of GO prepared by different methods
图 3 不同方法制备的氧化石墨扫描电子显微形貌：（a）GO-1；（b）GO-2；（c）GO-3
Figure 3. SEM of GO by different methods: (a) GO-1; (b) GO-2; (c) GO-3
图 4 不同方法制备的氧化石墨对亚甲基蓝的去除效率
Figure 4. Removal efficiency of methylene blue by GO prepared by different methods
表 1 三种氧化石墨制备方法参数比较
Table 1. Preparation parameter comparison of graphite oxide in three improved Hummers methods
试样 KMnO4用量/ g 低温反应时间/ h 高温反应温度/ ℃ GO-1 8 6 80 GO-2 3 1 98 GO-3 6 17 98 注：表中KMnO4用量为单位质量石墨所对应的氧化剂KMnO4用量。 
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表 2 不同方法制备的氧化石墨的傅里叶变换红外光谱图数据（波数）
Table 2. FT–IR pattern data of GO prepared by different methods
cm-1 试样 –OH伸缩振动 C=O伸缩振动 H2O变形振动C=C伸缩振动 –OH面内弯曲振动 C–OH伸缩振动 C–O–C伸缩振动 苯的间位二取代弯曲振动 GO-1 3382 1738 1625 1287 1174 1008 881 GO-2 3188 1740 1643 1394 1079 ― ― GO-3 3419 1738 1648 1388 1100 ― ―
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[1] Zhang G X. Effects of copper-coated graphite content and particle size on properties of the Cu/copper-coated graphite composite. Powder Metall Technol, 2016, 34(3): 196 doi: 10.3969/j.issn.1001-3784.2016.03.007张国玺. 石墨含量及粒度对铜–镀铜石墨复合材料性能的影响. 粉末冶金技术, 2016, 34(3): 196 doi: 10.3969/j.issn.1001-3784.2016.03.007 [2] Sun J P. The Application of Graphene Oxide Complex in Heavy Metal Ions Extraction[Dissertation]. Beijing: Tsinghua University, 2015孙杰萍. 氧化石墨烯复合材料在重金属离子分离中的应用[学位论文]. 北京: 清华大学, 2015 [3] Jeong H K, Lee Y P, Lahaye R J W E, et al. Evidence of graphitic AB stacking order of graphite oxides. J Am Chem Soc, 2008, 130(4): 1362 doi: 10.1021/ja076473o [4] Yin F, Chen D Z, Liu J J, et al. Preparation technology and thermostability of graphite oxide. J Mater Sci Eng, 2013, 31(3): 336 https://www.cnki.com.cn/Article/CJFDTOTAL-CLKX201303004.htm尹芳, 陈迪钊, 刘佳佳, 等. 氧化石墨烯的制备工艺及热稳定性. 材料科学与工程学报, 2013, 31(3): 336 https://www.cnki.com.cn/Article/CJFDTOTAL-CLKX201303004.htm [5] Zhou X Y. Microwave-Assisted Systhesis of Metal Oxide/Graphene Nanocomposite and Their Application as Anode Material for Lion Batteries[Dissertation]. Zhejiang: Zhejiang Normal University, 2015周小燕. 金属氧化物/石墨烯纳米复合材料的微波法制备及在锂离子电池负极材料上的应用[学位论文]. 浙江: 浙江师范大学, 2015 [6] Zhou W B. Study on the Preparation and Property of Several Inorganic Nanoparticles/Graphene (Oxide) Composites[Dissertation]. Nanjing: Nanjing University of Science and Technology, 2011邹文斌. 几种无机纳米粒子/(氧化)石墨烯复合材料的制备及性能研究[学位论文]. 南京: 南京理工大学, 2011 [7] Bai H W. The Heat Resistance of Silicone Resin Modified by Graphene Oxide[Dissertation]. Harbin: Harbin Institute of Technology, 2012白惠文. 氧化石墨烯改性有机硅树脂耐热性的研究[学位论文]. 哈尔滨: 哈尔滨工业大学, 2012 [8] Feng M Z, Peng T J, Sun H J, et al. Effect of oxidation degree on structure and cation exchange capacity of graphite oxide. Chin J Inorg Chem, 2016, 32(3): 427 https://www.cnki.com.cn/Article/CJFDTOTAL-WJHX201603007.htm冯明珠, 彭同江, 孙红娟, 等. 氧化程度对氧化石墨结构与阳离子交换容量的影响. 无机化学学报, 2016, 32(3): 427 https://www.cnki.com.cn/Article/CJFDTOTAL-WJHX201603007.htm [9] Yang Y S, Zhang B, Zhang Y P. Preparation and application research in composite of graphene oxide. Appl Chem Ind, 2013, 42(6): 1138 https://www.cnki.com.cn/Article/CJFDTOTAL-SXHG201306051.htm杨云裳, 张彬, 张应鹏. 氧化石墨烯的制备及在复合材料中的应用研究进展. 应用化工, 2013, 42(6): 1138 https://www.cnki.com.cn/Article/CJFDTOTAL-SXHG201306051.htm [10] Liu Z T. Manipulation of Surface Chemistry and Properties of Graphene and its Oxide[Dissertation]. Shanghai: East China University of Science and Technology, 2014刘芝婷. 石墨烯及其氧化物的表面结构和性质的调控[学位论文]. 上海: 华东理工大学, 2014 [11] Fu L. The Research on Synthesis, Characterization and Application of Grpaheite Oxide and Poylpyorrle/Grpaheit Oxide Nanocomposites[Dissertation]. Hunan: Hunan University, 2005傅玲. 氧化石墨和聚吡咯/氧化石墨纳米复合材料的制备、表征及应用研究[学位论文]. 湖南: 湖南大学, 2005 [12] Shao G L. The Preparation and Characterization of Graphene Oxide[Dissertation]. Shanghai: Donghua University, 2012邵桂林. 氧化石墨烯的制备与表征[学位论文]. 上海: 东华大学, 2012 [13] Bi C G. Synthesis and Characterization of Graphene Oxides and Their Composites[Dissertation]. Liaoning: Dalian University of Technology, 2014毕朝刚. 氧化石墨烯及其复合物的制备与表征[学位论文]. 辽宁: 大连理工大学, 2014 [14] Hummers Jr W S, Offeman R E. Preparation of graphitic oxide. J Am Chem Soc, 1958, 80(6): 1339 doi: 10.1021/ja01539a017 [15] Liu Y Z. Synthesisi of Magnetic Graphene Oxide and Research of its Abosorption Behavior[Dissertation]. Hebei: Yanshan University, 2015刘亚洲. 磁性氧化石墨烯复合材料的制备及其吸附性能的研究[学位论文]. 河北: 燕山大学, 2015 [16] Guo S. Preparation of Fe2O3/Graphene Oxide Catalyst and its Adsorption and Photo-Fenton Degradation of Organic Contaminants[Dissertation]. Hubei: Wuhan University of Technology, 2013郭盛. 新型Fe2O3/氧化石墨烯催化剂的制备及其吸附与可见光Fenton降解有机污染物的研究[学位论文]. 湖北: 武汉理工大学, 2013 [17] Peng Z. Studies on the Preparation and Properties of Graphene Oxide Nanocomposites[Dissertation]. Henan: Henan University, 2013彭展. 氧化石墨烯纳米复合材料的制备及其性能的研究[学位论文]. 河南: 河南大学, 2013 -
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