过硫酸钾插层膨胀-氧化法制备高阳离子交换容量氧化石墨及表征  

Preparation and Characterization of Graphite Oxide with High Cation Exchange Capacity by a Potassium Persulfate Intercalation Expansion-Oxidation Method

作　　者：张曦月 孙红娟[1,2] 彭同江[2,3] 王娅 ZHANG Xi-Yue;SUN Hong-Juan;PENG Tong-Jiang;WANG Ya(School of Resources and Enwironment,Southwest University of Science and Technology,Mianyang,Mianyang 621010,China;Institute of Mineral Materials&Applications,Southwest University of Science and Technology,Mianyang 621010,China;Center of Forecasting and Analysis,Southwest Uniwersity of Science and Technology,Mianyang 621010,China)

机构地区：[1]西南科技大学环境与资源学院,绵阳621010 [2]西南科技大学矿物材料及应用研究所,绵阳621010 [3]西南科技大学分析测试中心,绵阳621010

出　　处：《应用化学》2021年第7期816-824,共9页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(No.41772036);四川省重点研发项目(No.2018GZ0135);西南科技大学研究生创新基金(No.19ycx0046)资助。

摘　　要：以过硫酸钾为插层膨胀剂,高锰酸钾为氧化剂,采用膨胀-氧化一步法制备了具有高阳离子交换容量的氧化石墨(GO)。采用扫描电子显微镜、X射线衍射、傅里叶变换红外光谱和X射线光电子能谱对样品的形貌、结构、含氧官能团的种类及含量进行表征。结果表明,过硫酸钾插层膨胀处理能有效抑制GO的过氧化现象,获得片层更轻薄、氧化程度更均匀的GO。随过硫酸钾用量的增加,GO结构中的羟基与环氧基的相对含量比、羧基的相对含量均增大,GO的阳离子交换容量也随之增大,但当过硫酸钾用量过高,插层膨胀后的石墨浮在浓硫酸表面形成厚层,阻碍了后续氧化剂与样品的充分接触,反而使羟基与环氧基的相对含量比降低,导致阳离子交换容量减小。当过硫酸钾与石墨质量比为5∶1时,获得高氧化程度且氧化均匀的GO,此时羟基与环氧基的相对含量比最高,GO的阳离子交换容量为579.5 mmol/100 g。Graphite oxide(GO)with high cation exchange capacity was prepared with potassium persulfate as the expansion agent and potassium permanganate as the oxidant by an expansion-oxidation method in one step.Scanning electron microscopy,X-ray diffraction,Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy were used to characterize the morphology,structure,and the type and content of oxygen containing functional groups of the samples.As a result,the intercalating expansion treatment with K2S2O8 could effectively inhibit the peroxide phenomenon of GO,making the slice layer thinner and the oxidation degree more evenly.With the increase of potassium persulfate dosage,the ratio of epoxy groups to hydroxyl and the relative content of carboxyl in the structure of GO increases,so does the cation exchange capacity.However,when the dosage of potassium persulfate is too high,the ratio of epoxy groups to hydroxyl becomes lower,leading to the decrease of the cation exchange capacity.When the mass ratio of potassium persulfate to graphite is 5∶1,the obtained GO has a high degree of oxidation and a more uniform oxidation,and the ratio of hydroxyl group to epoxy group is the highest.The cation exchange capacity of GO is 579.5 mmol/100 g.

关 键 词：氧化石墨 过硫酸钾 膨胀-氧化一步法 含氧官能团 阳离子交换容量 

分 类 号：O613[理学—无机化学]