超细高岭石纳米片制备参数及片层结构优化  

Optimization of Preparation Parameters and Layer Structure of Kaolinite Nanosheets

作　　者：王雪松 赵雪淞 张雨涵 张婷 王力恒 靳荟怡 WANG Xuesong;ZHAO Xuesong;ZHANG Yuhan;ZHANG Ting;WANG Liheng;JIN Huiyi(School of Materials Science and Engineering,Liaoning Technical University,Fuxin 123000,Liaoning,China;College of Science,Liaoning Technical University,Fuxin 123000,Liaoning,China;College of Mining,Liaoning Technical University,Fuxin 123000,Liaoning,China;College of Environmental Science and Engineering,Liaoning Technical University,Fuxin 123000,Liaoning,China;The School of Humanities and Social Sciences,North University of China,Taiyuan 030000,China)

机构地区：[1]辽宁工程技术大学材料科学与工程学院,辽宁阜新123000 [2]辽宁工程技术大学理学院,辽宁阜新123000 [3]辽宁工程技术大学矿业学院,辽宁阜新123000 [4]辽宁工程技术大学环境科学与工程学院,辽宁阜新123000 [5]中北大学人文社会科学学院,太原030000

出　　处：《硅酸盐学报》2024年第12期3761-3771,共11页Journal of The Chinese Ceramic Society

基　　金：辽宁省教育厅科学研究项目(LJKZ0328);辽宁省教育厅理工类项目(JYTMS20230806)。

摘　　要：高岭石纳米片作为一种2D纳米材料,原料廉价易得,在涂料、生物医药以及复合材料等领域的需求日益增加。本研究采用一种新颖的二甲基亚砜(DMSO)插层–球磨剥片–超声分散–微波干燥工艺,成功制备出晶形完整、片层薄、比表面积大的高岭石纳米片,DMSO插层和球磨剥片优化参数为:插层温度66℃、插层时间400 min、DMSO和H2O的体积比为30:3、球磨时间3.1 h、球磨转速300 r·min^(–1)、六偏磷酸钠添加量0.22 g,该条件下制得超细高岭石纳米片平均粒径为0.77μm。X射线衍射、Fourier变换红外光、比表面积、扫描电子显微镜和原子力显微镜表征分析显示DMSO分子与高岭石内表面羟基成键,而球磨剥片后保持了高岭石的基本晶体结构,超细高岭石纳米片层厚降低至15 nm左右,片层分布均匀且晶形保持良好,比表面积扩大到原来的近3倍(9.28~26.62 m^(2)·g^(–1))。DMSO插层高岭石可以在保持高岭石基本晶形的同时显著降低其层间作用力,低速球磨使高岭石片层分离的同时保持了完整的片层结构。Introduction Kaolinite as one of the most widely distributed and commonly utilized minerals has an increasing demand in various fields,including coatings,adsorption,catalysis,rubber,and biomedicine.The utilization of kaolinite is affected by various factors like particle size,layer thickness,and specific surface area.Kaolinite nanosheets as a type of two-dimensional(2D)nanomaterial exhibit novel properties that encompass quantum size effects,surface effects,small size phenomena,as well as macroscopic quantum tunneling effects.The existing preparation process of kaolinite nanosheets has some notable challenges,including high thickness,small specific surface area,and severe damage to the crystal structure,all of which constrain their potential applications in industries.This study introduced a process for the preparation of kaolinite nanosheets,including dimethyl sulfoxideintercalation,ball milling exfoliation,ultrasonic dispersion,and microwave drying techniques.The structural and morphological changes of kaolinite during the DMSO intercalation and subsequent ball milling exfoliation processes were analyzed.Methods Initially,kaolinite of 5 g was accurately weighed and thoroughly ground in an agate mortar.Afterwards,the ground powder was mixed with 30 ml of DMSO and distilled water in a 100 ml beaker.The mixed suspension in the beaker was stirred magnetically at 66℃for 400 min.After the suspension was centrifugated,the subsequent precipitate was subjected in an oven at 90℃to yield the DMSO-kaolinite intercalation complex(DK).Subsequently,the DK of 10 g was mixed with 20 ml of distilled water.The mixed suspension with sodium hexametaphosphate as a dispersant was ground in a planetary ball mill with zirconia balls of 1–3 mm at 300r·min^(–1)for 3 h.The resulting ground suspension was centrifuged at 4000 r·min^(–1)for 5 min,and the precipitate was rinsed with ethanol for three times.Finally,the sample was placed in a microwave dryer at 700 W for 10 min,yielding kaolinite nanosheets(BDK).The structural and m

关 键 词：高岭石 二甲基亚砜 插层 球磨剥片 纳米片 

分 类 号：TD985[矿业工程—选矿]