光谱学与光谱分析
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磷酸二氢钾插层改性高岭土复合物的制备与表征
唐武飞,谷晓昱* ,张 胜,袁洪福,江 玉,赵静然
碳纤维及功能高分子教育部重点实验室(北京化工大学),北京 100029
Preparation and Characterization of Kaolinite-Potassium Dihydrogen Phosphate Intercalation Composite
TANG Wu-fei, GU Xiao-yu* , ZHANG Sheng, YUAN Hong-fu, JIANG Yu, ZHAO Jing-ran
Key Laboratory of Carbon Fiber and Functional Polymers, Beijing University of Chemistry Technology, Ministry of Education, Beijing 100029, China
摘要 : 实验制备了磷酸二氢钾插层改性高岭土用于新型复合阻燃材料。首先以二甲基亚砜(DMSO)为前驱体,采用超声法制备了高岭土-二甲基亚砜(K-DMSO)插层物,再将醋酸钾(KAc)取代DMSO,制备预插层体高岭土-醋酸钾(K-KAc)。最后通过第三步插层取代法,将磷酸二氢钾(KDP)引入,制备了高岭土-磷酸二氢钾(K-KDP)插层复合物,产物的插层率达到81.3%。通过红外光谱(FTIR)、X射线衍射(XRD)和扫描电子显微镜(SEM)对各步反应产物进行了表征。FTIR谱图显示,K-KDP在1 201 cm-1 出现PO的振动峰;XRD显示各步插层反应中高岭土(001)晶面特征衍射峰依次向低角度方向移动,层间距相应从0.716 nm增加到1.59 nm;SEM显示插层后的高岭土粒子分散更为均匀。
关键词 :高岭土;红外光谱;X射线衍射;扫描电子显微镜;插层
Abstract :Thepotassium dihydrogenphospiate (KDP) intercalated kaolinite (K-KDP) was prepared by a three-step reaction. Firstly, polar dimethyl sulphoxide (DMSO) was introduced into the layers of kaolinite by ultrasonic method and the product K-DMSO was obtained as precursor; secondly DMSO was replaced by potassium acetate (KAc) and the product K-KAc was gotten as intermediate; finally KAc was replaced by KDP. The intercalation ratio of the final product K-KDP reached 81.3%. The structure of products at differentreaction process was characterized by Fourier-transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM) in detail. FTIR results showed the existence of PO in the final product but moved from 1 300 to 1 201 cm-1 . XRD results documented that the interlayer spacing of kaolinite was enlarged during the whole intercalation reaction. SEM indicated that the agglomeration of kaolinite was destroyed and the particle size distribution became more uniform.
Key words :Kaolinite;Infrared spectroscopy;X-ray diffraction;Scanning electron microscope;Intercalation
收稿日期: 2013-12-31
修订日期: 2014-03-28
通讯作者:
谷晓昱
E-mail: guxy@mail.buct.edu.cn
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