微波辅助法合成磷酸锆铜及其光催化性能  

Microwave-Assisted Preparation of Copper Zirconium Phosphate and Its Photocatalytic Activity

作　　者：赵林[1] 胡晓霞[1] 程红玉[1] 王芳[2] 李戎[3] 邢彦军[1] 

机构地区：[1]东华大学化学化工与生物工程学院,上海201620 [2]南华大学化学化工学院,湖南衡阳421001 [3]东华大学国家染整工程技术中心,上海201620

出　　处：《东华大学学报（自然科学版）》2017年第6期841-849,共9页Journal of Donghua University(Natural Science)

基　　金：国家科技支撑计划资助项目(ID2012BAK30B03);中央高校基本科研业务费专项资助项目(2232013A3-05;CUSF-DH-D-2014036)

摘　　要：采用微波辅助加热法,以ZrOCl_2、NH_4F、CuCl_2及NaH_2PO_4为原料,水为溶剂,一步法制备磷酸锆铜(CuZr(PO_4)_2·4H_2O).运用X射线衍射(XRD)、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FE-SEM)、能谱仪(EDS)、电感耦合等离子体原子发射光谱(ICP-AES)、紫外-可见漫反射光谱(UV-Vis DRS)和比表面积及孔隙分析仪(BET)等对产物的微结构、元素组成、比表面积和光学性能等进行了表征,同时考察了不同的合成条件对磷酸锆铜微观结构与形貌的影响.结果表明,当[Zr4+]=0.005mol/L,n(Cu)/n(Zr)=1,n(F)/n(Zr)=6,n(P)/n(Zr)=20,pH值为4.8时,在90℃条件下反应30min,可得到尺寸均一、由纳米片插层组成的类线团形貌的磷酸锆铜颗粒.对不同形貌的磷酸锆铜进行了光催化测试,试验结果表明,磷酸锆铜在紫外可见光的照射下对罗丹明B有一定的光催化效果,反应体系加入H2O2后,催化效率大幅提高,在pH值为5.0~9.0的条件下磷酸锆铜与H2O2表现出较好的协同催化性能.Copper zirconium phosphate （CuZr （PO4）2 ~ 4H20） was synthesized by microwave-assisted method using ZrOCI2, NH4F, CuC12 and NaH2PO4 as raw materials and water as solvent. The microstructure, elemental composition, specific surface area and optical property of copper zirconium phosphate were characterized by XRD （X-ray diffraction）, SEM （scanning electronic microscopy）, FE- SEM（field emission scanning electron microscopy）, EDS （energy dispersive spectrometer）, ICP-AES （inductively coupled plasma-atomic emission spectrometry）, UV-Vis I）RS （ultraviolet-visible diffuse reflection spectroscopy） and BET （Brunauer-Emmet-Teller） surface area. The effects of different synthetic conditions on the microstructure and morphology of copper zirconium phosphate were investigated. It is found that, when reaction condition is：[Zr4＋ ] = O. 005 mol/L, n （Cu）/n （Zr） = 1, n（F）/ n （Zr） = 6, n （P） / n （Zr） = 20, pH = 4.8, 90℃ and 30 min, nanoslices being assembled coil-like with uniform size can be obtained. The photocatalytic properties of copper zirconium phosphate with different morphologies were evaluated by degrading rhodamine B （RhB）. The results reveal that CuZr（PO4）2 exhibit a little photocatalytic activity under ultraviolet visible light, the catalytic efficiency enhances obviously with the addition of H2O2. The system behaves an excellent photocatalytic activity at pH values from 5.0 to 9.0.

关 键 词：磷酸锆铜 微波辅助法 光催化 

分 类 号：TQ174[化学工程—陶瓷工业]