微波辅助加热法合成纳米二氧化锰及其性质研究
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摘要
目的以MnSO_4和(NH_4)_2S_2O_8为原料,采用微波辅助合成制备二氧化锰。方法经水洗、过滤、干燥得到高纯纳米二氧化锰粉体。实验确定制备纳米二氧化锰的最佳工艺条件是反应质量比为4∶9,微波功率10 W,微波时间30min,经过微波干燥后的二氧化锰采用透射电镜对纳米二氧化锰进行表征。并从纳米二氧化锰用量、温度、反应物的量几个方面对双氧水降解亚甲基蓝的催化条件进行优化。结果实验结果表明,在此条件下反应得到的二氧化锰产物呈刺球状,分散性较好,满足高纯纳米二氧化锰的要求。结论在30%过氧化氢用量为25mL,50mg·L~(-1)的亚甲基蓝250mL,温度为40℃,纳米二氧化锰用量为0.2g时,合成的纳米二氧化锰对双氧水降解亚甲基蓝的催化效果较好。
Objective With MnSO_4 and(NH_4)_2S_2O_8 as raw material,to synthesize manganese dioxide precipitation by microwave-assisted heating.Methods High purity nano manganese dioxide powder was obtained by water washing,filtrating and drying.The optimum process conditions for preparation of nano manganese dioxide were as follows:the reaction mass ratio was 4∶9,the microwave power was 10 W,the microwave time was 30 min.The manganese dioxide was characterized by transmission electron microscopy after microwave drying.The advantages of the nano manganese dioxide were determined by comparing the amount of manganese dioxide,the temperature,the amount of reactants,and the common manganese dioxide.Results The results show that under the condition of the reaction,the product of manganese dioxide had the advantages of spherical shape and good dispersion.The catalytic effect of synthesis of nano manganese dioxide on the degradation of methylene blue by hydrogen peroxide was determined.Conclusion The synthesis of nano manganese dioxide has a better catalytic effect on the degradation of methylene blue by hydrogen peroxide.
Objective With MnSO_4 and(NH_4)_2S_2O_8 as raw material,to synthesize manganese dioxide precipitation by microwave-assisted heating.Methods High purity nano manganese dioxide powder was obtained by water washing,filtrating and drying.The optimum process conditions for preparation of nano manganese dioxide were as follows:the reaction mass ratio was 4∶9,the microwave power was 10 W,the microwave time was 30 min.The manganese dioxide was characterized by transmission electron microscopy after microwave drying.The advantages of the nano manganese dioxide were determined by comparing the amount of manganese dioxide,the temperature,the amount of reactants,and the common manganese dioxide.Results The results show that under the condition of the reaction,the product of manganese dioxide had the advantages of spherical shape and good dispersion.The catalytic effect of synthesis of nano manganese dioxide on the degradation of methylene blue by hydrogen peroxide was determined.Conclusion The synthesis of nano manganese dioxide has a better catalytic effect on the degradation of methylene blue by hydrogen peroxide.
引文
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[2]宋旭春,杨娥,郑遗凡,等.α-MnO2和β-MnO2纳米棒的制备和催化性能研究[J].无机化学报,2007,23(05):919-922.
[3]许乃才,马昌,王建朝,等.不同形貌氧化锰纳米材料的研究进展[J].化学通报,2010,73(08):677-683.
[4]夏熙.二氧化锰的物理、化学性质与其电化学活性的相关(1)[J].电池,2005,35(06):433-437.
[5]李素梅,朱琦,尚屹,等.纳米二氧化锰制备及在环境治理方面应用的研究进展[J].环境保护,2009,37(04):75-77.
[6]DENG R R,XIE X J,Vendrell M,et al.Intracellular gluta thione detection using MnO2nanosheet-modified upconve rsion nanoparticles[J].Journal of the American Chemical Society,2011,133(50):20168-20171.
[7]肖鸽,胡彩园,郑华均.纳米二氧化锰的制备及其应用研究[J].广东化工,2011,38(08):73-74.
[8]万传云,沈绍典,朱贤.合成路径对超级电容器用二氧化锰性质的影响[J].化学学报,2007,67(14):1559-1565.
[9]FU X B,FENG J Y,Wang H,et al.Manganese oxide hollow structures with different phases:synthesis,characterization and catalytic application[J].Catal Commun,2009,10(14):1844-1848.
[10]李英品,周晓荃,周慧静,等.纳米结构MnO2的水热合成、晶型及形貌演化[J].高等学校化学学报,2007,28(07):1223-1226.
[11]YIN B S,ZHANG S W,JIAO Y,et al.Removal of congo reddye molecules by MnO2nanorods[J].Journal of Nano-science and Nanotechnology,2014,14(09):7157-7160.
[12]许乃才,马向荣,乔山峰,等.不同晶型和形貌MnO2纳米材料的可控制备[J].化学学报,2009,67(22):2566-2572.
[13]王佳伟,陈白珍,陈亚,等.溶胶-凝胶法制备超级电容器用二氧化锰[J].电池,2012,42(05):270-273.
[14]孙洁,张莉,张文莉,等.溶胶-乳状液-凝胶法制备纳米及其催化性质研究[J].应用化工,2007,36(07):656-659.
[15]朱刚,焦宝娟,晏志军.层状二氧化锰材料的制备及其电化学性能研究[J].应用化工,2012,41(10):1735-1737.
[16]RAGUPATHY P,VASAN H,MUNICHANDRAIAH N.Synthesis and characterization of nano-MnO2for electrochemical supercapacitor studies[J].Journal of The Electrochemical Society,2008,155(01):A34-A40.
[17]彭爱国,贺周初,肖伟,等.化学二氧化锰研究进展[J].无机盐工业,2011,43(03):8-10.
[18]刘小军,刘耀鹏,闫晓前.α-MnO2纳米线的制备及其电化学性能研究[J].化学与生物工程,2011,28(04):59-61.
[19]臧李纳,赵庆琦.微波辐射法在无机化学的应用[J].中山大学研究生学刊(自然科学版),2000,21(02):77-81.