无机材料学报 ›› 2011, Vol. 26 ›› Issue (3): 321-326.DOI: 10.3724/SP.J.1077.2011.00321 CSTR: 32189.14.SP.J.1077.2011.00321

• 研究论文 • 上一篇    下一篇

常压回流条件下拉锰矿的合成及其影响因素

殷 辉,刘 凡,冯雄汉, 谭文峰,邱国红, 陈秀华,刘名茗   

  1. 华中农业大学 资源与环境学院 武汉430070
  • 收稿日期:2010-05-20 修回日期:2010-07-26 出版日期:2011-03-20 网络出版日期:2011-02-18
  • 作者简介:殷 辉(1985-), 男, 博士研究生,
  • 基金资助:

    国家自然科学基金(20807019, 40771102); 教育部博士点基金新教师项目(20070504053)

Synthesis of Ramsdellite by Refluxing Processand Its Influencing Factors

YIN Hui, LIU Fan, FENG Xiong-Han, TAN Wen-Feng, QIU Guo-Hong, Chen Xiu-Hua, LIU Ming-Ming   

  1. Collegeof Resources and Environment, Huazhong Agricultural University, Wuhan 430070,China
  • Received:2010-05-20 Revised:2010-07-26 Published:2011-03-20 Online:2011-02-18
  • Supported by:

    National Natural Science Foundation of China (20807019, 40771102); Specialized Research Fund for the Doctoral Program of Higher Education of China (20070504053)

摘要: MnSO4与NaClO溶液常压回流反应制备纳米尺寸的拉锰矿, 采用X射线衍射、扫描电镜和比表面仪等表征产物的晶体结构、微观形貌和比表面积等物理化学性质, 探讨了反应温度、时间和盐酸添加量等对产物晶体结构、微观形貌和收率的影响. 结果表明, 60℃回流反应12 h产物为纳米颗粒, 并出现团聚现象, 温度升高, 颗粒粒径增大; 反应体系中添加盐酸, 颗粒粒径变小, 团聚体减少; 在100℃反应体系中添加盐酸, 首先形成粒状纳米拉锰矿, 在酸性环境中经溶解再沉淀反应转化为针状, 添加盐酸其针状形态的均一性增强, 且团聚结块趋势减弱. 低温加酸有利于形成高比表面积的拉锰矿, 可达66.32 m2/g. 产物收率随温度升高和盐酸添加量增大表现出先增加后减少的趋势, 最佳收率为97.5%.

关键词: 锰氧化物, 拉锰矿, 常压回流, 纳米材料

Abstract: Nanosized ramsdellite was synthesized by oxidizing 30mmol Manganese(II) sulfate dissolved in different amounts of hydrochloride (0,10, 20 and 40 mmol) with adding 60 mmol sodium hypochlorite solution atconstant velocity of 1 mL/min minute using a refluxing process at atmosphericpressure at different temperatures (60, 80 and 100℃). The products were characterized by XRD diffraction,scanning electron microscope and automated surface area analyzer. The effectsof reflux temperature, time and amount of hydrochloric acid on the crystalstructures, micromorphologies and yield of products were investigated. It was observed that nano-particles of conglobated ramsdellite was prepared at 60℃, and particle size increased with elevating the refluxing temperature. Both aggregate level and particle size of ramsdellite decrease after adding hydrochloric acid into the reaction solution. When the reflux reaction was carried out at 100℃ with adding different amount of hydrochloric acid,nano-size particles of ramsdellite were formed firstly, and then needle-like fibers of products came into being formed. The concentration of hydrochloricacid in the reaction system plays an important role in the morphologies of ramsdellitecrystal, which acts more remarkably at higher temperatures. It is favorable tothe formation of needle-like ramsdellite in nano size and aggregation with loose structures by addition of no less than 10 mmol hydrochloric acid into thereaction solution at 100℃. Ramsdellite particles with high specific surface area(maximum of 66.32 m2/g) are more prone to be formed byadding hydrochloric acid into the reaction solution at lower refluxing temperature. Product yield increases firstly and then decreases with the increase of the amount of hydrochloric acid and refluxing temperature, and the highest yield can be as high as 97.5%.

Key words: manganeseoxides, ramsdellite, refluxing at atmospheric pressure, nano-materials

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