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常压回流条件下红磷锰矿的合成及表征
发表时间：2013-04-15 浏览量：1620 下载量：511
| 全部作者： | 殷辉，刘凡，冯雄汉，谭文峰，邱国红 |
| 作者单位： | 华中农业大学资源与环境学院 |
| 摘 要： | 探讨了不同条件下红磷锰矿的合成，并使用粉末X射线衍射（X-ray diffraction, XRD）及Rietveld结构参数修正、傅里叶变换红外吸收光谱（Fourier transformed infrared, FTIR）和扫描电镜（scanning electron microscopy, SEM）表征产物晶体结构和微观形貌。Mn(H2PO4)2溶液在40～100℃常压回流反应生成非均一棱柱状红磷锰矿；添加等摩尔量磷酸，只有在100℃回流反应才能生成棒状红磷锰矿；进一步添加NaClO溶液可有效提高红磷锰矿收率，产物呈均一棒状。相同条件下，采用MnCl2和H3PO4混合溶液回流反应无红磷锰矿生成，但添加NaClO溶液可生成颗粒状红磷锰矿。Mn(H2PO4)2溶液在40℃回流12 h和24 h 时，产物为红磷锰矿和磷酸一氢锰混合物；随着回流时间延长至48 h，产物为纯相红磷锰矿。不同温度下制备的红磷锰矿具有相似的结构参数，但随着温度升高，产物密度逐渐增加。常压低温条件下合成的红磷锰矿密度低于热液成因矿物，为认识红磷锰矿在地表的形成转化提供了新途径。研究结果为红磷锰矿成因矿物学理论提供了新的内容，亦可为其在化学、材料科学等领域的应用提供新的制备方法。 |
| 关 键 词： | 无机合成化学；红磷锰矿；常压回流；形貌；Rietveld结构精修 |
| Title： | Synthesis and characterization of hureaulite at atmospheric pressure |
| Author： | YIN Hui, LIU Fan, FENG Xionghan, TAN Wenfeng, QIU Guohong |
| Organization： | College of Resources and Environment, Huazhong Agricultural University |
| Abstract： | Hureaulite was synthesized at different conditions, its crystal structure and micro-morphologies were characterized by powder X-ray diffraction (XRD), Rietveld structure refinement, Fourier transformed infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The results showed that prismatic hureaulite was synthesized by refluxing of Mn(H2PO4)2 solution at atmospheric pressure under different temperatures (40-100℃). Needle-like hureaulite was also fabricated at only 100℃ when H3PO4 was added. Hureaulite was prepared by further adding NaClO solution into the reaction system. However, hureaulite did not form when Mn(H2PO4)2 was substituted by MnCl2 and H3PO4, but it could form by further adding NaClO solution in the reaction solution. A mixture of hureaulite and MnHPO4·3H2O was produced by refluxing Mn(H2PO4)2 at 40℃ for 12 h and 24 h. After reaction of 48 h, single phase hureaulite was formed. Most of the crystal parameters were closely similar when products were fabricated at different temperatures. However, the calculated densities of hureaulite increased with the increase of reflux temperature. That was to say, the density of hureaulite in supergene soil was lower than that of those formed by hydrothermal reactions, which facilitated to know the formation mechanism of hureaulite in environment. The results presented here indicated that the genetic mineralogy of hureaulite should be re-recognized. The new preparation method also facilitated the exploitation and application of hureaulite in the field of chemistry and materials science. |
| Key words： | inorganic synthesis chemistry; hureaulite; refluxing at atmospheric pressure; micromorphology; Rietveld structure refinement |
| 发表期数： | 2013年4月第7期 |
| 引用格式： | 殷辉，刘凡，冯雄汉，等. 常压回流条件下红磷锰矿的合成及表征[J]. 中国科技论文在线精品论文，2013，6（7）：636-644. |
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