钨酸盐和钼酸盐的阳离子膜电解制备工艺研究

发布时间：2018-02-24 08:28

本文关键词： 阳离子膜电解法钨酸盐钼酸盐　出处：《上海应用技术学院》2015年硕士论文　论文类型：学位论文

【摘要】：钨/钼酸盐是一类具有广泛应用的无机功能性材料,可应用于微波、光学、催化剂、闪烁材料、传感器、磁性以及电化学等方面。钨/钼酸盐的合成方法有很多,然而这些方法存在许多缺点,比如,反应时间长、或者有机聚合物的添加、或者反应条件苛刻、或者操作过程繁杂。因此本文在研究了铜在钨酸钠水溶液中的电化学行为的基础上,首次利用阳离子膜电解法制备钨酸盐和钼酸盐功能性材料及钨/钼-过渡金属合金粉末,通过与以往的合成方法相比较,本方法不仅仅操作简单、反应条件温和、原料廉价并且无副反应、效率高等优点。论文主要内容概述如下：1.铜在钨酸钠水溶液中的电化学行为首次采用三电极体系在双极室隔膜电解槽中使用循环伏安法研究Cu在Na2WO4水溶液中的电化学行为。测试结果表明,Cu的氧化过程形成了内层的Cu20和CuO/Cu(OH)2以及外层的难溶于水的CuWO4水合物的混合薄层,稳定生成CuWO4水合物的电位范围为0.3V～1.0V。2.阳离子膜电解法制备金属钨酸盐以第二章的研究结果为理论基础,通过阳离子膜电解法制备钨酸铜、钨酸锌、钨酸镍、钨酸铝、钨酸银粉末以及钨-铜、钨-铁、钨-镍、钨-银合金粉末。采用TG、IR、EDX、 XRD、TEM及HRTEM等表征手段对钨酸铜进行了分析,证明通过阳离子膜电解法制备的钨酸铜是纯净的、无杂相的、结晶度高的纳米级颗粒。然后对其余的钨酸盐粉末以及钨-过渡金属合金粉末进行了EDX、XRD表征,结果表明制备的金属钨酸盐是纯净的,无杂相的并且结晶度很高；制备的钨-过渡金属合金粉末是纯净的、无杂相的,而且是分布均匀的。3.阳离子膜电解法制备金属钼酸盐通过阳离子膜电解法制备钼酸铜、钼酸锌、钼酸铁、钼酸镍、钼酸铝、钼酸银以及钼-铜、钼-铁、钼-镍、钼-银合金粉末。并且采用TG、IREDX、XRD、TEM及HRTEM等表征手段对钼酸铜进行了分析,证明了通过阳离子膜电解法制备的钼酸铜是纯净的、无杂相的、结晶度高的纳米级微粒。然后对其余的钼酸盐粉末以及钼-过渡金属合金粉末进行了EDX、XRD等表征,结果表明制备的金属钼酸盐是纯净的,无杂相的并且结晶度很高；制备的钨-过渡金属合金粉末是纯净的、无杂相的,而且是分布均匀的。
[Abstract]:Tungsten / molybdate is a kind of inorganic functional materials with wide application, which can be used in microwave, optics, catalyst, scintillation material, sensor, magnetism and electrochemistry. However, these methods have many disadvantages, such as the long reaction time, the addition of organic polymers, or the harsh reaction conditions. Therefore, on the basis of studying the electrochemical behavior of copper in sodium tungstate solution, we prepared tungstate and molybdate functional materials and tungsten / molybdenum transition metal alloy powder by cationic membrane electrolysis for the first time. Compared with the previous synthetic methods, this method is not only simple to operate, mild reaction conditions, cheap raw materials and no side reaction, The main contents of this paper are summarized as follows: 1. Electrochemical behavior of copper in sodium tungstate solution. The electrochemical behavior of copper in aqueous solution of sodium tungstate was studied by cyclic voltammetry in a bipolar chamber diaphragm electrolyzer using a three-electrode system for the first time. Chemical behavior. The results showed that the oxidation process of Cu formed a mixed layer of Cu20 and CuO/Cu(OH)2 in the inner layer and a mixed layer of the insoluble CuWO4 hydrate in the outer layer. The potential range of stable formation of CuWO4 hydrate is 0.3 V ~ (-1) V ~ (-1) V. 2.The preparation of metallic tungstate by cationic membrane electrolysis is based on the theoretical results in Chapter 2. Copper tungstate, zinc tungstate, nickel tungstate, aluminum tungstate are prepared by cationic membrane electrolysis. Silver tungstate powder and tungsten-copper, tungsten-iron, tungsten-nickel, tungsten-silver alloy powder. The copper tungstate prepared by cationic membrane electrolysis is pure and non-impurity phase. The other tungstate powder and tungsten transition metal alloy powder were characterized by EDX XRD. The results showed that the prepared tungstate was pure, impurity free and high crystallinity. The prepared tungsten transition metal alloy powder is pure, impurity free and evenly distributed. The preparation of metal molybdate by cationic membrane electrolysis method is used to prepare copper molybdate, zinc molybdate, ferric molybdate, nickel molybdate, aluminum molybdate, copper molybdate, zinc molybdate, ferric molybdate, nickel molybdate, aluminum molybdate by cationic membrane electrolysis, Silver molybdate and molybdenum-copper, molybdenum-iron, molybdenum-nickel, molybdenum-silver alloy powder. The copper molybdate prepared by cationic membrane electrolysis is pure and non-impurity phase. The other molybdate powder and the molybdenum transition metal alloy powder were characterized by EDX XRD. The results showed that the molybdate prepared was pure, impurity free and high crystallinity. The prepared tungsten-transition metal alloy powder is pure, impurity-free and uniformly distributed.
【学位授予单位】：上海应用技术学院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ136.13;TQ136.12

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