高纯纳米氧化铁的制备  

Preparation of high-purity nano iron oxide

作　　者：吴文军 韩召 张福元 刘鹏飞 李杰 WU Wenjun;HAN Zhao;ZHANG Fuyuan;LIU Pengfei;LI Jie(School of Metallurgical Engineering,Anhui University of Technology,Ma'anshan 243032,China)

机构地区：[1]安徽工业大学冶金工程学院,安徽马鞍山243032

出　　处：《中国粉体技术》2024年第1期56-65,共10页China Powder Science and Technology

基　　金：国家自然科学基金项目,编号:52074003。

摘　　要：【目的】改进纳米氧化铁的制备工艺流程,制备高纯纳米氧化铁。【方法】首先,采用重结晶法去除硫酸亚铁中Ca^(2+)、 Mg^(2+)、 Mn^(2+)等杂质离子,采用氟化铵沉淀进一步去除硫酸亚铁中的Ca^(2+)、 Mg^(2+)杂质离子,然后使用过氧化氢氧化法、氨水沉淀法对硫酸亚铁进行沉淀制得羟基氧化铁,接着采用调浆法和超声法洗涤羟基氧化铁制得前驱体,最后焙烧前驱体制得高纯纳米氧化铁;使用仪器和设备分析高纯纳米氧化铁的颗粒形貌、粒径分布和杂质离子的质量浓度。【结果】改进后的制备高纯纳米氧化铁的工艺流程为:将温度为60℃时的饱和硫酸亚铁溶液进行降温,在温度至10℃时实现2次重结晶,将重结晶后的硫酸亚铁配置为pH为6的溶液;在水浴温度为30℃时,氟化铵过量系数设为5以使Ca^(2+)、 Mg^(2+)沉淀,制得纯净硫酸亚铁溶液;利用过氧化氢氧化、氨水沉淀硫酸亚铁溶液制得羟基氧化铁;重复利用调浆洗涤、超声洗涤羟基氧化铁去除铵根离子和硫酸根离子;将沉淀物在温度为600℃时焙烧1 h,制得高纯纳米氧化铁。【结论】由改进的制备方法制得的高纯纳米氧化铁球形颗粒形貌均匀,中位粒径为300 nm,高纯纳米氧化铁中α-Fe_(2)O_(3)的质量分数大于99.95%。Objective Various application areas put forward demanding requirements for high-purity iron oxide nanoparticles with high purity,small particle size and narrow particle size distribution.Currently,studies on prepared iron oxide nanoparticles pay less attention to the purity,mainly because of the failure to purify the iron source used in the experiments.It is difficult to completely remove the remaining ammonium ion and sulfate ion in the iron oxide by hydrothermal method of preparation,so there is a need to find an operationally simple and effective method for the preparation of high-purity iron oxide nanoparticles.To prepare high-purity iron oxide nanoparticles,the preparation method of iron oxide nanoparticles needs to be further improve,followed by detailed phase analysis.Methods Firstly,the recrystallization method was used to purify ferrous sulfate at one time.The saturated ferrous sulfate solution was put into a low-temperature circulating thermostat for crystallization,and the ferrous sulfate crystals were prepared after removing impurities.The crystallization processes above were repeated until the purity reached the requirements.Secondly,the second purification of ferrous sulfate was carried out by ammonium fluoride precipitation method.The ferrous sulfate crystals after the initial purification were first configured as a solution,and then ammonium fluoride and ammonia were added to the ferrous sulfate solution.After precipitation and removing the impurities,a pure ferrous sulfate solution was obtained.Finally,hydrogen peroxide was added to the pure ferrous sulfate solution for oxidation.The hydroxyl iron oxide was precipitated by adding ammonia.After further removing impurities by the slurry mixing method and ultrasonic washing method,the iron oxide precursor was prepared and calcined to obtain high-purity nano iron oxide.Subsequently,atomic absorption spectroscopy and inductively coupled plasma atomic emission spectrometry were used to analyze the ionic mass concentration in ferrous sulfate solution an

关 键 词：高纯纳米氧化铁 重结晶法 氟化铵沉淀 调浆-超声洗涤法 氨水沉淀法 物相分析 

分 类 号：TQ138.1[化学工程—无机化工] TB4[一般工业技术]