撞击流反应器制备纳米四氧化三铁的研究

Preparation of Fe_3O_4 nanoparticles by impinging stream reactor

在浸没式循环撞击流反应器中,以氨水为沉淀剂,用七水合硫酸亚铁和六水合三氯化铁为原料,采用共沉淀法制备了纳米四氧化三铁粒子。考察了搅拌转速、亚铁与三价铁物质的量比、反应温度和溶液pH对所得纳米四氧化三铁的分散性和粒径的影响。采用傅里叶红外光谱仪、透射电镜、X射线衍射仪等对制得的纳米粒子的结构和性能进行了表征。结果表明:用撞击流反应器制备纳米四氧化三铁粒子的最佳工艺条件:亚铁与三价铁物质的量比为1∶1,反应温度为40℃,搅拌转速为1 600 r/min,以氨水作沉淀剂,最佳pH控制在11.0左右。在上述条件下,可以制备出分散性好、纯度高、平均粒径为10 nm的四氧化三铁粒子。

In submerged circulative impinging stream reactor, Fe3O4 nanoparticles were prepared by co-precipitation method,with FeSO4 · 7H2O and FeC13 · 6H2O as raw materials, and ammonia as precipitator. Effects of stirring rate, a- mount-of-substance ratio of Fe^2＋ to Fe^3＋, reaction temperature, and pH on dispersion and particle size of Fe3O4 nanoparticles were investigated. Structure and performance of Fe3O4 nanoparticles were characterized by Fourier transform infrared spectroscopy （FFIR） ,transmission electron microscopy （TEM）, and X -ray diffraction { XRD}. Results showed that Fe3O4 nanoparticles with good dispersion, high purity, and mean particle size of 10 nm could be prepared under following optimum technological conditions ： amount-of-substance ratio of Fe2＋ to Fe3＋ was 1 ： 1, reaction temperature was 40 ℃, stirring rate was 1 600 r/min, pH was about 11.0 in the presence of ammonia as precipitant.