空气氧化法合成微纳米四氧化三铁的研究

发布时间：2018-04-09 19:11

  本文选题：含铁酸洗废液　切入点：打印机墨粉　出处：《中国海洋大学》2015年硕士论文

【摘要】：钢铁酸洗液的资源化处理是企业的一大难题。本文针对含铁酸洗废液的特点,采用空气氧化法研究了制备打印机墨粉用磁粉(Fe_3O_4)的工艺条件。通过综合处理使之变废为宝。以FeCl_2、FeSO_4和含铁酸洗液三种不同原料制备出四氧化三铁磁性颗粒,采用扫描电镜、透射电子显微镜和粒度分析仪、X射线衍射表征了其形貌和结构。发现,以含铁酸洗液为原料制备的产品矫顽力低；以FeSO_4为原料制备的Fe_3O_4的形貌和分散性好。探讨了影响产品磁性能的因素。研究了原料加入顺序、反应温度、反应pH、碱的种类、反应终点判断、表面活性剂、N_2、掺杂等因素对产品磁性能的影响；氧化剂种类对产品形貌的影响。研究结果表明：反应pH=7.0、反应温度为85-90℃、以将7.5 mol/L的NaOH溶液加入到Fe~(2+)溶液中的顺序添加反应物为最佳反应条件,在此条件下,当Fe~(3+)/Fe~(2+)=1.99时,结束氧化反应能够得到纯度高、形貌接近球形、磁性数据好的Fe_3O_4磁粉微粒：采用N_2保护,有利于提高产品品质；氨水为沉淀剂制备出的Fe_3O_4力高、饱磁低,不如NaOH溶液制备的Fe_3O_4的磁性好；分散剂添加过多会导致颗粒变小；添加Zn可降低产品的矫顽力,添加mol/mol为4%Mn时,可使产品矫顽力降低且抗老化性提高；添加P会使产品品质下降；采用液体氧化剂氧化时产品的粒径变小。根据实验结果,进行了吨级实验放大,修改完善了部分参数,放大实验证明本文提出的以钢铁酸洗废液为原料制备打印机墨粉用Fe_3O_4磁粉的工艺可行,不仅使含铁酸洗液得到了无害化处理,而且得到的产品完全满足打印机墨粉的各项指标要求。
[Abstract]:The resource treatment of iron and steel acid lotion is a difficult problem for enterprises.According to the characteristics of ferric acid pickling waste liquid, the technological conditions of preparing Fe3O _ 4 for printer toner powder were studied by air oxidation method.To turn waste into treasure by comprehensive treatment.Fe _ 2O _ 3 magnetic particles were prepared from FeCl _ 2 + FeSOD _ 4 and ferric acid washing solution. The morphology and structure of the particles were characterized by scanning electron microscope, transmission electron microscope and particle size analyzer by X-ray diffraction.It was found that the product prepared from ferric acid lotion had low coercivity, and Fe_3O_4 prepared with FeSO_4 as raw material had good morphology and dispersibility.The factors influencing the magnetic properties of the products are discussed.The effects of addition order of raw materials, reaction temperature, pH of reaction, type of alkali, determination of reaction end point, surfactant N _ 2 and doping on the magnetic properties of the product and the influence of oxidant type on the morphology of the product were studied.The results showed that the optimum reaction conditions were as follows: reaction pH = 7.0, reaction temperature 85-90 鈩，

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