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利用钢厂除尘灰合成纳米级磁性氧化铁黑颜料的研究

Synthesis of Nanometer-sized Magnetic Black Iron Oxide Pigment by using Dust of Steel Industry

【作者】 沈腊珍

【导师】 谭俊茹;

【作者基本信息】 天津大学 , 物理化学, 2004, 硕士

【摘要】 论文综述了国内外除尘灰的综合利用现状,氧化铁系颜料的市场发展状况,重点介绍了铁黑颜料的应用和发展前景。本课题以钢厂废弃物除尘灰为原料,通过中和→沉淀→氧化→加成的方法制备出纳米级磁性氧化铁黑颜料,研究了制备的最佳工艺参数,如原料液中总铁的浓度、原料液中Fe3+离子与Fe2+离子摩尔比、沉淀剂的浓度、沉淀剂的种类、加入沉淀剂的方式及速度、反应温度、反应时间等。通过对颜料粒子TEM照片的分析研究,初步探讨了影响颜料粒子形状和粒度大小及分布的因素,以及影响颜料比表面积、吸油量、遮盖力等性能的因素。通过对氧化反应过程中二价铁离子浓度的监测,确定了不同温度下Fe(OH)2氧化反应的反应动力学及反应活化能。从理论上分析铁黑颜料晶体的成核机理及成核热力学。用热重-差热方法同时分析了铁黑的脱水过程及氧化过程。从结构入手解释了γ-FeOOH及Fe3O4的形成过程,探讨了铁黑前驱体的制备机理;分析了Fe3O4的磁性机理。铁黑的主要性能通过色彩分析仪、TEM、X射线衍射、BET、震动样品磁强计等方法进行表征,产品质量和主要性能指标超过市售铁黑颜料产品,达到了国家标准。本课题研究的意义在于打破了传统加晶种制备铁黑的方法,以除尘灰酸浸液制得的硫酸铁和硫酸亚铁的混合溶液为原料,经中和沉淀法合成出铁黑颜料,制备方法简单有效,工艺可行。

【Abstract】 This article summarized recently comprehensive utilization of dust and development state and utilization of iron oxide pigments in market, and introduced mainly the prospect of application and development at home and abroad. Preparation method took neutralize precipitation method,This study prepared nanometer-sized magnetic black iron oxide pigment through processes of neutralizing→precipitating→oxidation→addition with the mix liquor of Fe2(SO)4 and FeSO4 obtained by sulfuric acid leaching dust as starting material. The best technological conditions were determined, such as the total iron density in starting material, molar ratio of Fe3+ ions and Fe2+ ions in starting material, density of precipitant, style and speed of adding precipitant, reaction temperature, reaction time and etc. This article discussed preliminarily the factors to influence the particle shape, dimensions and distribution of particle size by analyzing and studying TEM pictures of pigment particles, and discussed the factors to influence characteristics such as specific surface area, oil absorption, covering power and so on. By the measurement of the Fe2+ ions concentration during the reaction process, components of Fe(OH)2 in precipitance regularity was obtained, furthermore, reaction kinetics and activity energy of Fe(OH)2 oxidation reaction at different temperature were determined. This article analysis dehydration process and oxidation process by TG-DTA analysis, and explain the formation process of γ-FeOOH and Fe3O4 from their structures, discussed preparation mechanism and magnetic mechanism of Fe3O4. were determined by measuring, and its saturated magnetization is better than that in given data report. The main characteristics of pigments were analyzed by chromometer, XRD, TEM, BET, magnetometer and so on, quantity of pigment and main characteristics are better than that of black iron oxide pigment on market and reached criterion and standard.The significance of this study is in that we create a new method with Fe2(SO)4 and FeSO4 mixture solution as starting material and break traditional method by adding crystal seeds and used the neutralization precipitation method to get black iron oxide pigment, this method is simple and effective and the process is feasible.

  • 【网络出版投稿人】 天津大学
  • 【网络出版年期】2004年 04期
  • 【分类号】TQ622
  • 【被引频次】1
  • 【下载频次】358
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