高纯异丙醇铝的制备及其在发光材料中的应用

【作者】 李淑珍；

【导师】 宁桂玲；

【作者基本信息】 大连理工大学 ， 化学工艺， 2004， 硕士

【摘要】 本文针对异丙醇铝-异丙醇有机体系中痕量铁杂质的脱除，做了以下几方面的工作： 1、异丙醇铝中痕量铁杂质测量方法的研究 邻菲罗啉分光光度法是测定化学品中微量铁的通用方法，为了考察该法是否适用于异丙醇铝中痕量铁杂质的测量，做了几方面的实验工作： (1)考察了异丙醇铝的盐酸溶液是否对邻菲罗啉亚铁配合物的吸收曲线、配合物的稳定性产生影响； (2)确定了显色溶液中存在大量铝离子和氯离子的条件下，邻菲罗啉亚铁配合物适宜的显色剂用量和显色PH范围； (3)线性回归得到了邻菲罗啉分光光度法测定异丙醇铝中痕量铁杂质的工作曲线。 2、“螯合-蒸馏法”脱除异丙醇铝-异丙醇有机体系中痕量铁杂质的研究 提出“螯合-蒸馏法”纯化异丙醇铝的理论，为了验证该法在异丙醇铝-异丙醇体系中脱除微量铁杂质的可行性，做了以下工作： (1)实验选择了对异丙醇铝-异丙醇体系有效的螯合试剂，包括：氧配位螯合剂酚酞和氧、氮配位螯合剂PAN及XO等。考察添加不同量螯合剂情况下的除铁效果，确定螯合剂的最优添加比。 (2)对螯合剂的除铁机理进行推理，得到了螯合剂-铁螯合物稳定存在的原因；并采用红外光谱和热重分析添加螯合剂会不会影响到产物的质量。 (3)综合比较各种螯合剂的除铁效果和生产成本，确定酚酞是比PAN更适合的除铁剂。实验证明螯合-蒸馏提纯技术是实际可行的。 (4)考察添加相同量酚酞对原始杂质含量不同铝的除铁效果，确定了酚酞是异丙醇铝-异丙醇体系的有效试剂。 3、考察了异丙醇铝中铁杂质含量对发光材料性能的影响；并对铝酸锶发光材料的前驱物中加入氧化铁时，材料发光性能的变化以及材料中铁的作用机理进行简单推理。更多还原

【Abstract】 This paper is focused on the removal of iron impurity in aluminium isopropoxide. Three aspects of this .study have been carefully carried out as following:1.Measuring methods of trace iron impurity in aluminium isopropoxideIn order to mensure Fe impurity-content in the aluminium isopropoxide, phenanthroline spectrophotometer method is considered roundly:(1)Influence on the absorption curve and the stability of Phen-Fe(II) chelate complex when aluminium isopropoxide exists in solution.(2)Choosing appropriate PH value and reagent addition of Phen-Fe( II) chelate complex in the presence of aluminium isopropoxide.(3)Getting linear equation as the working curve for the trace iron impurity measurement in aluminium isopropoxide.2. Removal of iron impurity in aluminium isopropoxide by chelate-distillation methodIn order to verify the chelate-distillation theory used in aluminium isopropoxide-isopropanol is feasible in practice, the following work has been done:(1)Choosing the effectual chelate reagent used in aluminium isopropoxide-isopropanol, including Phenolphthalein, Xylenol Orange and PAN etc. Investigating the relation between iron-removing effect and addition dosage, then getting optimal mass ratio.(2) Discussion the stability of Fe-chelate complex and removal of iron mechanism. Results of infrared spectroscopy and TG/DTG demonstrate that addition, such as PAN. has not impact on aluminium isopropoxide.(3)Making a review of all the chelate reagents; phenolphthalein is the better addition to remove iron in aluminum isopropoxide than PAN.(4) Investigation on the effect of removing iron impurity by using equal Phenolphthalein in different aluminum. Results demonstrate that Phenolphthalein is suitable for the removing iron impurity in aluminum isopropoxide- isopropanol.3. The dependence between luminescence performance and Fe impurity’s content in aluminum isopropoxide. Discussing the impact of Fe2O3 existed in SrAl2O4:Eu2+,Dy3+ on luminescence.更多还原