《磷酸锌锂的固相合成》-毕业论文.doc

磷酸锌锂的固相合成 摘 要 本文通过在不同温度下分别对NH4ZnPO4 +Li2CO3→LiZnPO4+CO2↑+H2O↑+NH3↑和NH4ZnPO4+LiOH?H2O→LiZnPO4+H2O↑+NH3↑两种可能可行的LiZnPO4合成路线进行了试验性的固相合成研究，并用XRD分别对所得的产物进行表征。XRD结果显示两条合成路线同时在700℃保温时2小时以后获得比较纯的LiZnPO4晶体。接着通过均匀设计法设计实验方案，以NH4ZnPO4和Li2CO3为原料，在不同的因素水平下进行实验。计算收率；用分分光光度法测定产物中的锌含量。然后经逐步回归分析，建立锌含量、收率与各因素的两个数学模型，对这些数据进行优化处理得到合成工艺的优化条件。通过计算机辅助设计使得锌含量与收率同时达到最优的双重目标。经XRD表征为纳米级晶体,分子式为LiZnPO4,平均粒径为62.6 nm。对不同温度下的产物分别用红外光谱进行分析，进一步确认产物的结构。最后通过对NH4ZnPO4和Li2CO3的混合物体系的TG-DTA曲线进行分析，探讨合成过程中NH4ZnPO4和Li2CO3的分解动力学过程。实验证明本文固相合成磷酸锌锂的方法不仅是可行的而且具有设备简单、绿色环保等特点，很符合我们所倡导的绿色化学思想。 关键词：磷酸锌锂，固相合成，均匀设计 Synthesis of Lithium Zinc Phosphate by solid reaction Abstract In this paper, the direct synthesis method of lithium zinc phosphate was tried to study under the two possible synthesis routes as route NH4ZnPO4+Li2CO3 → LiZnPO4 + CO2↑ +H2O↑+NH3↑ and route NH4ZnPO4+LiOH?H2O→LiZnPO4 +H2O↑++NH3↑ by heating the mixture of NH4ZnPO4,Li2CO3 and the mixture of NH4ZnPO4, LiOH?H2O at different temperatures and characterized the products by X-ray powder diffraction. It was showed that lithium zinc phosphate can be synthesized by heating the two mixtures mentioned for two hours by X-ray power diffraction patterns. The experimental project was formed by uniform design, and the experiments were done in vary factors as well as vary levels. The zinc content was determined by spectrophotometer, Two progress models respectively describing the relationships between the zinc content and vary factors ,as well as between the efficiency of products. The optimum synthesis process conditions were got through optimization with the two models. Controled reaction was achieve with the assistant of the PC computer, so the double optimum aims for the content of zinc and the efficiency of the products were synchronously got. The characterization results of XRD shown the crystals of the product are nanocrystals, and the molecular form of the crystal is LiZnPO4, the average size of the crystals is about 62.6 nm. The IR spectrums of the p