【摘要】 对微波加热磷酸二氢钾制备适用于光学玻璃的高纯偏磷酸钾(其中杂质Fe质量分数小于2×10^-6,Cu质量分数小于1×10^-7的工艺进行了研究。考察了合成磷酸二氢钾溶液的pH值、磷酸二氢钾溶液的结晶浓度、磷酸二氢钾微波加热时间以及微波功率等因素对制备高纯偏磷酸钾纯度的影响。研究表明:合成磷酸二氢钾溶液终点pH值约为3时,有利于杂质的去除;合适的结晶浓度既有利于杂质的去除,又利于提高产量;微波加热时间控制好,既可以使产品质量合格,又可以避免产品烧结,而加热时间还与盛装的产品量有关,尤其是产品均匀平铺有利于脱水迅速挥发;微波功率大小对产品含量影响不大。通过ICP检测与XRD表征发现,微波制备的样品结构与马弗炉500℃灼烧的样品结构未有明显的区别。更多还原

【Abstract】 As a phosphate glass raw material,KPO₃ with high purity was prepared by microwave heating of potassium dihydrogen phosphate. The effect of potassium dihydrogen phosphate solution pH,the crystallization concentration of potassium dihydrogen phosphate,the microwave heating time and microwave power on the purity of prepared potassium metaphosphate was investigated. The results showed that, when the end point pH value of potassium dihydrogen phosphate solution was about 3, the condition was helpful to remove impurities; The suitable crystallization concentration was not only beneficial to the removal of impurities,but also beneficial to increasing the yield of potassium dihydrogen phosphate; The appropriate time of microwave heating made the product quality be qualified and avoided the sintering of products; And the heating time was also related to the quantity of products, the uniformly dispersed products were conducive to dehydrate and rapidly volatilize; Microwave the power had little effect on the purity of potassium metaphosphate.The purity and structure of KPO₃ were characterized by X-ray diffraction（XRD）and ICP-OES.Results showed that there was no obvious difference between the structures of samples prepared by microwave heating and roasting in muffle furnace at temperature of 500 ℃.更多还原