四氟化锗制备二氧化锗的方法研究  

Study on the Conversion of Germanium Dioxide from Germanium Tetrafluoride

作　　者：王晶[1] 周红艳[1] 高林华 陈俭月 王珂 Wang Jing;Zhou Hongyan;Gao Linhua;Chen Jianyue;Wang Ke(National Key Laboratory of Particle Transport and Enrichment Technology,Nuclear industry physical and chemical engineering Research Institute,Tianjin 300180,China)

机构地区：[1]核工业理化工程研究院粒子输运与富集技术全国重点实验室,天津300180

出　　处：《云南化工》2024年第8期78-81,共4页Yunnan Chemical Technology

摘　　要：高纯度二氧化锗-76是制备锗探测器的原料,由富集四氟化锗-76制备。介绍了一种由四氟化锗为原料两步转化为二氧化锗的方法,首先通过四氟化锗水解,水解液酸化得到四氯化锗;再通过蒸馏收集四氯化锗,四氯化锗水解得到二氧化锗。研究并确定了工艺过程的重要实验参数,即四氯化锗水解温度为20~25℃,氯化蒸馏时溶液中盐酸浓度为9 mol/L,助剂氯化钠与原料四氟化锗的物质的量比为2∶1。通过对产品进行定性及定量分析,确定该方法制备的产品为六方型二氧化锗,纯度≥99.98%。该方法具有环保、安全、条件温和、易于控制等特点,产品纯度高,产率可达到80%以上。该工艺可应用于制备高纯锗探测器的重要原料-高丰度的二氧化锗-76,对于航空航天以及核物理探测领域的研究具有重要意义。High purity germanium dioxide-76 is the raw material for preparing germanium nuclear radiation detector,which is prepared by enrichment of germanium tetrafluoride-76.In this paper,a two-step conversion method of germanium dioxide from germanium tetrafluoride was introduced.Firstly,germanium tetrafluoride was hydrolyzed and acidified to obtain germanium tetrachloride.Then germanium tetrachloride was collected by distillation,and germanium tetrachloride was hydrolyzed to obtain germanium dioxide.The important experimental parameters of the process were studied and established,that is,the hydrolysis temperature of germanium tetrachloride was 20~25 ℃,the concentration of hydrochloric acid in the chlorination distillation solution was 9 mol/L,and the molar ratio of auxiliary sodium chloride to raw germanium tetrafluoride was 2∶1.By qualitative and content analysis,the product prepared by this method is hexagonal germanium dioxide with purity ≥99.98%.The method has the characteristics of environmental protection,safety,mild conditions and easy control.The product purity is high and the yield can reach more than 80%.The process can be used to prepare high abundance germanium dioxide-76,which is an important raw material of high purity germanium detector,and is of great significance for the research of aerospace and nuclear physics detection.

关 键 词：四氟化锗 二氧化锗 转化 

分 类 号：TQ134[化学工程—无机化工] TL81[核科学技术—核技术及应用]