核纯级^(7)LiF的制备  

Preparation of the nuclear-pure grade ^(7)LiF

作　　者：宗国强[1] 向绍基 崔振华[1] 王荣荣[1] 陆人杰[1] 张婷[1] 肖吉昌[1] ZONG Guo-qiang;XIANG Shao-Ji;CUI Zhen-Hua;WANG Rong-Rong;LU Ren-Jie;ZHANG Ting;XIAO Ji-Chang(Key Laboratory of Organofluorine Chemistry,Shanghai Institute of Organic Chemistry,University of Chinese Academy of Sciences,Chinese Academy of Sciences,Shanghai 200032,China)

机构地区：[1]中国科学院上海有机化学研究所有机氟化学重点实验室中国科学院大学,上海200032

出　　处：《化学研究与应用》2021年第11期2240-2246,共7页Chemical Research and Application

基　　金：中国科学院战略性先导科技专项子课题(XDA02010501,XDA02020105,XDA02020106)资助。

摘　　要：采用^(7)LiOH·H_(2)O和电子级氢氟酸进行氟化反应制备核纯级^(7)LiF,对各种制备工艺条件进行了研究。考察了氢氟酸的浓度和加入量、反应温度与时间、陈化时间、干燥温度等条件对^(7)LiF质量和收率的影响,找到了较好的^(7)LiF制备工艺条件。称取20.00g^(7)LiOH·H_(2)O加入质量浓度20%的氢氟酸,摩尔比n(HF)∶n(^(7)LiOH·H_(2)O)=1.1,滴加完成后升温至80℃进行氟化反应2 h,然后陈化10 h后过滤、洗涤,130℃条件下真空干燥20 h,高收率制备得到核纯级^(7)LiF。制备的^(7)LiF产率≥99.0%;纯度≥99.98%;总氧含量≤0.20%。^(7)LiF质量指标达到熔盐堆熔盐制备原材料要求,为第四代先进核能反应堆用熔盐(^(7)LiF-BeF_(2))的规模化制备及应用提供主要原材料和技术支持。Nuclear-pure grade^(7)LiF was prepared by fluorination reaction of^(7)LiOH·H_(2)O with electronic grade hydrofluoric acid,and various preparation process conditions were studied.The effects of the concentration and adding amounts of hydrofluoric acid,reaction temperature,reaction time,aging time and drying temperature on the quality and yield of^(7)LiF were screened and optimized preparation condition of^(7)LiF was established.Firstly,20.00g of^(7)LiOH·H_(2)O was added into the hydrofluoric acid with a mass concentration of 20%and a molar ratio of 1.1.Then,the mixture was stirred at 80℃for 2 h,and followed by being aged for 10 h.After that,it was filtered,washed,and then dried in vacuum at 130℃for 20 h.Finally,the nuclear-pure grade^(7)LiF was obtained with a high yield of≥99.0%,a Purity≥99.98%and a total oxygen content of≤0.20%.As the quality index of^(7)LiF meets the requirements of molten salt preparation raw materials for molten salt reactors,our research provides key raw material and technical support for the large-scale preparation and application of fluoride molten salt(^(7)LiF-BeF_(2))for the fourth-generation advanced nuclear power reactor.

关 键 词：核纯级 ^(7)LiF 制备 熔盐堆(MSR) 

分 类 号：TL281[核科学技术—核燃料循环与材料]