硝酸氧化法和区域熔融法联合净化工业黄磷的研究  

Study on purification of yellow phosphorus by nitric acid oxidation combined with zone melting

作　　者：蒋祥飞[1] 李军[1] 刘雪峰[1] 罗建洪[1] 金央[1] 姚卫东[1] 

机构地区：[1]四川大学化学工程学院,四川成都610065

出　　处：《无机盐工业》2014年第3期32-35,共4页Inorganic Chemicals Industry

基　　金：国家科技支撑计划项目(项目编号2007BAE58B00)

摘　　要：研究了硝酸氧化法和区域熔融法联合净化工业黄磷生产高纯黄磷的方法。考察了硝酸氧化法反应时间和硝酸质量分数对脱砷率和磷收率的影响,结果表明,当硝酸质量分数为13%、液固体积比7∶1、氧化增强剂用量占黄磷质量的5%、反应温度为75℃、反应时间为4 h时,可使黄磷中砷质量分数降低到1×10-6,磷收率>80%。采用区域熔融法对氧化后的黄磷做二次处理,进一步脱除黄磷中的金属杂质,其中钙、铁、镁的脱除率分别达到97.67%、98.15%、85.29%。硝酸氧化法和区域熔融法联用能有效净化工业黄磷,生产高纯黄磷。A method to purify industrial yellow phosphorus by nitric acid oxidation combined with zone mehing was devel- oped in this work.The effects of reaction time and mass fraction of nitric acid on arsenic removal rate and phosphorus recovery rate were investigated.Resuhs showed that the mass fraction of arsenic in yellow phosphorus could be decreased to less than 1×10-6 and the phosphorus recovery rate was up to 80.0% when the experiments were carried out under the following condi- tions： mass fraction of nitric acid was 13% ,volume ratio of liquid to solid was 7：1 ,amount of the new oxidation enhancer ac- counted for 5% （mass fraction）of yellow phosphorus, reaction temperature was 75 ℃ and reaction time was 4 h.In order to fur- ther remove metal impurities, zone melting method was used to refine yellow phosphorus after the processing of oxidation. The removal rates of Ca,Fe,and Mg reached 97.67% ,98.15% ,and 85.29% ,respectively.The method of nitric acid oxidation combined with zone melting could purify industrial yellow phosphorus effectively and improve the production of high purity yellow phosphorus.

关 键 词：黄磷 硝酸氧化 脱砷 区域熔融 金属杂质 

分 类 号：TQ126.3[化学工程—无机化工]