冶金法制备高纯硅过程中石油焦粉的净化研究

李峰, 邢鹏飞, 涂赣峰, 郭菁

东北大学 材料与冶金学院,沈阳 110004



摘要:

为给高纯硅的制备提供一种高纯原料,详细研究了石油焦粉的酸浸除杂、超声酸浸除杂、真空高温除杂,考察了石油焦粉粒度、盐酸浓度、酸浸时间、酸浸温度、酸浸液固比和搅拌对除杂效果的影响.得到的最佳工艺条件为:石焦粉颗粒控制在150 μm以下,盐酸质量分数5%,反应时间6 h,水浴温度70 ℃,浸出液固比10∶1,搅拌速度40 r/min.在此工艺条件下,石油焦粉中金属元素杂质的去除率可高达94.69%,非金属元素杂质的去除率达39.95%.实验同时探讨了超声场作用下酸洗时间对杂质去除效果的影响,以及在真空高温焙烧条件下杂质的去除效果,最终金属元素杂质和非金属元素杂质的去除率分别达到了99.55%和99.23%.

关键词:  石油焦粉  除杂  高纯硅  酸浸  超声场  真空

DOI：10.11951/j.issn.1005-0299.20120607

分类号:

基金项目:国家自然科学基金资助项目(51074043);国家科技支撑计划资助项目(2011BAE03B01).



Remove of impurity of petrol coke during preparing high purity silicon by metallurgical method

LI Feng, XING Peng-fei, TU Gan-feng, GUO Jing

College of Materials and Metallurgy,Northeastern University,Shenyang 110004,China

Abstract:

To provide a high purity raw materials for preparing high purity silicon,the removal of impurity of petrol coke is studied in this paper by acid leaching,ultrasonic field purification and vacuum heating purification.The optimal parameters of acid leaching are as follows:the size of petroleum coke particles below 150 μm;hydrochloric acid of 5wt%,reaction time of 6h,temperature of 70 ℃,the ratio of leaching liquid to solid of 10∶1 and stirring speed of 40 r/min,under which up to 94.69wt% metallic in petrol coke powder and 39.95% non-metallic can be removed.At the same time,the effects of ultrasonic field and high-temperature roasting in vacuum on the results of purification by acid leaching are investigated.As a result,the elimination of metallic and non-metallic impurities reached 99.55% and 99.23% respectively.

Key words:  petrol coke  impurity remove  high purity silicon  acid leaching  ultrasonic field  vacuum