真空蒸馏加剂除铅制备高纯铋

journal6 ›› 2009, Vol. 30 ›› Issue (3): 95-101.

真空蒸馏加剂除铅制备高纯铋

（1.中南大学化学化工学院，湖南长沙 410083；2.吉首大学化学化工学院，湖南吉首 416000；3.昆明理工大学材料与冶金工程学院，云南昆明 650093）

出版日期:2009-05-25 发布日期:2012-04-23
作者简介:熊利芝（1974-），女，讲师，中南大学化学化工学院博士研究生,主要从事真空冶金、高纯材料与能源材料研究.
基金资助:
973国家重点基础研究发展计划（2007CB613601）

Preparation of High-Purity Bismuth by Reagent Deleadization with Vacuum Distillation

(1.School of Chemistry and Chemical Engineering,Central South University,Changsha 410083,China；2.College of Chemistry and Chemical Engineering,Jishou University,Jishou,416000,Hunan China;3.College of Materials and Metallurgical Engineering,Kunming University of Science and Technology,Kunming,650093,China)

Online:2009-05-25 Published:2012-04-23

摘要/Abstract

摘要：从理论上分析了用真空蒸馏分离精铋中各杂质和通过加硫、加氯除铅的可行性.在真空炉内进行了精铋加剂除铅的实验研究，考察了加剂量、蒸馏温度、残压和蒸馏时间等4个因素对除铅的影响，得到了最佳工艺条件：加硫除铅，蒸馏温度控制在1 073 K，每克精铋加硫0.02 g，可将含铅3.0×10-⁵的精铋中的铅降到2.1×10^-7，脱铅率约为99.3%；氯化除铅，蒸馏温度控制在1 023 K，每克精铋加氯化铜0.06 g，可将含铅3.0×10^-5的精铋中的铅的含量降到2.4×10^-7，脱铅率约为99.2%.精铋中的其他杂质也可在一定条件下通过真空蒸馏有效除去,均达到“99.999%”高纯铋的要求.

关键词： 真空蒸馏, 加剂, 除铅, 金属铋, 高纯

Abstract: The feasibility of separation of impurities in refined bismuth and reagent deleadization with vacuum distillation is studied theoretically.Experimental studies on reagent deleadization were carried out in vacuum and the influence of various factors,including amount of reagent,distillation temperature,vacuum degree and distillation time on the deleadization are inspected;then an optimal technical condition is achieved to be the following: as to sulphur deleadization,addition of sulphur is about 0.02 g/g of refined bismuth,at distillation temperature of 1 073 K,lead content in refined bismuth decreases from 3.0×10^-5 to 2.1×10^-7,and the deleadization rate is about 99.3%;as to chloridized deleadization,addition of copper chloride is about 0.06 g/g of refined bismuth,at distillation temperature of 1 023 K,lead content in refined bismuth decreases from 3.0×10^-5 to 2.4×10^-7,and the deleadization rate is about 99.2%.Other impurities in refined bismuth can be also removed effectively under certain conditions,the content of bismuth has reached the level of “99.999%”with vacuum distillation.

Key words: vacuum distillation；reagent, deleadization, metal bismuth；High-purity

熊利芝, 戴永年, 尹周澜, 陈启元. 真空蒸馏加剂除铅制备高纯铋[J]. journal6, 2009, 30(3): 95-101.

XIONG Li-Zhi, DAI Yong-Nian, YIN Zhou-Lan, CHEN Qi-Yuan. Preparation of High-Purity Bismuth by Reagent Deleadization with Vacuum Distillation[J]. journal6, 2009, 30(3): 95-101.

参考文献

[1] 汪立果.铋冶金 [M].北京:冶金工业出版社,1983：193-195.

[2] 郭青蔚.高纯金属研究现状及展望 [J].世界有色金属,1996,4:17-18.

[3] 张小琴，姜银举，代清.真空蒸馏法制备高纯金属钆 [J].包钢科技，2007,33(3)：17-20.

[4] 徐静，张炜,肖锋，等.中间合金-真空蒸馏法制备高纯金属镝工艺研究民 [J].稀土，2003,24(4):36-38.

[5] 苏毅,李国斌,罗康碧，等.高纯金属镓制备技术研究进展 [J].稀有金属,2003,27(4):495-499.

[6] 胡华业.高纯金属钪的制备 [J].稀土,1999,20(4):70-72.

[7] 陈雯,戴永年,唐文榕.金属铋真空蒸馏规律的研究 [J].真空科学与技术,1994,14(4):254-259.

[8] 陈雯,胡翠.金属铋在真空蒸发过程中临界压强的研究 [J].有色矿冶,2000,16(3):25-29.

[9] 李宗安,张炜,徐静，等.高纯金属铽制备工艺的研究 [J].稀土,2002,23(6):36-39.

[10] 周智华,莫红兵,曾冬铭.高纯铟的制备方法 [J].矿冶工程,2003,23(3):40-43.

[11] ALI S T,PRASAD D S,NUNIRATHNAM N R,et al.Purification of Tellurium by Single-Run Multiple Vacuum Distillation Technique [J].Separation Purification Technology,2005,43:263-267.

[12] ALI S T,NUNIRATHNAM N R,SUDHEER C,et al.Purification of Cadmium by Vacuum Distillation and Its Analysis [J].Materials Letters,2004,58:1 638-1 641.

[13] KOVALEVSKI S V,KOSYAKOV V I,SHELPAKOVA I R.Cadmium Purification by Vacuum Distillation in the Presence of Its Oxide:Thermodynamic Modeling and Experiment [J].Journal of Crystal Growth,1996,167:208-211.

[14] 金世平,杨斌,黄占超，等.真空蒸馏脱硒的研究 [J].真空科学与技术,2003,23(5):369-372.

[15] 周园，韩金铎，贾永忠，等.青海盐湖初级碳酸锂产品制备高纯金属锂研究 [J].稀有金属,2004,28(2):343-345.

[16] 戴永年.真空冶金 [M].北京:冶金工业出版社,2000：19-61,523-525.

[17] XIONG Li-zhi,HE Ze-qiang,LIU Wen-ping,et al.Preparation of High￣Purity Bismuth by Sulphur Deleadization in Vacuum distillation [J].Transactions of Nonferrous Metals Society of China，2004,14(6):1 210-1 214.

[18] 昆明理工大学真空冶金及材料研究所，真空蒸馏除铅制备高纯铋新工艺研究 [R].编号：（2003）53b200611,云南：云南省科学技术情报研究所，2003.

[19] 邱竹贤.冶金热化学 [M].北京:冶金工业出版社,1985:326-536.

[20] 苏联标准汇编 [S].前苏联，TOCT,109 28-75.

[21] 虞觉奇.二元合金状态图集 [M].上海:上海科学技术出版社出版,1987:223-240.