碘化法制备高纯金属钛
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摘要
以工业海绵钛为原料,研究了海绵钛碘化提纯过程中原料温度和K值对沉积速率的影响。结果表明,当K值一定时,沉积速率先随原料温度的升高而增加,而当原料温度大于600℃时,随原料温度升高沉积速率增速明显变缓。当原料温度一定时,沉积速率随K值的升高而增加。在原料温度600℃,K值80的工艺条件下,进行了多批次试验,结果表明,结晶棒直径可达23～26 mm,总收率约98%,所得可锻性高纯金属钛结晶棒产品晶粒粗大,表面光亮,沉积速率达到30 g/(h·m)左右,生产效率较高。同时,钛提纯效果显著,纯度达到4 N级以上。
In this paper,the influences of raw material temperature and K value on the average deposition rate for iodization reaction were studied using industrial sponge titanium as raw material.The results show that the deposition rate increases with raw material temperature rising at a fixed K value,while the deposition rate increases at an obviously slow trend with raw material temperature over 600 ℃.Furthermore,the deposition rate increases with increase of K value at a certain raw material temperature.At a raw material temperature of 600 ℃ and K value of 80,multi-batch trial production results show that the diameter of the obtained crystal rods is about 23～26 mm with a total yield rate of about 98% and a deposition rate of 30 g/(h·m).Meanwhile,the prepared forgeable high-purity metallic titanium owns a thick grain size,shining surface and a purity higher than 99.99%,showing an excellent purification effect.
In this paper,the influences of raw material temperature and K value on the average deposition rate for iodization reaction were studied using industrial sponge titanium as raw material.The results show that the deposition rate increases with raw material temperature rising at a fixed K value,while the deposition rate increases at an obviously slow trend with raw material temperature over 600 ℃.Furthermore,the deposition rate increases with increase of K value at a certain raw material temperature.At a raw material temperature of 600 ℃ and K value of 80,multi-batch trial production results show that the diameter of the obtained crystal rods is about 23～26 mm with a total yield rate of about 98% and a deposition rate of 30 g/(h·m).Meanwhile,the prepared forgeable high-purity metallic titanium owns a thick grain size,shining surface and a purity higher than 99.99%,showing an excellent purification effect.
引文
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[16] Yin Yanxi,Hu Zhifang,Tian Lisen,et al.Air-cooling temperature control device for reaction furnace body,CN :CN202925075U[P].2013-05-08.(尹延西,胡志方,田丽森,等.一种反应炉炉体风冷控温装置,中国:CN202925075U[P].2013-05-08.)
[2] Yu Zhentao,Zhang Minghua,Yu Sen,et al.Analysis of R & D,production and application of biomedical Ti alloys materials applied in medical devices of China[J].China Medical Device Information,2012,18(7):1-8.(于振涛,张明华,余森,等.中国医疗器械用钛合金材料研发、生产与应用现状分析[J].中国医疗器械信息,2012,18(7):1-8.)
[3] Jiang Dongwen,Zheng Lijing,Zhou Lei,et al.High temperature tensile properties of directionally solidified Ni-43Ti-4Al-2Nb-2Hf alloy[J].Rare Metals,2012,31(4):328-331.
[4] Liu Zhenghong,Chen Zhiqiang.Application of high purity titanium and methods to produce it[J].Materials China,2008,27(2):1-8.(刘正红,陈志强.高纯钛的应用及其生产方法[J].中国材料进展,2008,27(2):1-8.)
[5] Chen Xiaohu,Wang Hua,Liu Yimin,et al.Thermodynamic analysis of production of high purity titanium by thermal decomposition of titanium iodide[J].Transactions of Nonferrous Metals Society of China,2009,19(5):1348-1352.
[6] Kotsar M L ,Morenko O G,Shtutsa M G,et al.Obtaining of high-purity titanium,zirconium and hafnium by the method of iodide refining in industrial conditions[J].Inorganic Materials,2010,46(3):282-290.
[7] Tian Lisen,Yin Yanxi,Hu Zhifang,et al.Research progress of high purity metal hafnium preparation[J].Mining and Metallurgy,2014,23(2):49-54.(田丽森,尹延西,胡志方,等.高纯金属铪制备技术研究进展[J].矿冶,2014,23(2):49-54.)
[8] Tian Lisen,Yin Yanxi,Hu Zhifang,et al.Deposition of hafnium crystal bar by iodide process[J].Rare Metals,2014,33(2):161-165.
[9] Hu Zhifang,Yin Yanxi,Jiang Honglin.Prevention iodine steam escape structure of iodate purification reactor,CN:CN206956118U[P].2018-02-02.(胡志芳,尹延西,江洪林.一种碘化提纯反应器的阻止碘蒸汽逃逸结构,中国:CN206956118U[P].2018-02-02.)
[10] Jiang Honglin,Hu Zhifang,Yin Yanxi.Female silk connecting device of metal iodate purification reacting furnace electrode,CN:CN205616939U[P].2016-10-05.(江洪林,胡志方,尹延西.金属碘化提纯反应炉电极母丝连接装置,中国:CN205616939U[P].2016-10-05.)
[11] Jiang Honglin,Hu Zhifang,Yin Yanxi,et al.Iodate purification reacting furnace iodized controlling means,CN:CN205473930U[P].2016-08-17.(江洪林,胡志方,尹延西,等.一种碘化提纯反应炉加碘控制装置,中国:CN205473930U[P].2016-08-17.)
[12] Wang Lijun,Tian Lisen,Yin Yanxi,et al.Molten salt heat exchange temperature control device for reaction furnace body,CN:CN203683628U[P].2014-07-02.(王力军,田丽森,尹延西,等.一种反应炉炉体的熔盐换热控温装置,中国:CN203683628U[P].2014-07-02.)
[13] Wang Lijun,Tian Lisen,Yin Yanxi,et al.Molten-salt heat-exchange temperature-controlling device and method of reaction furnace body,CN:CN104762487A[P].2015-07-08.(王力军,田丽森,尹延西,等.一种反应炉炉体的熔盐换热控温装置及方法,中国:CN104762487A[P].2015-07-08.)
[14] Yin Yanxi,Hu Zhifang,Tian Lisen,et al.Iodinating and purifying device and molten salt heat exchange method based on same,CN:CN103805790A[P].2014-05-21.(尹延西,胡志方,田丽森,等.一种碘化提纯装置及其熔盐换热方法,中国:CN103805790A[P].2014-05-21.)
[15] Yin Yanxi,Tian Lisen,Hu Zhifang,et al.Iodination-purification reaction unit for rare metals,CN:CN202925073U[P].2013-05-08.(尹延西,田丽森,胡志方,等.一种稀有金属碘化提纯反应装置,中国: CN202925073U[P].2013-05-08.)
[16] Yin Yanxi,Hu Zhifang,Tian Lisen,et al.Air-cooling temperature control device for reaction furnace body,CN :CN202925075U[P].2013-05-08.(尹延西,胡志方,田丽森,等.一种反应炉炉体风冷控温装置,中国:CN202925075U[P].2013-05-08.)