新型胺类萃取剂N1633萃取钨的研究
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摘要
采用自制的胺类萃取剂N1633作萃取剂,考察了其在钨萃取冶金中的性能。当有机相组成为40%N1633+40%异辛醇+磺化煤油(体积比),在p H=8.27、相比(O/A)为1∶1、振荡时间10 min、萃取温度25℃时,对WO_3含量116.25 g/L的钨酸钠溶液进行萃取,单级萃取率大于99%。绘制了N1633的萃取等温线,经过三级萃取饱和容量达到109.03 g/L。用2.5 mol/L的氨水对负载有机相进行反萃,相比2.5∶1时,反萃液中WO_3浓度达到174.31 g/L。绘制了负载有机相的反萃等温线,理论上以相比1.25∶1进行四级逆流萃取可将有机相中的钨基本反萃,反萃液中WO_3的饱和反萃浓度达到202.82 g/L。采用0.6 mol/L的硫酸以相比2∶1进行酸化再生后,N1633仍具有良好的萃取性能。
A self-made amine extractant N1633 was taken as an extraction agent in a metallurgical test on tungsten extraction for investigating its performance.With the organic phase composed of 40%N1633+40%isooctyl alcohol+sulfonated kerosene(v/v)with O/A of 1∶1,oscillation time of 10 min,and extraction temperature of 25℃,the sodium tungstate solution containing 116.25 g/L WO_3was extracted at p H of 8.27,showing the single-stage extraction rate above 99%.An extraction isotherm of N1633 was plotted.After three stages of extraction,the saturation capacity reached 109.03 g/L.Then,the loaded organic phase was stripped with 2.5 mol/L ammonia at O/A of 2.5∶1,leading to the concentration of tungsten in stripping solution at 174.31 g/L.A stripping isotherm of loaded organic phase was also plotted.It is found that most of tungsten in organic phase can be theoretically stripped at O/A of 1.25∶1 after a four-stage counter-current extraction,leading to the concentration of WO_3in stripping solution at 202.82 g/L.And after the regeneration with 0.6 mol/L H_2SO_4solution,N1633 was still good in the performance.
A self-made amine extractant N1633 was taken as an extraction agent in a metallurgical test on tungsten extraction for investigating its performance.With the organic phase composed of 40%N1633+40%isooctyl alcohol+sulfonated kerosene(v/v)with O/A of 1∶1,oscillation time of 10 min,and extraction temperature of 25℃,the sodium tungstate solution containing 116.25 g/L WO_3was extracted at p H of 8.27,showing the single-stage extraction rate above 99%.An extraction isotherm of N1633 was plotted.After three stages of extraction,the saturation capacity reached 109.03 g/L.Then,the loaded organic phase was stripped with 2.5 mol/L ammonia at O/A of 2.5∶1,leading to the concentration of tungsten in stripping solution at 174.31 g/L.A stripping isotherm of loaded organic phase was also plotted.It is found that most of tungsten in organic phase can be theoretically stripped at O/A of 1.25∶1 after a four-stage counter-current extraction,leading to the concentration of WO_3in stripping solution at 202.82 g/L.And after the regeneration with 0.6 mol/L H_2SO_4solution,N1633 was still good in the performance.
引文
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[15]Andersson I,Hastings J J,Howarth O W,et al.Aqueous molybdotungstates[J].Journal of the Chemical Society,Dalton Transactions,1994(7):1061-1066.
[16]柯兆华,张贵清,关文娟,等.季铵盐从碱性钨酸钠溶液中萃取钨的研究[J].稀有金属与硬质合金,2012(6):1-4.
[17]于亮,吴绍祖,程红光.季铵盐GW05和N263对Na2WO4溶液的萃钨性能对比研究[J].稀有金属,2015,39(3):193-200.
[2]Zaitsev V P,Ivanov I M,Kalish N K,et al.Scientific foundations of a new extraction technology for the processing of tungsten containing solutions[C]∥Proceeding of the Second International Conference on Hydrometallurgy(ICHM).Changsha:International Academic Publisher,1992:768-772.
[3]黄成通.钨的离子交换新工艺的发展[J].稀有金属与硬质合金,2003,31(3):37-41.
[4]张贵清.从碱性介质中萃取钨制取纯钨酸铵溶液的研究[D].长沙:中南工业大学冶金系,1994.
[5]Zhang G,Guan W,Xiao L,et al.A novel process for tungsten hydrometallurgy based on direct solvent extraction in alkaline medium[J].Hydrometallurgy,2016,165:233-237.
[6]李家杰.Na2WO4的溶剂萃取转化[J].稀有金属,1989(5):379-383.
[7]关文娟,张贵清.用季铵盐从模拟钨矿苏打浸出液中直接萃取钨[J].中国有色金属学报,2011,21(7):1756-1762.
[8]刘长畿.胺类萃取剂[J].有机化学,1979(1):72-91.
[9]朱屯.溶剂萃取与离子交换[M].北京:冶金工业出版社,2005.
[10]Baes C F,Mesmer R E.The hydrolysis of cations[M].New York:Wiley,1976.
[11]Cruywagen J J,van der Merwe I F J.Tungsten(VI)equilibria:a potentiometric and calorimetric investigation[J].Journal of the Chemical Society,Dalton Transactions,1987(7):1701-1705.
[12]Rozantsev G M,Sazonova O I.Thermodynamic parameters of interconversions of isopolyanions in solutions of tungsten(VI)[J].Russian Journal of Coordination Chemistry,2005,31(8):552-558.
[13]Tytko K H,Baethe G,Cruywagen J J.Equilibrium studies of aqueous polymolybdate solutions in 1 M sodium chloride medium at 25℃[J].Inorganic Chemistry,1985,24(20):3132-3136.
[14]Sano M,Shibata J,Harada M,et al.Extraction of Molybdenum and Tungsten with D2EHPA and LIX63[J].J Min Metall Inst Jpn,1988,104(1205):475-479.
[15]Andersson I,Hastings J J,Howarth O W,et al.Aqueous molybdotungstates[J].Journal of the Chemical Society,Dalton Transactions,1994(7):1061-1066.
[16]柯兆华,张贵清,关文娟,等.季铵盐从碱性钨酸钠溶液中萃取钨的研究[J].稀有金属与硬质合金,2012(6):1-4.
[17]于亮,吴绍祖,程红光.季铵盐GW05和N263对Na2WO4溶液的萃钨性能对比研究[J].稀有金属,2015,39(3):193-200.