超声辅助二壬基萘磺酸萃取镁的工艺研究
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摘要
为提高冶金废水中镁离子回收萃取效率,缩短萃取时间,实现连续进料萃取工艺。采用超声辅助二壬基萘磺酸萃取冶金废水中的镁离子,分别考察了二壬基萘磺酸浓度、超声变幅杆浸入液面深度、萃取时间、超声器功率和有机相与水相体积比(相比)等因素对镁离子萃取率的影响。结果表明,超声辅助萃取的萃取速度是传统萃取方法的20倍,节约了大量萃取时间。最佳工艺条件为:25℃,萃取剂浓度0.8 mol×L~(-1),变幅杆浸入深度5 mm,超声萃取时间2 min,超声萃取功率108 W,相比3:1。紫外分析结果表明超声作用不会破坏萃取剂的结构与性能,萃取剂能够再生后重复利用。因此,与传统间歇萃取法相比,该工艺将更利于实现连续进料萃取,从而提高生产效率。
An ultrasound-assisted process for magnesium(Mg2+) extraction from metallurgy wastewater was developed using dinonyl naphthalene sulfonic acid. Effects of extractant concentration, immersion depth of ultrasonic horn, extraction time, ultrasonic power and the volume ratio of organic phase and aqueous phase(O/A) on Mg~(2+) extraction were investigated. The results show that ultrasonic-assisted extraction can decrease extraction time and improve extraction speed for 20 times. The optimal process parameters are: 25℃, extractant concentration = 0.8 mol×L~(-1), immersion depth of ultrasonic horn = 5 mm, ultrasonic extraction time = 2 minutes,extraction power = 108 W and O/A ratio = 3:1. UV spectrophotometry analysis shows that ultrasonic irradiation does not destroy the structure and performance of the extractant which can be reused after regeneration.Therefore, the ultrasonic-assisted process is beneficial for continuous Mg~(2+) extraction and improves productivity.
An ultrasound-assisted process for magnesium(Mg2+) extraction from metallurgy wastewater was developed using dinonyl naphthalene sulfonic acid. Effects of extractant concentration, immersion depth of ultrasonic horn, extraction time, ultrasonic power and the volume ratio of organic phase and aqueous phase(O/A) on Mg~(2+) extraction were investigated. The results show that ultrasonic-assisted extraction can decrease extraction time and improve extraction speed for 20 times. The optimal process parameters are: 25℃, extractant concentration = 0.8 mol×L~(-1), immersion depth of ultrasonic horn = 5 mm, ultrasonic extraction time = 2 minutes,extraction power = 108 W and O/A ratio = 3:1. UV spectrophotometry analysis shows that ultrasonic irradiation does not destroy the structure and performance of the extractant which can be reused after regeneration.Therefore, the ultrasonic-assisted process is beneficial for continuous Mg~(2+) extraction and improves productivity.
引文
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[7]YANG Wei-jun(阳卫军),ZHU Li-jun(朱利军),QU Xiao-juan(屈晓娟).Study on removal of calcium and magnesium ions from leaching solution of poor pyrolusite by extraction(萃取法去除贫软锰矿浸出液中钙、镁离子的研究)[J].Journal of Hunan University(Natural Sciences)(湖南大学学报(自然科学版)),2014,41(12):83-88.
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[10]HAN Lu-lu(韩路路),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊).et al.Study of magnesium ions in purified wet-process phosphoric acid by synergic extraction(协同萃取净化湿法磷酸中镁离子的研究)[J].Chemical Fertilizer Industry(化肥工业),2015,42(1):10-12.
[11]JIANG De-min(蒋德敏),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊),et al.Study on preparation of magnesium sulphate by extraction and recovery of magnesium from metallurgy wastewater(从冶金废水中萃取回收镁制备硫酸镁的研究)[J].Inorganic Chemicals Industry(无机盐工业),2015,47(10):61-64.
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[13]JIANG De-min(蒋德敏),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊),et al.Stipping of magnesium from magnesium-containing dinonyl naphthalene sulfonic acid-erosene solution(从含镁二壬基萘磺酸-磺化煤油溶液中反萃取镁的研究)[J].Chemical Research and Application(化学研究与应用),2015,27(5):733-736.
[14]Yin P F,Sun L L,Han X Y,et al.Controlled synthesis of cobalt sulfide nanocrystalline by ultrasonic spray pyrolysis process[J].Rare Metal Materials and Engineering,2016,45(7):1700-1704.
[15]Yang Y,Wang Z J,Bi S,et al.Raman spectroscopy study structural changes in black bean protein isolate upon ultrasonic treatment[J].Spectroscopy and Spectral Analysis,2016,36(7):2318-2324.
[16]Khalifa W,Tsunekawa Y.Production of grain-refined AC7A Al-Mg alloy via solidification in ultrasonic field[J].Transactions of Nonferrous Metals Society of China,2016,26(4):930-937.
[17]Hu J,Jia X J,Fang X B,et al.Ultrasonic extraction antioxidant and anticancer activities of novel polysaccharides from chuanxiongrhizome[J].International Journal of Biological Macromolecules,2016,85:277-284.
[18]Khezeli T,Daneshfar A,Sahraei R.A green ultrasonic assisted liquid-liquid microextraction based on deep eutectic solvent for the HPLC-UV determination of ferulic,caffeic and cinnamic acid from olive,almond,sesame and cinnamon oil[J].Talanta,2016,150:577-585.
[19]Lv X B,Liu D J,Ji J Y,et al.UItrasound-assisted extraction of Fe(Ш)from wet-process phosphoric acid[J].Solvent Extraction Research and Development,2017,24(1):11-22.
[20]WANG Peng(王鹏),BAI Min-li(白敏丽),LüJi-zu(吕继组),et al.Turbulent flow characteristics of nanofluids inside circular tube(纳米流体圆管内的湍流流动特性)[J].CIESC Journal(化工学报),2014,65(S1):17-26.
[21]MA Kong-jun(马空军),WU Xiao-xia(吴晓霞),ZHANG Hua-yu(张华余),et al.Mechanisms of enhanced mass transfer induced by interfacial turbulence under ultrasonic cavitation(超声空化引起界面湍动促进的传质机理)[J].Applied Acoustics(应用声学),2013,32(5):348-353.
[2]GUAN Qing-jun(管青军),LUO Peng-hui(骆朋辉),GUO Liang(郭亮),et al.Separation of magnesium,calcium and low content of nickel and cobalt from bioleaching solution by versatic10(versatic10萃取分离微生物浸出液中钙镁和低含量镍钴)[J].Nonferrous Metals(Extractive Metallurgy)(有色金属(冶炼部分)),2016(3):1-5.
[3]Guan Q J,Sun W,Zhou G Y,et al.Recovery of cobalt and nickel in the presence of magnesium and calcium from sulfate solutions by versatic 10 and mixtures of versatic 10 and cyanex 301[J].Transactions of Nonferrous Metals Society of China,2016,26(3):865-873.
[4]LI Liang(李亮),WANG Zhi-fen(王芝芬),ZHANG Dong-xiang(张东翔),et al.Research on Sr2+extraction with p-tert-butylcalix[6]arene(对叔丁基杯[6]甲酯芳烃萃取Sr2+的特性研究)[J].Journal of Chemical Engineering of Chinese Universities(高校化学工程学报),2015,29(6):1496-1501.
[5]LIU Jiu-miao(刘久苗),TAN Ding-sheng(谈定生),JIANG Jian-jun(江建军),et al.Research on separating calcium and magnesium from nickel sulfate with P507(用P507从硫酸镍溶液中萃取分离钙镁的研究)[J].Shanghai Nonferrous Metals(上海有色金属),2002,23(4):149-152.
[6]HE Bin-bin(何宾宾),LIANG Yu-jun(梁玉军),YANG Chao(杨超).Research on separating of manganese and magnesium from qualified solution of electrolytic manganese(电解金属锰合格液中锰镁的萃取分离研究)[J].China’s Manganese Industry(中国锰业),2010,28(1):41-44.
[7]YANG Wei-jun(阳卫军),ZHU Li-jun(朱利军),QU Xiao-juan(屈晓娟).Study on removal of calcium and magnesium ions from leaching solution of poor pyrolusite by extraction(萃取法去除贫软锰矿浸出液中钙、镁离子的研究)[J].Journal of Hunan University(Natural Sciences)(湖南大学学报(自然科学版)),2014,41(12):83-88.
[8]XU Bi(徐碧),LIU Dai-jun(刘代俊),YU Jing(余静),et al.Study of magnesium ion extraction from phosphoric acid by DNNSA reverse micelles(DNNSA反胶团溶液净化磷酸中镁的研究)[J].Chemical Research and Application(化学研究与应用),2009,21(4):590-593.
[9]YU Jing(余静),LIU Dai-jun(刘代俊).Kinetics of reverse micelles extraction of magnesium from phosphoric acid solution(反胶团萃取磷酸溶液中镁的动力学)[J].Journal of Chemical Engineering of Chinese Universities(高校化学工程学报),2009,23(6):939-944.
[10]HAN Lu-lu(韩路路),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊).et al.Study of magnesium ions in purified wet-process phosphoric acid by synergic extraction(协同萃取净化湿法磷酸中镁离子的研究)[J].Chemical Fertilizer Industry(化肥工业),2015,42(1):10-12.
[11]JIANG De-min(蒋德敏),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊),et al.Study on preparation of magnesium sulphate by extraction and recovery of magnesium from metallurgy wastewater(从冶金废水中萃取回收镁制备硫酸镁的研究)[J].Inorganic Chemicals Industry(无机盐工业),2015,47(10):61-64.
[12]Yu J,Liu D J.Extraction of magnesium from phosphoric acid using dinonylnaphthalene sulfonic acid[J].Chemical Engineering Research and Design,2010,88:712-717.
[13]JIANG De-min(蒋德敏),CHEN Jian-jun(陈建钧),LIU Dai-jun(刘代俊),et al.Stipping of magnesium from magnesium-containing dinonyl naphthalene sulfonic acid-erosene solution(从含镁二壬基萘磺酸-磺化煤油溶液中反萃取镁的研究)[J].Chemical Research and Application(化学研究与应用),2015,27(5):733-736.
[14]Yin P F,Sun L L,Han X Y,et al.Controlled synthesis of cobalt sulfide nanocrystalline by ultrasonic spray pyrolysis process[J].Rare Metal Materials and Engineering,2016,45(7):1700-1704.
[15]Yang Y,Wang Z J,Bi S,et al.Raman spectroscopy study structural changes in black bean protein isolate upon ultrasonic treatment[J].Spectroscopy and Spectral Analysis,2016,36(7):2318-2324.
[16]Khalifa W,Tsunekawa Y.Production of grain-refined AC7A Al-Mg alloy via solidification in ultrasonic field[J].Transactions of Nonferrous Metals Society of China,2016,26(4):930-937.
[17]Hu J,Jia X J,Fang X B,et al.Ultrasonic extraction antioxidant and anticancer activities of novel polysaccharides from chuanxiongrhizome[J].International Journal of Biological Macromolecules,2016,85:277-284.
[18]Khezeli T,Daneshfar A,Sahraei R.A green ultrasonic assisted liquid-liquid microextraction based on deep eutectic solvent for the HPLC-UV determination of ferulic,caffeic and cinnamic acid from olive,almond,sesame and cinnamon oil[J].Talanta,2016,150:577-585.
[19]Lv X B,Liu D J,Ji J Y,et al.UItrasound-assisted extraction of Fe(Ш)from wet-process phosphoric acid[J].Solvent Extraction Research and Development,2017,24(1):11-22.
[20]WANG Peng(王鹏),BAI Min-li(白敏丽),LüJi-zu(吕继组),et al.Turbulent flow characteristics of nanofluids inside circular tube(纳米流体圆管内的湍流流动特性)[J].CIESC Journal(化工学报),2014,65(S1):17-26.
[21]MA Kong-jun(马空军),WU Xiao-xia(吴晓霞),ZHANG Hua-yu(张华余),et al.Mechanisms of enhanced mass transfer induced by interfacial turbulence under ultrasonic cavitation(超声空化引起界面湍动促进的传质机理)[J].Applied Acoustics(应用声学),2013,32(5):348-353.
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