Fe+Al+Ca溶液中的萃取除铁与载铁有机相水热反萃的研究
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摘要
以二（2-乙基己基）磷酸(P204)、磷酸三丁酯（TBP）、伯胺（N1923）和叔胺三烷基胺(N235)为萃取剂，研究了盐酸溶解铝矿石模拟溶液“FeCl~(3+)AlCl~(3+)CaCl2+HCl”中的溶剂萃取除铁与载铁有机相的水热反萃。考察了萃取剂、稀释剂、模拟液中各组分的浓度、萃取时间、温度、相比等因素对铁铝分离的影响。结果表明，以TBP和N235为萃取剂萃取分离Fe~(3+)与Al~(3+)时，其效果远远优于萃取剂P204，N1923。以TBP做萃取剂，盐酸浓度为3mol?L-1时，Fe的一级萃取率可以达到84.57%，Fe~(3+)和Al~(3+)的分离系数为643.9；以N235做萃取剂，盐酸浓度为3 mol?L-1时, Fe的一级萃取率可以达到99.89%，Fe~(3+)和Al~(3+)的分离系数可达到1.59×105。
以TBP和N235为负载铁的有机相，研究了反萃过程中水相的组成、温度、反萃取时间、相比等因素对氧化铁形成的影响，并对生成的氧化铁样品进行了XRD分析、TEM和SEM表征以及元素分析。XRD分析表明，在180℃时用1:5的氨水反萃取以TBP和N235为萃取剂制得的载铁有机相可得到结晶良好的α-Fe2O3。TEM和SEM的结果说明以负载铁的N235有机相制得的样品是粒度较为均匀的球形颗粒，元素分析可知其纯度在97.00%以上。
与传统的分离工艺相比，本文采用溶剂萃取法从盐酸溶液中分离铁和铝，萃取流程不存在沉淀、澄清、过滤以及铁渣污染等问题，且具有分离效果好、流程短、有机溶剂可循环利用、节省成本等优点，除铁的同时又能转化为高品质的氧化铁产品，初步解决了酸溶铝土矿新工艺条件下铁和铝的分离及铁的回收利用这个难题，为将来的工业应用奠定了理论基础。
The extractive separation of Fe and Al from the simulated liq uor ofFeCl~(3+)AlCl~(3+)CaCl2+HCl by bis(2-ethylhexyl) phosphoric acid(P204),tributylphospha te(TBP), Prima ry amine N1923 and trialkylamine(N235) and thehydrolytic stripping of Fe from the organic phase have been studied. Some factorsinfluencing the extractive separation of Fe and Al, such as extracta nt, diluents, ironconcentration in aqueous phase, extractive time and temperature, ratio of organicphase and water phase were investigated. The experimental results indica ted that theextracta nt TBP and N235 are much effectiver tha n P204 and N1923 for separation ofFe and Al. The extraction percentage of Fe is 84.57% in 3 Molar HCl, and theseparation factor of Fe3 +/Al~(3+) is 643.9. The extraction percentage of Fe is 99.89%, andthe separation factor of Fe3 +/Al~(3+) is 1.59×105 for N235 in the same conditions.
Some factors influencing the stripping experiment, such as the composition insimulated liq uor, stripping temperature and time, ratio of organic phase loaded ironand water phase were investigated, and the samples were tested by XRD, TEM, SEMand element analysis. The X-ray powder diffraction patterns that the Fe2O3 powdersobtained from the organic phase loaed iron by TBP and N235 was well crysta llizedand composed ofα- Fe2O3. The TEM and SEM ima ges showd that the particles ofFe2O3 obtained from the N235 organic phase powers were spherical fine crysta llitesand the purity of the particles can get much tha n 97.00 percent.
Compared to traditiona l separation technologica l, a whole extractive process forthe separation of iron(Ⅲ) and aluminum from hydrochloric acid was described. Itdoes not have so much complex problems，such as precipitation clarifica tion, filtering,leaching and scruff pollution. It has better separation efficiency, significa nt costsavings , simple process and organic solvents can be recycled. In this process, it madeiron into high-quality iron products removing iron at the same time. It resolved theproblem of separation of iron and aluminum and the recycling of iron first. Under theconditions of acid-soluble bauxite it la id a theoretica l basis for the practicalapplica tion in the future.
以TBP和N235为负载铁的有机相，研究了反萃过程中水相的组成、温度、反萃取时间、相比等因素对氧化铁形成的影响，并对生成的氧化铁样品进行了XRD分析、TEM和SEM表征以及元素分析。XRD分析表明，在180℃时用1:5的氨水反萃取以TBP和N235为萃取剂制得的载铁有机相可得到结晶良好的α-Fe2O3。TEM和SEM的结果说明以负载铁的N235有机相制得的样品是粒度较为均匀的球形颗粒，元素分析可知其纯度在97.00%以上。
与传统的分离工艺相比，本文采用溶剂萃取法从盐酸溶液中分离铁和铝，萃取流程不存在沉淀、澄清、过滤以及铁渣污染等问题，且具有分离效果好、流程短、有机溶剂可循环利用、节省成本等优点，除铁的同时又能转化为高品质的氧化铁产品，初步解决了酸溶铝土矿新工艺条件下铁和铝的分离及铁的回收利用这个难题，为将来的工业应用奠定了理论基础。
The extractive separation of Fe and Al from the simulated liq uor ofFeCl~(3+)AlCl~(3+)CaCl2+HCl by bis(2-ethylhexyl) phosphoric acid(P204),tributylphospha te(TBP), Prima ry amine N1923 and trialkylamine(N235) and thehydrolytic stripping of Fe from the organic phase have been studied. Some factorsinfluencing the extractive separation of Fe and Al, such as extracta nt, diluents, ironconcentration in aqueous phase, extractive time and temperature, ratio of organicphase and water phase were investigated. The experimental results indica ted that theextracta nt TBP and N235 are much effectiver tha n P204 and N1923 for separation ofFe and Al. The extraction percentage of Fe is 84.57% in 3 Molar HCl, and theseparation factor of Fe3 +/Al~(3+) is 643.9. The extraction percentage of Fe is 99.89%, andthe separation factor of Fe3 +/Al~(3+) is 1.59×105 for N235 in the same conditions.
Some factors influencing the stripping experiment, such as the composition insimulated liq uor, stripping temperature and time, ratio of organic phase loaded ironand water phase were investigated, and the samples were tested by XRD, TEM, SEMand element analysis. The X-ray powder diffraction patterns that the Fe2O3 powdersobtained from the organic phase loaed iron by TBP and N235 was well crysta llizedand composed ofα- Fe2O3. The TEM and SEM ima ges showd that the particles ofFe2O3 obtained from the N235 organic phase powers were spherical fine crysta llitesand the purity of the particles can get much tha n 97.00 percent.
Compared to traditiona l separation technologica l, a whole extractive process forthe separation of iron(Ⅲ) and aluminum from hydrochloric acid was described. Itdoes not have so much complex problems，such as precipitation clarifica tion, filtering,leaching and scruff pollution. It has better separation efficiency, significa nt costsavings , simple process and organic solvents can be recycled. In this process, it madeiron into high-quality iron products removing iron at the same time. It resolved theproblem of separation of iron and aluminum and the recycling of iron first. Under theconditions of acid-soluble bauxite it la id a theoretica l basis for the practicalapplica tion in the future.
引文
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[2]谢岷,铝土矿选矿试验研究,有色金属(选矿部分)，1995，(6)：12～16
[3]R.Bhima Rao.Novel approach for the beneficiation of ferruginous bauxite bymicrowa ve,Minera ls And Metallurgical processing,1996,13 (3):103～106
[4]Pha lguni Anand, Biobeneficiation of Bacillus polymyx: Calcium and iron remova l.Int. J. Miner. Process, 1996 ,48:51～60
[5]李军亮，周吉奎，生物浸出脱除铝土矿选矿尾矿中铁矿物的实验研究,矿业研究与开发，2006，26(2)，55～57
[6]Kan Sen Chou, Extracting iron from aluminium sulfate solution, Hydrometa llurgy ,1986, 15(3), 391
[7]马建民，曹智战，一种生产优质硫酸铝的新方法，信阳师范学院学报(自然科学版)，1999，12(2):228～230.
[8]吴建宁，蔡会武，郭红梅等，从含铁硫酸铝中除铁，湿法冶金，2005，24(3)：155～158.
[9]谢玉群，童九如，高岭土生产硫酸铝及沉淀法除铁的研究，现代化工，1996(2):26～27
[10]梅永进，陆英英，工业硫酸铝除铁实验，鹭江职业大学学报，2002，10(1): 73～75.
[11]魏永聪，林庆扬，高岭土电解除铁初探，华侨大学学报（自然科学版），1990，1（2）：147～153
[12]刘安昌，利用工业废硫酸制备高纯度无铁离子硫酸铝，化工生产与技术，2002,9(4),7～10
[13]H.W. Flood , Removel of ferric iron from aqueous solution of aluminiumsa lts ,USPatent , 35864771971 206222
[14]田衡水，唐崇千，苏元复,协同萃取法从湿法磷酸中分离铁,华东化工学院学报,1988,14 (5) ,544
[15]贵阳铝镁设计研究院科研室,伯胺萃取除去硫酸铝溶液中的杂质铁的试验,轻金属,1980, (6) ,6
[16]于淑秋等,用叔胺自硫酸铝溶液中萃取除铁,中国专利，CN 85100720，1987207230
[17]于淑秋,伍志春,叔胺自硫酸铝溶液中萃取铁,化工冶金,1988，9 (3)，34
[18]Dalton, R.F., The Cuprex meta l extraction process:recovering from sulfide ores,Journal of Inorganic Materia ls,1991,43(8),51～56
[19]袁承业，N1923从硫酸铝溶液中除铁,有机化学.1979，1:33～35
[20]A.P.Paiva, M.C. Costa, Application of N,N-Tetrasubstituted ma lonaa mides to therecovery of iron(Ⅲ) from choloride solutions , Hydrometa llurgy, 2005, 77(3),103～108
[21]Chen Jia yong,Yu Shuqiu,liu Huizhou etal,New mixed solvent systems for theextraction and separation of ferric iron in sulphate solutions , Hydrometa llurgy,1992, 30(1),401
[22]Stefanakis M I, Monhemius A J.Computer modeling of the solvent extraction ofiron by Versatic acid from aluminum nitrate solutions. Hydrometa llurgy. 1987, 19(2):187～198
[23]Preston J S.Solvent extraction of meta ls by carboxylic acids. Hydrometa llurgy.1985,14(2):171～188
[24]C.Mouvet,Cla veri,Bruno.Loca liza tion of copper accumula ted in Rhynchostegiumri Parioides using sequential chemica l extraction.Aq uatic Botany，1999(2) 63:1～10
[25]陆九芳，李总称，包铁竹等，分离过程化学，北京，1993，清华大学出版社，42～45
[26]Zhichun W，Shuqiu Y，Chen J.Extraction of Fe(III)from sulfate solutions withtertiary amines as solvent [C].IN Proceedings of the Internationa l SolventExtraction Conferrence.1988，(3):276～281
[27]于淑秋，位阻和溶剂效应对胺类萃取铁的影响及其作用机理的讨论，化工冶金，1986，(15)：45～52
[28]高翠英,纳米氧化铁的性质及制备方法进展，广西轻工业，2007，1（1），37～38
[29]Sesigur H, Acma E, Addemir O. The preparation of Magnetic iron oxide. MaterRes Bull,1996,31(2):1573～1579
[30]张强，超细氧化铁的制备进展，无机盐工业,2005,37(1),7～11
[31]董睿，姜继森，杨焱龙，非水介质中制备纳米氧化铁，无机材料学报, 2002, 17(5) : 967～972
[32]王兴尧，康晓红，谢慧琴等，水热反萃法制备纳米α-Fe2O3，应用化学，2004，21（7）：655～659
[33]Doyle-Garner F M, Monhemius A J, Hydrolytic Stripping of Single and MixedMeatal-Versatic Solutions,Meta llurgica l Transactions B,1985,16B:671～677
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