黑云母硫酸浸出液回收铁铝及提取钾镁研究
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摘要
针对硫酸分解黑云母得到的酸浸液的高效清洁利用问题,研究了针铁矿法回收铁铝沉淀物、沉淀法制取氢氧化镁、蒸发析晶法分离硫酸钾铵和硫酸铵的过程。结果表明,酸浸液中Fe_2O_3的回收率为99.8%、Al_2O_3的回收率为99.4%,回收的铁铝氢氧化物可制备氧化铝和氧化铁红;氨化精制溶液制取了结晶良好的氢氧化镁制品,精制溶液中MgO的沉淀率为86.2%。依据5%NH_3-K_2SO_4-(NH_4)_2SO_4-H_2O体系相图,分析了从硫酸钾铵溶液中析出硫酸钾铵并回收硫酸铵的过程。整个工艺简捷高效,为黑云母资源化利用提供了新的技术途径。
Aiming at the efficient cleaning and utilization of sulfuric acid leaching solution from biotite dissolved by sulfuric acid solution,the processes of recovering iron and aluminum precipitates by goethite method,preparing magnesium hydroxide by precipitation method,and separating ammonium potassium sulfate and ammonium sulfate by evaporation crystallization method were studied.The results showed that the recoveries of Fe_2 O_3 and Al_2 O_3 from sulfuric acid leaching solution were 99.8%and 99.4%respectively,and aluminum oxide and iron oxide red could be prepared from the recovered iron-aluminum hydroxides.Magnesium hydroxide products with good crystallization were prepared by ammonia refined solution.The precipitation rate of MgO in the refining solution was 86.2%,the process of precipitation of potassium ammonium sulfate and recovery of ammonium sulfate from ammonium potassium sulfate solution was analyzed according to the 5%NH_3-K_2 SO_4-(NH_4)_2 SO_4-H_2 O phase diagram.The whole process is simple and efficient,which provides a new technical approach for the utilization of biotite resources.
Aiming at the efficient cleaning and utilization of sulfuric acid leaching solution from biotite dissolved by sulfuric acid solution,the processes of recovering iron and aluminum precipitates by goethite method,preparing magnesium hydroxide by precipitation method,and separating ammonium potassium sulfate and ammonium sulfate by evaporation crystallization method were studied.The results showed that the recoveries of Fe_2 O_3 and Al_2 O_3 from sulfuric acid leaching solution were 99.8%and 99.4%respectively,and aluminum oxide and iron oxide red could be prepared from the recovered iron-aluminum hydroxides.Magnesium hydroxide products with good crystallization were prepared by ammonia refined solution.The precipitation rate of MgO in the refining solution was 86.2%,the process of precipitation of potassium ammonium sulfate and recovery of ammonium sulfate from ammonium potassium sulfate solution was analyzed according to the 5%NH_3-K_2 SO_4-(NH_4)_2 SO_4-H_2 O phase diagram.The whole process is simple and efficient,which provides a new technical approach for the utilization of biotite resources.
引文
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[17]章永洁,曹吉林,李琳.25 oC K2SO4-(NH4)2SO4-H2O体系溶解度计算[J].河北工业大学学报,2002,31(5):19-22.
[18]Xue C Y,Zhao B,Guo H F,et al.Phase equilibrium of the quaternary system K2SO4-MgSO4-(NH4)2SO4-H2O at 25°C[J].Fluid Phase Equilibria,2016,408:115-122.
[19]杨静,蒋周青,马鸿文,等.中国铝资源与高铝粉煤灰提取氧化铝研究进展[J].地学前缘,2014,21(5):313-324.
[20]何苏萍,高倩,余晓婷,等.氧化铁红的制备方法及其在涂料中的应用[J].化工生产与技术,2011,18(1):29-32.
[21]曹吉林,章永洁,李琳,等.25 oC NH3-K2SO4-(NH4)2SO4-H2O体系相平衡的研究[J].海湖盐与化工,2002,31(6):6-8.
[22]范芸珠,曹发海.硫酸铵热分解反应动力学研究[J].高校化学工程学报,2011,25(2):341-346.
[23]王艳梅,刘梅堂,孙华,等.磷石膏转氨法制硫酸技术原理与过程评价[J].化工进展,2015,34(S1):196-201.
[24]Casas J M,Crisóstomo G,Cifuentes L.Speciation of the Fe(II)-Fe(III)-H2SO4-H2O system at 25and 50℃[J].Hydrometallurgy,2005,80(4):254-264.
[25]Kobylin P,Kaskiala T,Salminen J.Modeling of H2SO4-FeSO4-H2O and H2SO4-Fe2(SO4)3-H2O systems for metallurgical applications[J].Industrial &Engineering Chemistry Research,2007,46(8):2601-2608.
[26]Yue G,Zhao L,Olvera O G,et al.Speciation of the H2SO4-Fe2(SO4)3-FeSO4-H2O system and development of an expression to predict the redox potential of the Fe3+/Fe2+couple up to 150°C[J].Hydrometallurgy,2014,147:196-209.
[2]Luo Z,Yang J,Ma H W,et al.Recovery of magnesium and potassium from biotite by sulfuric acid leaching and alkali precipitation with ammonia[J].Hydrometallurgy,2015,157:188-193.
[3]马玺.黑云母酸法分解制取硫酸钾及缓释钾肥关键反应研究[D].北京:中国地质大学(北京),2016.
[4]何小凤,李运刚,陈金.镀锌灰的热酸浸出和除铁试验研究[J].湿法冶金,2014,33(6):463-465.
[5]岳明,孙宁磊,邹兴,等.锌浸出液三价铁直接水解赤铁矿法除铁的探讨[J].中国有色冶金,2012,41(4):80-85.
[6]吴远桂,谈定生,丁伟中,等.针铁矿法除铁及其在湿法冶金中的应用[J].湿法冶金,2014,33(2):86-89.
[7]刘铭,周雍茂.用N235-TBP混合体系从硫酸盐溶液中协同萃取除铁[J].中国有色金属学报,2006,15(10):1648-1654.
[8]肖超,李婕,吴海国.硫酸法提取铍工艺中铝杂质分离的研究现状[J].稀有金属与硬质合金,2013,41(3):8-10.
[9]旷戈,郭慧,刘善军,等.锂云母矿石提锂浸取液体系中除铝的研究[J].稀有金属,2014,38(1):102-107.
[10]王乐,翟玉春,申晓毅,等.针铁矿法同时除硫酸锌溶出液中的铁和铝[J].中国稀土学报,2012,30:953-955.
[11]孙宁磊,刘金山,王魁珽,等.某厂红土镍矿酸浸沉镍后液综合回收镁[J].矿冶,2013,22(S11):129-132.
[12]Ma X,Ma H,Jiang X,et al.Preparation of magnesium hydroxide nanoflowers from boron mud via anti-drop precipitation method[J].Materials Research Bulletin,2014,56:113-118.
[13]曹吉林,谭朝阳.氯化钾硫酸转化法制硫酸氢钾的研究[J].化工科技,2000,8(6):26-28.
[14]曹吉林,章永洁,李琳.氯化钾和硫酸分步反应制备氮钾硫肥的研究[J].海湖盐与化工,2002,31(4):9-11.
[15]章永洁,曹吉林,任宝山,等.硫酸钾生产方法综述[J].化肥设计,2003,41(1):8-11.
[16]曹吉林,章永洁,纪志永,等.25 oC K2SO4-(NH4)2SO4-H2O体系相平衡的研究[J].河北工业大学学报,2002,31(3):14-17.
[17]章永洁,曹吉林,李琳.25 oC K2SO4-(NH4)2SO4-H2O体系溶解度计算[J].河北工业大学学报,2002,31(5):19-22.
[18]Xue C Y,Zhao B,Guo H F,et al.Phase equilibrium of the quaternary system K2SO4-MgSO4-(NH4)2SO4-H2O at 25°C[J].Fluid Phase Equilibria,2016,408:115-122.
[19]杨静,蒋周青,马鸿文,等.中国铝资源与高铝粉煤灰提取氧化铝研究进展[J].地学前缘,2014,21(5):313-324.
[20]何苏萍,高倩,余晓婷,等.氧化铁红的制备方法及其在涂料中的应用[J].化工生产与技术,2011,18(1):29-32.
[21]曹吉林,章永洁,李琳,等.25 oC NH3-K2SO4-(NH4)2SO4-H2O体系相平衡的研究[J].海湖盐与化工,2002,31(6):6-8.
[22]范芸珠,曹发海.硫酸铵热分解反应动力学研究[J].高校化学工程学报,2011,25(2):341-346.
[23]王艳梅,刘梅堂,孙华,等.磷石膏转氨法制硫酸技术原理与过程评价[J].化工进展,2015,34(S1):196-201.
[24]Casas J M,Crisóstomo G,Cifuentes L.Speciation of the Fe(II)-Fe(III)-H2SO4-H2O system at 25and 50℃[J].Hydrometallurgy,2005,80(4):254-264.
[25]Kobylin P,Kaskiala T,Salminen J.Modeling of H2SO4-FeSO4-H2O and H2SO4-Fe2(SO4)3-H2O systems for metallurgical applications[J].Industrial &Engineering Chemistry Research,2007,46(8):2601-2608.
[26]Yue G,Zhao L,Olvera O G,et al.Speciation of the H2SO4-Fe2(SO4)3-FeSO4-H2O system and development of an expression to predict the redox potential of the Fe3+/Fe2+couple up to 150°C[J].Hydrometallurgy,2014,147:196-209.