低碳醇强化铝酸钾溶液晶种分解过程研究
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摘要
铝酸盐溶液的晶种分解工艺是氧化铝生产过程中的关键步骤。针对铝酸钾溶液,考察了60℃下加入水、乙醇、甲醇以及晶种对铝酸钾溶液分解效率和粒度的影响。结果表明,加入乙醇和甲醇均能强化晶种分解过程。加入水后分解率提高至约68%,粒度仅为24.5μm;加入乙醇后分解率可提高至63%,但所得的氢氧化铝晶体粒径约为110μm,产品呈六棱柱状附聚物;加入甲醇后分解率提高到81%,粒度约为90μm,产品呈片状附聚物。同时晶种的加入可明显提高乙醇过程分解率和反应速率,而对甲醇过程的影响不大;在未加晶种的条件下,甲醇的存在会导致新晶型诺三水铝石的产生。
Seeded precipitation of aluminate solution is an important step in alumina production. Effects of water, ethanol, methanol and seeds on precipitation ratio and product particle size in potassium aluminate solution were investigated. The results show that the precipitation ratio increases to approximately 68% by adding water, and the average particle size is ～ 24.5 μm. The precipitation ratio increases to 63% by adding ethanol, but the average particle size is ～ 110 μm. The product aluminum hydroxide had a form of agglomerates of hexagonal prims. The precipitation ratio was improved to 81% by adding methanol and the average particle size was ～ 90 μm with a form of agglomerates of plate-shaped prims. Meanwhile, the seed can improve precipitation ratio and reaction rate of seeded precipitation with ethanol, but it has no significant effect on seeded precipitation with methanol. Methanol leads to the generation of new crystal form of Nordstrandite without seed.
Seeded precipitation of aluminate solution is an important step in alumina production. Effects of water, ethanol, methanol and seeds on precipitation ratio and product particle size in potassium aluminate solution were investigated. The results show that the precipitation ratio increases to approximately 68% by adding water, and the average particle size is ～ 24.5 μm. The precipitation ratio increases to 63% by adding ethanol, but the average particle size is ～ 110 μm. The product aluminum hydroxide had a form of agglomerates of hexagonal prims. The precipitation ratio was improved to 81% by adding methanol and the average particle size was ～ 90 μm with a form of agglomerates of plate-shaped prims. Meanwhile, the seed can improve precipitation ratio and reaction rate of seeded precipitation with ethanol, but it has no significant effect on seeded precipitation with methanol. Methanol leads to the generation of new crystal form of Nordstrandite without seed.
引文
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[17]DU C H,ZHENG S L,ZHANG Y,Phase equilibria in the K2O-Al2O3-H2O system at 40℃[J].Fluid Phase Equilibria,2005,238(2):239-241.
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[19]王雪.铝酸钠甲醇分解制备超细氢氧化铝的基础研究及工艺优化[D].北京:中国科学院过程工程研究所,2007.WANG X.Fundamental research and optimization on the ultrafine aluminum hydroxide preparation process of sodium aluminate by methanol decomposition[D].Beijing:Institute of process engineering,Chinese Academy of Sciences,2007.
[20]张盈,郑诗礼,徐红彬,等.甲醇分解铝酸钠溶液制备大颗粒氢氧化铝的工艺与表征[J].过程工程学报,2009,9(2):300-306.ZHANG Y,ZHENG S L,XU H B,et al.Preparation and characterization of Al(OH)3 coarse particles by decomposition of caustic aluminate solution with methanol[J].The Chinese Journal of Process Engineering,2009,9(2):300-306.
[21]TERO T,MARJALLA L K,SEPPO P.On-line measurement of crystal size distribution during batch crystallization.14th ISIC[C].Cambridge,U.K.1999.
[22]张纲,王静康,熊晖.沉淀结晶过程中的添加晶种技术[J].化学世界,2002,43(6):326-328.ZHANG G,WANG J K,XIONG H.Seeding technology on the precipitation crystallization process[J].Chemical World,2002,43(6):326-328.
[2]顾松青.我国的铝土矿资源和高效低耗的氧化铝生产技术[J].中国有色金属学报,2004(S1):91-97.GU S Q.Alumina production technology with high efficiency and low consumption from Chinese bauxite resource[J].Transactions of Nonferrous Metals Society of China,2004(S1):91-97.
[3]王雪,郑诗礼,张懿.甲醇溶析铝酸钠制备氢氧化铝[J].过程工程学报,2008,8(1):72-77.WANG X,ZHENG S L,ZHANG Y.Preparation of aluminum hydroxide with dissolution of sodium aluminate in methanol-water solvent[J].The Chinese Journal of Process Engineering,2008,8(1):72-77.
[4]姜妲,张帅,曲丽英.铝酸钠溶液晶种分解制备超细氢氧化铝[J].材料与冶金学报,2015,14(1):62-66.JIANG D,ZHANG S,QU L Y.Preparation of superfine aluminum hydroxide by seed precipitation in sodium aluminate solution[J].Journal of Material and Metallurgy,2015,14(1):62-66.
[5]阎丽.铝酸钠溶液晶种分解过程中颗粒行为及其调控[D].长沙:中南大学,2012.YAN L.Behavior and adjustment of particles in seeded precipitation process of sodium aluminate solution[D].Changsha:Central South University,2012.
[6]杨帅帅.铝酸钠溶液晶种分解过程强化与粒子行为研究[D].长沙:中南大学,2013.YANG S S.Studies on enhancing seeded precipitation of sodium aluminate solution and particles behavior in precipitation process[D].Changsha:Central South University,2013.
[7]王丹琴.晶种分解过程中铝酸钠溶液的结构演变[D].长沙:中南大学,2012.WANG D Q.Structure evolution of sodium aluminate solution during the seeded precipitation process[D].Changsha:Central South University,2012.
[8]刘战伟.铝酸钠溶液晶种分解附聚过程及其强化的研究[D].长沙:中南大学,2011.LIU Z W.Study on agglomeration process during gibbsite precipitation from sodium aluminate solution and its enhancement[D].Changsha:Central South University,2011.
[9]LUO M J,LIU C L,XUE J,et al.Leaching kinetics and mechanism of alunite from alunite tailings in highly concentrated KOHsolution[J].Hydrometallurgy,2017,174:10-20.
[10]LUO M J,LIU C L,JIANG Y F,et al.Green recovery of potassium and aluminum elements from alunite tailings using gradient leaching process[J].Journal of Cleaner Production,2017,168:1080-1090.
[11]陈金清,刘吉波,张平民,等.铝酸钠(钾)溶液种分过程的分解率和粒度分布[J].中国有色金属学报,2004,14(3):515-519.CHEN J Q,LIU J B,ZHANG P M,et al.Precipitation rate and particle size distribution of seeded precipitation proceeding in sodium and potassium aluminate solutions[J].Transactions of Nonferrous Metals Society of China,2004,14(3):515-519.
[12]JIANG Y F,LIU C L,XUE J,et al.Insights into the polymorphic transformation mechanism of aluminum hydroxide during carbonation of potassium aluminate solution[J].CrystEngComm,2018,20(10):1431-1442.
[13]孙迎姣,王菊,杜春华,等.铝酸钾溶液碳酸化分解的动力学[J].中国有色金属学报,2017,27(10):2164-2169.SUN Y J,WANG J,DU C H,et al.Kinetics of carbonation decomposition of potassium aluminate solution[J].Transactions of Nonferrous Metals Society of China,2017,27(10):2164-2169.
[14]尹周澜,曾纪术,陈启元.晶种活化强化铝酸钠溶液的种分分解[J].中国有色金属学报,2008,18(2):361-365.YIN Z L,ZENG J S,CHEN Q Y.Decomposition enhancement of seeded sodium aluminate liquor by activated seed[J].Transactions of Nonferrous Metals Society of China,2008,18(2):361-365.
[15]ZHANG Y,ZHENG S L,DU H,et al.Improved precipitation of gibbsite from sodium aluminate solution by adding methanol[J].Hydrometallurgy,2009,98(1-2):38-44.
[16]刘光启,马连湘,刘杰.化学化工物性数据手册:无机卷[M].北京:化学工业出版社,2002:297-298.LIU G Q,MA L X,LIU J.Handbook of chemistry and chemical engineering properties data:inorganic volume[M].Beijing:Chemical Industry Press,2002:297-298.
[17]DU C H,ZHENG S L,ZHANG Y,Phase equilibria in the K2O-Al2O3-H2O system at 40℃[J].Fluid Phase Equilibria,2005,238(2):239-241.
[18]吴晓华,陈滨,李小斌,等.表面活性剂强化铝酸钠溶液晶种分解的研究进展[J].江西有色金属,2006,20(2):13-19.WU X H,CHEN B,LI X B,et al.Research development of intensifying the process of seeded precipitation from caustic aluminate solutions with surfactants[J].Jiangxi Nonferrous Metals,2006,20(2):13-19.
[19]王雪.铝酸钠甲醇分解制备超细氢氧化铝的基础研究及工艺优化[D].北京:中国科学院过程工程研究所,2007.WANG X.Fundamental research and optimization on the ultrafine aluminum hydroxide preparation process of sodium aluminate by methanol decomposition[D].Beijing:Institute of process engineering,Chinese Academy of Sciences,2007.
[20]张盈,郑诗礼,徐红彬,等.甲醇分解铝酸钠溶液制备大颗粒氢氧化铝的工艺与表征[J].过程工程学报,2009,9(2):300-306.ZHANG Y,ZHENG S L,XU H B,et al.Preparation and characterization of Al(OH)3 coarse particles by decomposition of caustic aluminate solution with methanol[J].The Chinese Journal of Process Engineering,2009,9(2):300-306.
[21]TERO T,MARJALLA L K,SEPPO P.On-line measurement of crystal size distribution during batch crystallization.14th ISIC[C].Cambridge,U.K.1999.
[22]张纲,王静康,熊晖.沉淀结晶过程中的添加晶种技术[J].化学世界,2002,43(6):326-328.ZHANG G,WANG J K,XIONG H.Seeding technology on the precipitation crystallization process[J].Chemical World,2002,43(6):326-328.