添加混合晶种强化铝酸钠溶液的晶种分解过程（英文）
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摘要
本文报道了工业晶种和自制活性晶种组成的混合晶种强化铝酸钠溶液中三水铝石结晶析出的工艺,并初步研究了其强化机理。对比研究了活性晶种/铝酸钠溶液、工业晶种/铝酸钠溶液的界面性质。分别采用坐滴法和BET法测定了晶种/铝酸钠溶液接触角及晶种比表面积;采用激光衍射法和SEM分别测定了种分产品的粒度分布及形貌。研究结果表明,相对于工业晶种,活性晶种的润湿性能更好、比表面积更大以及晶种/铝酸钠溶液界面张力更低,这些性质均利于加速铝酸钠溶液中氢氧化铝在晶种/铝酸钠溶液界面的析出。结晶产物的SEM分析表明,细小颗粒会嵌入、堆积及附聚到粗粒度工业晶种表面,从而可有效地控制结晶产物中的细颗粒含量。额外加入3.1～4.6 g/L活性晶种,种分分解率可提高3.23%～3.92%,且种分产物中<45μm颗粒含量比工业晶种及传统种分产物的均略有减少。研究结果有利于为氧化铝工业生产开发一种新的铝酸钠溶液晶种分解过程强化工艺。
Gibbsite precipitation from sodium aluminate solution was intensified by adding mixed industrial and self-prepared active seeds, and its mechanism was researched preliminarily. The interfacial properties of seed/aluminate solution were determined for separate industrial and active seed. Contact angles of seed/aluminate solution and the specific surface area of seeds were respectively measured by sessile drop and BET method, and the morphology and particle size of precipitates were recorded by SEM and laser diffraction. The results show that, compared with the industrial seed, the active seed has a better wettability, lower interfacial tension, and larger specific surface area, being conducive to enhancing gibbsite precipitation from sodium aluminate solution. SEM analysis of the precipitates indicates that the embedment and accumulation/agglomeration of extremely fine particles on the surface of coarse industrial seed can effectively control the content of fine particles in the precipitation product. With extra 3.1–4.6 g/L active seed, the gibbsite precipitation ratio was increased by 3.23%–3.92%. Moreover, the mass percentage of particles<45 μm in precipitation product has even a slight decrease compared with that for the traditional precipitation product or of the industrial seed itself. The result presented is favorable to developing an intensified gibbsite precipitation process for commercial alumina manufacture.
Gibbsite precipitation from sodium aluminate solution was intensified by adding mixed industrial and self-prepared active seeds, and its mechanism was researched preliminarily. The interfacial properties of seed/aluminate solution were determined for separate industrial and active seed. Contact angles of seed/aluminate solution and the specific surface area of seeds were respectively measured by sessile drop and BET method, and the morphology and particle size of precipitates were recorded by SEM and laser diffraction. The results show that, compared with the industrial seed, the active seed has a better wettability, lower interfacial tension, and larger specific surface area, being conducive to enhancing gibbsite precipitation from sodium aluminate solution. SEM analysis of the precipitates indicates that the embedment and accumulation/agglomeration of extremely fine particles on the surface of coarse industrial seed can effectively control the content of fine particles in the precipitation product. With extra 3.1–4.6 g/L active seed, the gibbsite precipitation ratio was increased by 3.23%–3.92%. Moreover, the mass percentage of particles<45 μm in precipitation product has even a slight decrease compared with that for the traditional precipitation product or of the industrial seed itself. The result presented is favorable to developing an intensified gibbsite precipitation process for commercial alumina manufacture.
引文
[1]XUE Sheng-guo,YE Yu-zhen,ZHU Feng,WANG Qiong-li,JIANG Jun,WILLIAM H.Changes in distribution and microstructure of bauxite residue aggregates following amendments addition[J].Journal of Environmental Sciences,2019,78:276-286.DOI:10.1016/j.jes.2018.10.010.
[2]XUE Sheng-guo,WU Yu-jun,LI Yi-wei,KONG Xiang-feng,ZHU Feng,WILLIAM H,LI Xiao-fei,YE Yu-zhen.Industrial wastes applications for alkalinity regulation in bauxite residue:A comprehensive review[J].Journal of Central South University,2019,26(2):268-288.DOI:https://doi.org/1031007/s11771-019-4000-3.
[3]LI Xiao-bin,ZHAO Dong-feng,WANG Dan-qin,YAN Li.Research progress in theory and technology of gibbsite precipitation from sodium aluminate solution[J].The Chinese Journal of Nonferrous Metals,2011,21(10):2577-2593.(in Chinese)
[4]LI Xiao-bin,WANG Dan-qin,ZHOU Qiu-sheng,LIUGui-hua,PENG Zhi-hong.Influence of magnetic field on the seeded precipitation of gibbsite from sodium aluminate solution[J].Minerals Engineering,2012,32(3):12-18.DOI:10.1016/j.mineng.2012.02.015.
[5]ZHANG Bin,LI Jie,CHEN Qi-yuan,CHEN Guo-hui.Precipitation of Al(OH)3 crystals from supersaturated sodium aluminate solution irradiated with ultrasonic sound[J].Minerals Engineering,2009,22(9,10):853-858.DOI:10.1016/j.mineng.2009.03.008.
[6]CHEN Nian-yi,LU Wen-cong,ZHANG Liang-miao,GUSong-qin,QI Li-juan,BAI Wan-quan.Liquid-liquid extraction modified Bayer process and its physic-chemical basis[J].Journal of the Chinese Rare Earth Society,2006,24(special issue):78-81.(in Chinese)
[7]LI Yuan-gao,CHEN Qi-yuan,WANG Song-sen,YINZhou-lan,ZHANG Ping-min.Preparation of Al(OH)3 by ion membrane electrolysis and precipitation of sodium aluminate solution with seeds[J].The Chinese Journal of Nonferrous Metals,2008,18(4):974-979.DOI:10.1016/S1003-6326(08)60168-5.(in Chinese)
[8]WILHELMY R B.Control of form of crystal precipitation of aluminum hydroxide using cosolvents and varying caustic concentration:United States,4900537[P].1990-02-13.
[9]ZHANG Ying,ZHENG Shi-li,DU Hao,XU Hong-bin,WANG Shao-na,ZHANG Yi.Improved precipitation of gibbsite from sodium aluminate solution by adding methanol[J].Hydrometallurgy,2009,98(1,2):38-44.DOI:10.1016/j.hydromet.2009.03.014.
[10]LIU Gui-hua,WU Guo-yu,CHEN Wei,LI Xiao-bin,PENGZhi-hong,ZHOU Qiu-sheng,QI Tian-gui.Increasing precipitation rate from sodium aluminate solution by adding active seed and ammonia[J].Hydrometallurgy,2018,176:253-259.DOI:10.1016/j.hydromet.2018.02.003.
[11]ZENG Ji-shu,YIN Zhou-lan,CHEN Qi-yuan.Effect of tetracarbon additives on gibbsite precipitation from seeded sodium aluminate liquor[J].Journal of Central South University,2008,15(5):622-626.DOI:10.1007/s11771-008-0116-6.
[12]LI Xiao-bin,YAN Li,ZHOU Qiu-sheng,PENG Zhi-hong,LIU Gui-hua.Effect of ethers additive B35 on seeded precipitation of sodium aluminate solution[J].The Chinese Journal of Nonferrous Metals,2011,21(2):459-464.(in Chinese)
[13]BROWN N.Effect of calcium ions on agglomeration of bayer aluminium trihydroxide[J].Journal of Crystal Growth,1988,92(1):26-32.DOI:10.1016/0022-0248(88)90429-0.
[14]GNYRA N,BROWN N.The coarsening of Bayer alumina trihydrate by means of crystallization modifiers[J].Powder Technology,1975,11(2):101-105.DOI:10.1016/0032-5910(75)80035-0.
[15]TIAN Lv.Study on preparation of high whiteness aluminum trihydroxide powder from high concentration sodium aluminate solution by seeded precipitation[D].Changsha:Central South University,2012.(in Chinese)
[16]PRADHAN J K,GOCHHAYAT P K,BHATTACHARYA I N,DAS S C.Study on the various factors affecting the quality of precipitated non-metallurgical alumina trihydrate particles[J].Hydrometallurgy,2001,60(2):143-153.DOI:10.1016/S0304-386X(00)00196-1.
[17]XIE Yan-li,BI Shi-wen,YANG Yi-hong,WANG Zhi.Surface acidity of Al(OH)3 seed and its effect on precipitation of sodium aluminate liquors[J].The Chinese Journal of Nonferrous Metals,2000,10(6):896-898.(in Chinese)
[18]YIN Jian-guo.Intensifying the seeded agglomeration process of supersaturated sodium aluminate liquors[D].Changsha:Central South University,2007.(in Chinese)
[19]ZENG Ji-shu,YIN Zhou-lan,CHEN Qi-yuan.Intensification of precipitation of gibbsite from seeded caustic sodium aluminate liquor by seed activation and addition of crown ether[J].Hydrometallurgy,2007,89(1):107-116.DOI:10.1016/j.hydromet.2007.07.001.
[20]ZHANG Xuan.Particle size control of products from precipitation process with seeds prepared by inducing nucleation in sodium aluminate solution[D].Changsha:Central South University,2011.(in Chinese)
[21]LIU Giu-hua,LI Zheng,QI Tian-gui,LI Xiao-bin,ZHOUQiu-sheng,PENG Zhi-hong.Two-stage process for precipitating coarse boehmite from sodium aluminate solution[J].JOM,2017,69(10):1888-1893.DOI:10.1007/s11837-017-2468-6.
[22]ADDAI-MENSAH J,RALSTON J.The influence of interfacial structuring on gibbsite interactions in synthetic Bayer liquors[J].Journal of Colloid and Interface Science,1999,215(1):124-130.DOI:10.1006/jcis.1999.6237.
[23]ADDAI-MENSAH J,PRESTIGE C A,RALSTON J.Interparticle forces,interfacial structure development and agglomeration of gibbsite particles in synthetic Bayer liquors[J].Minerals Engineering,1999,12:655-669.DOI:10.1016/S0892-6875(99)00050-3.
[24]WATTS H L,UTLEY D W.Volumetric analysis of sodium aluminate solutions[J].Analytical Chemistry,1953,25(6):864-867.DOI:10.1021/ac60078a005.
[25]YANG Chong-yu.Technology of alumina production[M].Beijing:Metallurgical Industry Press,2011:53.(in Chinese)
[26]OWENS D K,WENDT R C.Estimation of the surface free energy of polymers[J].Journal of Applied Polymer Science,1969,13(8):1741-1747.DOI:10.1002/app.1969.070130815.
[27]LUNER P E,OH E.Characterization of the surface free energy of cellulose ether films[J].Colloids&Surfaces A:Physicochemical&Engineering Aspects,2001,181(1-3):31-48.DOI:10.1016/S0927-7757(00)00805-0.
[28]LI Xiao-bin,XU Xiang-ming,ZHOU Qiu-sheng,QITian-gui,LIU Gui-hua,PENG Zhi-hong,CUI Yuan-fa,LIJian-pu.Ca3WO6 prepared by roasting tungsten-containing materials and its leaching performance[J].International Journal of Refractory Metals&Hard Materials,2015,52:151-158.DOI:10.1016/j.ijrmhm.2015.06.003.
[29]ADAMSON A W,GAST A P.Physical chemistry of surfaces[M].New York:Wiley,1997:353.
[30]ZHU Ding-yi,DAI Pin-qiang,LUO Xiao-bin,ZHANGYuan-chao.Novel characterization of wetting properties and the calculation of liquid-solid interface tension(I)[J].Science Technology and Engineering,2007,7(13):3057-3062.(in Chinese)
[31]ZHU Ding-yi,ZHANG Yuan-chao,DAI Pin-qiang,LUOXiao-bin.Novel characterization of wetting properties and the calculation of liquid-solid interface tension(II)[J].Science Technology and Engineering,2007,7(13):3063-3069.(in Chinese)
[32]LI Xiao-bin,YAN Li,ZHAO Dong-feng,ZHOU Qiu-sheng,LIU Gui-hua,PENG Zhi-hong,YANG Shuai-shuai,QITian-gui.Relationship between Al(OH)3 solubility and particle size in synthetic Bayer liquors[J].Transactions of Nonferrous Metals Society of China,2013,23(5):1472-1479.DOI:10.1016/S1003-6326(13)62619-9.
[33]WANG Jian-li,CHEN Qi-yuan,LI Wang-xing,YINZhou-lan.Kinetics of super-fine aluminum hydroxide precipitation from sodium aluminate solutions with gel-seed[C]//Light Metals.San Francisco,California:TMS,2009:177-182.
[34]BHATTACHARYA I N,PRADHAN J K,GOCHHAYATP K,DAS S C.Factors controlling precipitation of finer size alumina trihydrate[J].International Journal of Mineral Processing,2002,65(2):109-124.DOI:10.1016/S0301-7516(01)00084-9.
[2]XUE Sheng-guo,WU Yu-jun,LI Yi-wei,KONG Xiang-feng,ZHU Feng,WILLIAM H,LI Xiao-fei,YE Yu-zhen.Industrial wastes applications for alkalinity regulation in bauxite residue:A comprehensive review[J].Journal of Central South University,2019,26(2):268-288.DOI:https://doi.org/1031007/s11771-019-4000-3.
[3]LI Xiao-bin,ZHAO Dong-feng,WANG Dan-qin,YAN Li.Research progress in theory and technology of gibbsite precipitation from sodium aluminate solution[J].The Chinese Journal of Nonferrous Metals,2011,21(10):2577-2593.(in Chinese)
[4]LI Xiao-bin,WANG Dan-qin,ZHOU Qiu-sheng,LIUGui-hua,PENG Zhi-hong.Influence of magnetic field on the seeded precipitation of gibbsite from sodium aluminate solution[J].Minerals Engineering,2012,32(3):12-18.DOI:10.1016/j.mineng.2012.02.015.
[5]ZHANG Bin,LI Jie,CHEN Qi-yuan,CHEN Guo-hui.Precipitation of Al(OH)3 crystals from supersaturated sodium aluminate solution irradiated with ultrasonic sound[J].Minerals Engineering,2009,22(9,10):853-858.DOI:10.1016/j.mineng.2009.03.008.
[6]CHEN Nian-yi,LU Wen-cong,ZHANG Liang-miao,GUSong-qin,QI Li-juan,BAI Wan-quan.Liquid-liquid extraction modified Bayer process and its physic-chemical basis[J].Journal of the Chinese Rare Earth Society,2006,24(special issue):78-81.(in Chinese)
[7]LI Yuan-gao,CHEN Qi-yuan,WANG Song-sen,YINZhou-lan,ZHANG Ping-min.Preparation of Al(OH)3 by ion membrane electrolysis and precipitation of sodium aluminate solution with seeds[J].The Chinese Journal of Nonferrous Metals,2008,18(4):974-979.DOI:10.1016/S1003-6326(08)60168-5.(in Chinese)
[8]WILHELMY R B.Control of form of crystal precipitation of aluminum hydroxide using cosolvents and varying caustic concentration:United States,4900537[P].1990-02-13.
[9]ZHANG Ying,ZHENG Shi-li,DU Hao,XU Hong-bin,WANG Shao-na,ZHANG Yi.Improved precipitation of gibbsite from sodium aluminate solution by adding methanol[J].Hydrometallurgy,2009,98(1,2):38-44.DOI:10.1016/j.hydromet.2009.03.014.
[10]LIU Gui-hua,WU Guo-yu,CHEN Wei,LI Xiao-bin,PENGZhi-hong,ZHOU Qiu-sheng,QI Tian-gui.Increasing precipitation rate from sodium aluminate solution by adding active seed and ammonia[J].Hydrometallurgy,2018,176:253-259.DOI:10.1016/j.hydromet.2018.02.003.
[11]ZENG Ji-shu,YIN Zhou-lan,CHEN Qi-yuan.Effect of tetracarbon additives on gibbsite precipitation from seeded sodium aluminate liquor[J].Journal of Central South University,2008,15(5):622-626.DOI:10.1007/s11771-008-0116-6.
[12]LI Xiao-bin,YAN Li,ZHOU Qiu-sheng,PENG Zhi-hong,LIU Gui-hua.Effect of ethers additive B35 on seeded precipitation of sodium aluminate solution[J].The Chinese Journal of Nonferrous Metals,2011,21(2):459-464.(in Chinese)
[13]BROWN N.Effect of calcium ions on agglomeration of bayer aluminium trihydroxide[J].Journal of Crystal Growth,1988,92(1):26-32.DOI:10.1016/0022-0248(88)90429-0.
[14]GNYRA N,BROWN N.The coarsening of Bayer alumina trihydrate by means of crystallization modifiers[J].Powder Technology,1975,11(2):101-105.DOI:10.1016/0032-5910(75)80035-0.
[15]TIAN Lv.Study on preparation of high whiteness aluminum trihydroxide powder from high concentration sodium aluminate solution by seeded precipitation[D].Changsha:Central South University,2012.(in Chinese)
[16]PRADHAN J K,GOCHHAYAT P K,BHATTACHARYA I N,DAS S C.Study on the various factors affecting the quality of precipitated non-metallurgical alumina trihydrate particles[J].Hydrometallurgy,2001,60(2):143-153.DOI:10.1016/S0304-386X(00)00196-1.
[17]XIE Yan-li,BI Shi-wen,YANG Yi-hong,WANG Zhi.Surface acidity of Al(OH)3 seed and its effect on precipitation of sodium aluminate liquors[J].The Chinese Journal of Nonferrous Metals,2000,10(6):896-898.(in Chinese)
[18]YIN Jian-guo.Intensifying the seeded agglomeration process of supersaturated sodium aluminate liquors[D].Changsha:Central South University,2007.(in Chinese)
[19]ZENG Ji-shu,YIN Zhou-lan,CHEN Qi-yuan.Intensification of precipitation of gibbsite from seeded caustic sodium aluminate liquor by seed activation and addition of crown ether[J].Hydrometallurgy,2007,89(1):107-116.DOI:10.1016/j.hydromet.2007.07.001.
[20]ZHANG Xuan.Particle size control of products from precipitation process with seeds prepared by inducing nucleation in sodium aluminate solution[D].Changsha:Central South University,2011.(in Chinese)
[21]LIU Giu-hua,LI Zheng,QI Tian-gui,LI Xiao-bin,ZHOUQiu-sheng,PENG Zhi-hong.Two-stage process for precipitating coarse boehmite from sodium aluminate solution[J].JOM,2017,69(10):1888-1893.DOI:10.1007/s11837-017-2468-6.
[22]ADDAI-MENSAH J,RALSTON J.The influence of interfacial structuring on gibbsite interactions in synthetic Bayer liquors[J].Journal of Colloid and Interface Science,1999,215(1):124-130.DOI:10.1006/jcis.1999.6237.
[23]ADDAI-MENSAH J,PRESTIGE C A,RALSTON J.Interparticle forces,interfacial structure development and agglomeration of gibbsite particles in synthetic Bayer liquors[J].Minerals Engineering,1999,12:655-669.DOI:10.1016/S0892-6875(99)00050-3.
[24]WATTS H L,UTLEY D W.Volumetric analysis of sodium aluminate solutions[J].Analytical Chemistry,1953,25(6):864-867.DOI:10.1021/ac60078a005.
[25]YANG Chong-yu.Technology of alumina production[M].Beijing:Metallurgical Industry Press,2011:53.(in Chinese)
[26]OWENS D K,WENDT R C.Estimation of the surface free energy of polymers[J].Journal of Applied Polymer Science,1969,13(8):1741-1747.DOI:10.1002/app.1969.070130815.
[27]LUNER P E,OH E.Characterization of the surface free energy of cellulose ether films[J].Colloids&Surfaces A:Physicochemical&Engineering Aspects,2001,181(1-3):31-48.DOI:10.1016/S0927-7757(00)00805-0.
[28]LI Xiao-bin,XU Xiang-ming,ZHOU Qiu-sheng,QITian-gui,LIU Gui-hua,PENG Zhi-hong,CUI Yuan-fa,LIJian-pu.Ca3WO6 prepared by roasting tungsten-containing materials and its leaching performance[J].International Journal of Refractory Metals&Hard Materials,2015,52:151-158.DOI:10.1016/j.ijrmhm.2015.06.003.
[29]ADAMSON A W,GAST A P.Physical chemistry of surfaces[M].New York:Wiley,1997:353.
[30]ZHU Ding-yi,DAI Pin-qiang,LUO Xiao-bin,ZHANGYuan-chao.Novel characterization of wetting properties and the calculation of liquid-solid interface tension(I)[J].Science Technology and Engineering,2007,7(13):3057-3062.(in Chinese)
[31]ZHU Ding-yi,ZHANG Yuan-chao,DAI Pin-qiang,LUOXiao-bin.Novel characterization of wetting properties and the calculation of liquid-solid interface tension(II)[J].Science Technology and Engineering,2007,7(13):3063-3069.(in Chinese)
[32]LI Xiao-bin,YAN Li,ZHAO Dong-feng,ZHOU Qiu-sheng,LIU Gui-hua,PENG Zhi-hong,YANG Shuai-shuai,QITian-gui.Relationship between Al(OH)3 solubility and particle size in synthetic Bayer liquors[J].Transactions of Nonferrous Metals Society of China,2013,23(5):1472-1479.DOI:10.1016/S1003-6326(13)62619-9.
[33]WANG Jian-li,CHEN Qi-yuan,LI Wang-xing,YINZhou-lan.Kinetics of super-fine aluminum hydroxide precipitation from sodium aluminate solutions with gel-seed[C]//Light Metals.San Francisco,California:TMS,2009:177-182.
[34]BHATTACHARYA I N,PRADHAN J K,GOCHHAYATP K,DAS S C.Factors controlling precipitation of finer size alumina trihydrate[J].International Journal of Mineral Processing,2002,65(2):109-124.DOI:10.1016/S0301-7516(01)00084-9.