EDTA络合-球磨法制备超细棒状BaSO_4
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摘要
采用EDTA络合-球磨法在室温下制备超细沉淀BaSO_4,研究了工艺参数对BaSO_4粒度分布和形貌的影响。通过XRD、SEM、激光粒度分布仪和FTIR等分析手段对产物的晶相、形貌和粒度进行表征,并探讨了反应机理。结果表明:BaCO_3浓度、EDTA的添加量和反应时间对BaSO_4的粒径影响较大,Na_2SO_4的添加速度对粒度影响相对较小。随着反应体系pH增大,BaSO_4颗粒形貌由不规整的针状逐渐转变为竖直排列的棒状团簇体,并且颗粒边缘趋于光滑。在BaCO_3浓度为0.2 mol·L~(-1),BaCO_3、EDTA、Na_2SO_4摩尔质量比为1:0.5:1.2,反应体系pH=8时可以得到平均粒径为130 nm均匀分散的棒状团簇体沉淀BaSO_4微粒。
Ultrafine precipitated barium sulfate was synthesized by wet ball milling in the presence of EDTA at room temperature. Effects of preparation parameters on BaSO_4 size distribution and morphology were investigated. XRD, SEM, FTIR and laser particle size analyzer were used to characterize crystalline,morphology and particle size of BaSO_4 particles. Furthermore, the reaction mechanism was discussed. The results show that BaCO_3 concentration, EDTA amount and reaction time have obvious effects on BaSO_4 particle size. However, feeding rate of Na_2SO_4 has few effects on BaSO_4 size distribution. The morphology of BaSO_4 particles changes from needle-like to vertical arrangement of rod-like clusters with pH increase, and particle edge becomes smooth. The well-dispersed rod clusters with average size of 130 nm are synthesized at c(BaCO_3)= 0.2 mol·L~(-1), x(BaCO_3):x(EDTA):x(Na_2SO_4) = 1:0.5:1.2 and pH = 8.
Ultrafine precipitated barium sulfate was synthesized by wet ball milling in the presence of EDTA at room temperature. Effects of preparation parameters on BaSO_4 size distribution and morphology were investigated. XRD, SEM, FTIR and laser particle size analyzer were used to characterize crystalline,morphology and particle size of BaSO_4 particles. Furthermore, the reaction mechanism was discussed. The results show that BaCO_3 concentration, EDTA amount and reaction time have obvious effects on BaSO_4 particle size. However, feeding rate of Na_2SO_4 has few effects on BaSO_4 size distribution. The morphology of BaSO_4 particles changes from needle-like to vertical arrangement of rod-like clusters with pH increase, and particle edge becomes smooth. The well-dispersed rod clusters with average size of 130 nm are synthesized at c(BaCO_3)= 0.2 mol·L~(-1), x(BaCO_3):x(EDTA):x(Na_2SO_4) = 1:0.5:1.2 and pH = 8.
引文
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[2]SUN Y Y,ZHANG F,WU D X,et al.Roles of polyacrylate dispersant in the synthesis of well-dispersed BaSO4 nanoparticles by simple precipitation[J].Particuology,2014,14(3):33-37.
[3]王晓辉,蒋斌波,陈纪忠.溶析结晶法制备高纯度亚微米硫酸钡粒子[J].无机材料学报,2005,20(4):801-807.WANG X H,JIANG B B,CHEN J Z.Preparation of barium sulfate submicro-particals with high purity by solvening-out process[J].Journal of Inorganic Materials,2005,20(4):801-807.
[4]NANDAKUMAR N,KURIAN P.Chemosynthesis of monodispersed porous BaSO4 nano powder by polymeric template process and its characterisation[J].Powder Technology,2012,224:51-56.
[5]WONG D C Y,JAWORSKI Z,NIENOW A W.Effect of ion excess on particle size and morphology during barium sulphate precipitation:An experimental study[J].Chemical Engineering Science,2001,56(3):727-734.
[6]CHEN Q,SHEN X.Formation of mesoporous BaSO4 microspheres with a larger pore size via Ostwald pipening at room temperature[J].Crystal Growth&Design,2010,10(9):3838-3842.
[7]HU L,WANG G,YANG C,et al.Fabrication of submicron barium sulfate aggregates in the presence of ethylenediaminetetraacetic acid anions[J].Particuology,2015,22(5):157-162.
[8]ZHAO Y H,LIU J R.Effect of EDTA and phosphate on particle size during precipitation of nanosized baso4 particles[J].Chemistry Letters,2006,35(9):1040-1041.
[9]赵华,刘洪杰,朱建伟,等.微反应器制备纳米BaSO4研究[J].无机盐工业,2008,40(1):29-31.ZHAO H,LIU H J,ZHU J W,et al.Preparation of nano-sized barium sulfate by micro-reactor[J].Inorganic Chemicals Industry,2008,40(1):29-31.
[10]NIEMANN B,KAI S.Reduced discrete population balance model for precipitation of barium sulfate nanoparticles in non-ionic microemulsions[J].Chemical Engineering Journal,2008,143(1-3):314-325.
[11]HU L,WANG G,CAO R,et al.Fabrication and surface properties of hydrophobic barium sulfate aggregates based on sodium cocoate modification[J].Applied Surface Science,2014,315(1):184-189.
[12]LI J,LIU D,JIANG H,et al.Effects of polyacrylic acid additive on barium sulfate particle morphology[J].Materials Chemistry&Physics,2016,175:180-187.
[13]JONES F,JONES P,OGDEN M I,et al.The interaction of EDTA with barium sulfate[J].Journal of Colloid&Interface Science,2007,316(2):553-561.
[14]ZHANG M,ZHANG B,LI X,et al.Synthesis and surface properties of submicron barium sulfate particles[J].Applied Surface Science,2011,258(1):24-29.
[15]黄洁芳,刘俊康.粒度及分布可控的亚微米级硫酸钡的制备研究[J].应用化工,2015,44(3):423-427.HUANG J F,LIU J K.Synthesis of sub-micron grade barium sulfate with controllable particle size and distribution[J].Applied Chemical Industry,2015,44(3):423-427.
[16]WANG S,LIU R,YAO J,et al.Fabrication of mesoporous magnesium substitutedβ-tricalcium phosphate nanospheres by self-transformation and assembly involving EDTA ions[J].Microporous&Mesoporous Materials,2013,179(4):172-181.
[17]RENZO F D.Zeolites as tailor-made catalysts:Control of the crystal size[J].Catalysis Today 1998,41(1-3):37-40.
[18]林晓,李新海,周湘君,等.络合法制备纳米BaSO4及其影响因素的分析[J].广东微量元素科学,2010,17(4):25-32.LIN X,LI X H,ZHOU X J,et al.Preparation of nanobarium sulfate complexation and analysis of its impact factors[J].Guangdong Trace Elements Science,2010,17(4):25-32.
[19]张明,李新海,胡启阳,等.EDTA络合法合成硫酸钡微粒[J].中国有色金属学报,2009,19(8):1511-1516.ZHANG M,LI X H,HU Q Y,et al.Synthesis of barium sulfate particles by complexation method in presence of EDTA[J].The Chinese Journal of Nonferrous Metals,2009,19(8):1511-1516.
[20]BALA H,FU W Y,ZHAO J Z,et al.Preparation of BaSO4 nanoparticles with self-dispersing properties[J].Colloids and Surfaces,2005,252:129-134.
[21]NAKAMOTO K.Infrared and ramanspectra of inorganic and coordination compounds,parts A and B[J].Theory&Applications in Inorganic Chemistry,1963,p(5):88-97.