沉淀法制备低维纳米AlO(OH)的工艺条件研究
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摘要
在不同工艺条件下采用沉淀法制备了低维纳米AlO(OH),并对样品进行了XRD、FT-IR及SEM表征分析。结果表明,pH值较低和较高时,样品的结晶度均较低。反应温度为75℃和95℃时,样品的结晶度均较好,无杂质。当pH值为9.0、反应温度为85℃时,样品中存在大量缔合-OH,AlO(OH)结晶度较好,且有少量Al(OH)3晶体存在。由于SDBS在Al(OH)3颗粒表面形成完整胶束,且有空间位阻效应,此时形成的样品为5nm厚、长宽可达100~300nm的边缘卷曲的蓬松片状物,形貌规则、尺寸均匀、分散性较好。
A series of low-dimensional nanoscale AlO(OH)were prepared by precipitation method under diverse technological conditions,and were characterized by XRD,FT-IR and SEM.The results showed that the crystallinities of the samples were lower both at high and low pH values.While the reaction temperature was 75℃ or 95℃,the products exhibited higher crystallinities and contained no impurity.At pH value of 9.0,reaction temperature of 85℃,the sample had a lot of associate-OH,and high crystallinity AlO(OH)with a little Al(OH)3crystal.Because of the complete micelles of SDBS formed on the surface of Al(OH)3particles and their space location-obstruct effect,the sample showed curly fluffy flake with thickness of 5nm and width of 100-300 nm,regular shape,uniform size and good dispersion.
A series of low-dimensional nanoscale AlO(OH)were prepared by precipitation method under diverse technological conditions,and were characterized by XRD,FT-IR and SEM.The results showed that the crystallinities of the samples were lower both at high and low pH values.While the reaction temperature was 75℃ or 95℃,the products exhibited higher crystallinities and contained no impurity.At pH value of 9.0,reaction temperature of 85℃,the sample had a lot of associate-OH,and high crystallinity AlO(OH)with a little Al(OH)3crystal.Because of the complete micelles of SDBS formed on the surface of Al(OH)3particles and their space location-obstruct effect,the sample showed curly fluffy flake with thickness of 5nm and width of 100-300 nm,regular shape,uniform size and good dispersion.
引文
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15 Wang Yinhu,Fan Guangyin,Zhang Chun,et al.High active and selective hydrogenation of p-chloronitrobenzene over Ir/AlO(OH)[J].Appl Chem Ind,2013,42(3):397(in Chinese)王银虎,樊光银,张春,等.Ir/AlO(OH)催化剂对氯代硝基苯催化加氢反应的研究[J].应用化工,2013,42(3):397
16 Chen Wei.Study on the microstructure evolution ofα-Al2O3in the formation process and it′s controlling[D].Changsha:Central South University,2010(in Chinese)陈伟.α-Al2O3形成过程显微结构演变及其调控[D].长沙:中南大学,2010
17 Lu Shaoyuan,He Yunqiu.Application of surfactant to synthesis of nano-alumina[J].Mater Rev,2006,20(6):149(in Chinese)卢少元,贺蕴秋.表面活性剂在纳米氧化铝制备中的应用研究[J].材料导报,2006,20(6):149
2 Xu Z,Yu J,Jaroniec M.Efficient catalytic removal of formaldehyde at room temperature using AlOOH nanoflakes with deposited Pt[J].Appl Catal B:Environ,2015,163:306
3 Motta A,Gaigeot M P,Costa D.AIMD evidence of inner sphere adsorption of glycine on a stepped(101)boehmite AlOOH surface[J].J Phys Chem C,2012,116(44):25418
4 Gao C,Yu X Y,Xu R X,et al.AlOOH-reduced graphene oxide nanocomposites:One-pot hydrothermal synthesis and their enhanced electrochemical activity for heavy metal ions[J].ACS Appl Mater Interf,2012,4(9):4672
5 Miao Y E,Wang R,Chan D,et al.Electrospun self-standing membrane of hierarchical SiO2γ-AlOOH(Boehmite)core/sheath fibers for water remediation[J].ACS Appl Mater Interf,2012,4(10):5353
6 Peng Weiguo,Zhou Jicheng,Xie Fanghua,et al.Preparation of nano fibrousγ-Al2O3 with large pore volume by high gravitational reactive carbonation in rotating bed with helix channels[J].Mater Rev,2007,21(S1):41(in Chinese)彭卫国,周继承,谢放华,等.螺旋通道型旋转床碳分法制备大孔容纳米拟薄水铝石[J].材料导报,2007,21(专辑Ⅷ):41
7 Demichelis R,Noel Y,Civalleri B,et al.The vibrational spectrum ofα-AlOOH diaspore:An Ab initio study with the CRYSTAL code[J].J Phys Chem B,2007,111(31):9337
8 Yang Qi,Hu Wenbin.Thermal decomposition kinetics ofγ-AlOOH nanocrystalline prepared by hydrothermal method[J].J Inorg Mater,2010,25(1):96(in Chinese)杨琪,胡文彬.水热合成的纳米γ-AlOOH的热分解动力学[J].无机材料学报,2010,25(1):96
9 Zhang L,Jiao X L,Chen D R,et al.γ-AlOOH nanomaterials with regular shapes:Hydrothermal fabrication and Cr2O72-adsorption[J].Eur J Inorg Chem,2011,34:5258
10 Feng Y L,Lu W C,Zhang L M,et al.One-step synthesis of hierarchical cantaloupe-like AlOOH superstructures via a hydrothermal route[J].Cryst Growth Des,2008,8(4):1426
11 Liu Changhua,Liao Haida,Long Xiangyun.Transformation of crystillion AlOOH prepared by sol-gel and hydrothermal treatment[J].J South-Central University Nationalities:Nat Sci Ed,2004,23(1):18(in Chinese)刘昌华,廖海达,龙翔云.Sol-Gel水热偶合法制备纳米AlOOH的晶相转变[J].中南民族大学学报:自然科学版,2004,23(1):18
12 Li Yuping,He Weiwei,Chen Zhiqiao,et al.Preparation and characterization of fibrous pseudoboehmite nano-particles with low bulk density[J].Petroleum Process Petrochem,2006,37(7):25(in Chinese)李玉平,贺卫卫,陈智巧,等.低堆密度拟薄水铝石纳米纤维粒子的制备与表征[J].石油炼制与化工,2006,37(7):25
13 Qin Zhiyang,Qin Linqing,Zhang Lianmeng,et al.Study on the thermal decomposition of basic magnesium carbonate by XRD,TG,DSC and FTIR[J].Non-Metallic Mines,2012,35(4):52(in Chinese)秦志扬,秦麟卿,张联盟,等.XRD、TG、DSC和FTIR法研究碱式碳酸镁的热分解[J].非金属矿,2012,35(4):52
14 Xu Bing.Study of self-assembly and growth mechanism of nano-micro boehmite[D].Dalian:Dalian Jiaotong University,2010(in Chinese)徐冰.纳米/微米薄水铝石自组装及其生长机理研究[D].大连:大连交通大学,2010
15 Wang Yinhu,Fan Guangyin,Zhang Chun,et al.High active and selective hydrogenation of p-chloronitrobenzene over Ir/AlO(OH)[J].Appl Chem Ind,2013,42(3):397(in Chinese)王银虎,樊光银,张春,等.Ir/AlO(OH)催化剂对氯代硝基苯催化加氢反应的研究[J].应用化工,2013,42(3):397
16 Chen Wei.Study on the microstructure evolution ofα-Al2O3in the formation process and it′s controlling[D].Changsha:Central South University,2010(in Chinese)陈伟.α-Al2O3形成过程显微结构演变及其调控[D].长沙:中南大学,2010
17 Lu Shaoyuan,He Yunqiu.Application of surfactant to synthesis of nano-alumina[J].Mater Rev,2006,20(6):149(in Chinese)卢少元,贺蕴秋.表面活性剂在纳米氧化铝制备中的应用研究[J].材料导报,2006,20(6):149