快速沉淀法制备高分散高纯度球霰石晶体
|
摘要
旨在提出一种简单、高效的高分散、高纯度球霰石制备方法。在高速搅拌(10000 r/min)条件下,研究了溶液反应时间对球霰石形貌、纯度和粒度的影响,并使用SEM、XRD、TEM分析了球霰石形貌和晶型。研究表明,高速搅拌是制备高分散、粒径均匀多孔球霰石的有效措施。反应时间对球霰石晶型和形貌影响显著,反应时间为30 s时,球霰石纯度为100%,继续增大反应时间则会轻度降低其纯度。然而反应时间增长可使球霰石颗粒更加均匀,分散度提高。60 s或90 s可为优选反应时间,所制备的球霰石粒径为别为1.69μm和1.63μm。
A simple and effective synthesis method of vaterite with high dispersibility and purity was proposed in this study. By mixing solutions with high speed at 10000 r/min,effect of reaction durations on the crystal,morphology and particle sizes of synthesized vaterite was examined using SEM,XRD and TEM. It was found that stirring with high speed was an effective measure to ensure the production of vaterite with high dispersibility and uniform particle sizes. Reaction duration also played significant roles in affecting the crystal and morphology of vaterite. When reaction duration was 30 s,pure vaterite can be gained,nevertheless,increased reaction duration slightly reduced the purity of vaterite. However,increased reaction duration was beneficial for achieving uniform vaterite. 60 s or 90 s can be selected as optimal reaction duration by this study that particle sizes of the synthesized vaterite were 1. 69 μm and1. 63 μm,respectively.
A simple and effective synthesis method of vaterite with high dispersibility and purity was proposed in this study. By mixing solutions with high speed at 10000 r/min,effect of reaction durations on the crystal,morphology and particle sizes of synthesized vaterite was examined using SEM,XRD and TEM. It was found that stirring with high speed was an effective measure to ensure the production of vaterite with high dispersibility and uniform particle sizes. Reaction duration also played significant roles in affecting the crystal and morphology of vaterite. When reaction duration was 30 s,pure vaterite can be gained,nevertheless,increased reaction duration slightly reduced the purity of vaterite. However,increased reaction duration was beneficial for achieving uniform vaterite. 60 s or 90 s can be selected as optimal reaction duration by this study that particle sizes of the synthesized vaterite were 1. 69 μm and1. 63 μm,respectively.
引文
[1]Udera I,Capat C,Olaru E A,et al.Vaterite Synthesis via Gas-Liquid Route under Controlled p H Conditions[J].Industrial&Engineering Chemistry Research,2012,51(24):8185-8193.
[2]Zhao D,Jiang J,Xu J,et al.Synthesis of template-free hollow vaterite Ca CO3microspheres in the H2O/EG system[J].Materials Letters,2013,104:28-30.
[3]Hadiko G,Han Y S,Fuji M,et al.Synthesis of hollow calcium carbonate particles by the bubble templating method[J].Materials Letters,2005,59(19-20):2519-2522.
[4]Saikia J,Das G.Vaterite for selective adsorption of anionic dyes[J].Journal of Environmental Chemical Engineering,2014,2(2):1165-1173.
[5]Chong K Y,Chia C H,Zakaria S,et al.Vaterite calcium carbonate for the adsorption of Congo red from aqueous solutions[J].Journal of Environmental Chemical Engineering,2014,2(4):2156-2161.
[6]Yu S,Wang X,Wu D.Self-Assembly Synthesis of Microencapsulated n-Eicosane Phase-Change Materials with Crystalline-Phase-ControllableCalcium Carbonate Shell[J].Energy and Fuels,2014,28(5):3519-3529.
[7]Fujiwara M,Shiokawa K,Araki M,et al.Encapsulation of Proteins into Ca CO3by Phase Transition from Vaterite to Calcite[J].Crystal Growth&Design,2010,10(9):4030-4037.
[8]Maver U,Bele M,Jamnik J,et al.A fast and simple method for preparation of calcium carbonate-drug composites for fast drug release[J].Materials Research Bulletin,2013,48(1):137-145.
[9]Fujiwara M,Shiokawa K,Hayashi K,et al.Direct encapsulation of BSA and DNA into silica microcapsules(hollow spheres)[J].Journal of Biomedical Materials Research Part A,2007,81A(1):103-112.
[10]夏宏宇,张群,王刚,等.球形和橄榄形球霰石的简易制备研究[J].人工晶体学报,2015,44(6):1701-1706.
[11]Wang Y,Moo Y X,Chen C,et al.Fast precipitation of uniform Ca CO3nanospheres and their transformation to hollow hydroxyapatite nanospheres[J].Journal of Colloid and Interface Science,2010,352(2):393-400.
[12]Han Y S,Hdiko G,Fuji M,et al.Effect of flow rate and CO2content on the phase and morphology of Ca CO3prepared by bubbling method[J].Journal of Crystal Growth,2005,276(3-4):541-548.
[13]Qi R J,Zhu Y J.Microwave-assisted synthesis of calcium carbonate(vaterite)of various morphologies in water-ethylene glycol mixed solvents[J].Journal of Physical Chemistry B,2006,110(16):8302-8306.
[14]汪小红,董晓庆.超声辅助的荔枝状球霰石的制备与表征[J].人工晶体学报,2013,42(10):2164-2169.
[15]Chen P Y,Wang J L,Wang L,et al.Producing vaterite by CO2sequestration in the waste solution of chemical treatment of recycled concrete aggregates[J].Journal of Cleaner Production,2017,149:735-742.
[16]Wu J,Zhu Y J,Zhao X Y,et al.Amorphous calcium silicate hydrate/block copolymer hybrid nanoparticles:synthesis and application as drug carriers[J].Dalton Transactions,2013,42(19):7032-7040.
[17]Nagaraja A T,Pradhan S,Mc Shane M J.Poly(vinylsulfonic acid)assisted synthesis of aqueous solution stable vaterite calcium carbonate nanoparticles[J].Journal of Colloid and Interface Science,2014,418:366-372.
[18]Chen P Y,Ma H H,Xu Y,et al.Improving the productivity and purity of vaterite produced by bubbling method[J].International Journal of Materials Research,2017,108:600-606.
[2]Zhao D,Jiang J,Xu J,et al.Synthesis of template-free hollow vaterite Ca CO3microspheres in the H2O/EG system[J].Materials Letters,2013,104:28-30.
[3]Hadiko G,Han Y S,Fuji M,et al.Synthesis of hollow calcium carbonate particles by the bubble templating method[J].Materials Letters,2005,59(19-20):2519-2522.
[4]Saikia J,Das G.Vaterite for selective adsorption of anionic dyes[J].Journal of Environmental Chemical Engineering,2014,2(2):1165-1173.
[5]Chong K Y,Chia C H,Zakaria S,et al.Vaterite calcium carbonate for the adsorption of Congo red from aqueous solutions[J].Journal of Environmental Chemical Engineering,2014,2(4):2156-2161.
[6]Yu S,Wang X,Wu D.Self-Assembly Synthesis of Microencapsulated n-Eicosane Phase-Change Materials with Crystalline-Phase-ControllableCalcium Carbonate Shell[J].Energy and Fuels,2014,28(5):3519-3529.
[7]Fujiwara M,Shiokawa K,Araki M,et al.Encapsulation of Proteins into Ca CO3by Phase Transition from Vaterite to Calcite[J].Crystal Growth&Design,2010,10(9):4030-4037.
[8]Maver U,Bele M,Jamnik J,et al.A fast and simple method for preparation of calcium carbonate-drug composites for fast drug release[J].Materials Research Bulletin,2013,48(1):137-145.
[9]Fujiwara M,Shiokawa K,Hayashi K,et al.Direct encapsulation of BSA and DNA into silica microcapsules(hollow spheres)[J].Journal of Biomedical Materials Research Part A,2007,81A(1):103-112.
[10]夏宏宇,张群,王刚,等.球形和橄榄形球霰石的简易制备研究[J].人工晶体学报,2015,44(6):1701-1706.
[11]Wang Y,Moo Y X,Chen C,et al.Fast precipitation of uniform Ca CO3nanospheres and their transformation to hollow hydroxyapatite nanospheres[J].Journal of Colloid and Interface Science,2010,352(2):393-400.
[12]Han Y S,Hdiko G,Fuji M,et al.Effect of flow rate and CO2content on the phase and morphology of Ca CO3prepared by bubbling method[J].Journal of Crystal Growth,2005,276(3-4):541-548.
[13]Qi R J,Zhu Y J.Microwave-assisted synthesis of calcium carbonate(vaterite)of various morphologies in water-ethylene glycol mixed solvents[J].Journal of Physical Chemistry B,2006,110(16):8302-8306.
[14]汪小红,董晓庆.超声辅助的荔枝状球霰石的制备与表征[J].人工晶体学报,2013,42(10):2164-2169.
[15]Chen P Y,Wang J L,Wang L,et al.Producing vaterite by CO2sequestration in the waste solution of chemical treatment of recycled concrete aggregates[J].Journal of Cleaner Production,2017,149:735-742.
[16]Wu J,Zhu Y J,Zhao X Y,et al.Amorphous calcium silicate hydrate/block copolymer hybrid nanoparticles:synthesis and application as drug carriers[J].Dalton Transactions,2013,42(19):7032-7040.
[17]Nagaraja A T,Pradhan S,Mc Shane M J.Poly(vinylsulfonic acid)assisted synthesis of aqueous solution stable vaterite calcium carbonate nanoparticles[J].Journal of Colloid and Interface Science,2014,418:366-372.
[18]Chen P Y,Ma H H,Xu Y,et al.Improving the productivity and purity of vaterite produced by bubbling method[J].International Journal of Materials Research,2017,108:600-606.