多步种子溶胀法制备微米级大粒径单分散胶体微球
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摘要
为制备大粒径(接近20μm)、单分散聚苯乙烯(PS)微球,首先采用分散聚合法制备PS种子微球,再经过多步种子溶胀策略实现制备目标。讨论了多步溶胀过程中稳定剂聚乙烯醇(PVA)浓度对PS微球的粒径和单分散性Cv的影响,以及阻聚剂NaNO_2对聚合过程中二次核心的影响。结果表明:种子PS微球粒径为(3. 15±0. 13)μm,在种子溶胀过程中,随着变异系数先减小后增大;加入NaNO_2可有效抑制二次核心生成;经三步种子溶胀最终制得平均粒径为18. 76μm、变异系数为0. 209的PS微球。
In order to prepare large size( nearly 20 μm),monodisperse polystyrene( PS) micro-spheres,PS seed microspheres were prepared by dispersion polymerization method,and then PS microspheres was prepared by multistep seed swelling method. The effect of PVA concentration on the particle size and monodispersity of PS microspheres were discussed,and the effect of the inhibitor NaNO_2 on the secondary particles was discussed. The results showed that the diameter of seed PS microshperes was 3. 15( ± 0. 13) μm. In each step of the seed swelling process,the particle size of PS microspheres decreased gradually,and the variation coefficient( Cv) decreased first and then increased with the increase of PVA concentration. The addition of NaNO_2 could effectively inhibit the generation of secondary particles. The average particle diameter and Cvof PS microspheres prepared by the three-step seed swelling was 18. 76 μm and 0. 209,respectively.
In order to prepare large size( nearly 20 μm),monodisperse polystyrene( PS) micro-spheres,PS seed microspheres were prepared by dispersion polymerization method,and then PS microspheres was prepared by multistep seed swelling method. The effect of PVA concentration on the particle size and monodispersity of PS microspheres were discussed,and the effect of the inhibitor NaNO_2 on the secondary particles was discussed. The results showed that the diameter of seed PS microshperes was 3. 15( ± 0. 13) μm. In each step of the seed swelling process,the particle size of PS microspheres decreased gradually,and the variation coefficient( Cv) decreased first and then increased with the increase of PVA concentration. The addition of NaNO_2 could effectively inhibit the generation of secondary particles. The average particle diameter and Cvof PS microspheres prepared by the three-step seed swelling was 18. 76 μm and 0. 209,respectively.
引文
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[10]龚小燕,袁桂梅,陈胜利.微米级单分散聚苯乙烯微球的制备[J].中国粉体技术,2010,16(2):4-7.GONG X Y,YUAN G MCHEN S L. Synthesis of microsized monodisperse polystyrene icrospheres[J]. China Powder Science and Technology,2010,16(2):4-7.
[11] MA G H. Control of polymer particle size using porous glass membrane emulsification[J]. China Particuology,2003,1(3):105-114.
[2]曹同玉,戴兵,戴俊燕,等.单分散、大粒径聚苯乙烯微球的制备[J].高分子学报,1994(2):158-164.CAO T Y,DAI B,DAI J Y,et al. Preparation of monodisperse polystyrene microspheres with large size[J].Acta Polymerica Sinica,1994(2):158-164.
[3]董聿生,梁峰,金红霞,等.新型磁性亲和吸附剂的制备及其在尿激酶纯化中的应用研究[J].高等学校化学学报,2002,23(6):1013-1017.DONG Y S,LIAN G F,JIN H X,et al. Preparation of novel magnetic affinity adsorbents and application for purification of urokinase[J]. Chemical Research In Chinese Universities,2002,23(6):1013-1017.
[4]王群,钱瑜,府寿宽,等.不同尺寸(0. 02~0. 5μm)单分散聚苯乙烯乳液微球的制备[J].功能高分子学报,1993,6(1):12-20.WANG Q,QIAN Y,FU S K,et al. The synthesis of monodispersed polystyrene colloid spheres with different sizes(0. 02~0. 5μm)[J]. Journal of Functional Polymers,1993,6(1):12-20.
[5]吴其晔,高卫平,贾云,等.乳液聚合法合成单分散交PS纳米微球[J].青岛化工学院报,2000,21(1):1-4.WU Q Y,GAO W P,JIA Y,et al. Synthesis and characterization of monodisperse cross-linked polystyrene microspheres[J]. Journal of Qingdao Institute of Chemical Technology,2000,21(1):1-4.
[6]马光辉,苏志国.高分子微球材料[M].北京:化学工业出版社,2005.MA G H,SU Z G. Polymer microspheres[M]. Beijing:Chemical Industry Press,2005.
[7]曹同玉,刘庆普,胡金生.聚合物乳液合成原理、性能及应用[M].北京:化学工业出版社,1997.CAO T Y,LIU Q P,HU J S. Synthesis principle,properties and application of polymer emulsion[M]. Beijing:Chemical Industry Press,1997.
[8]李红,关燕霞,薛新民,等.悬浮聚合法合成纳米级单分散交联聚苯乙烯微球[J].石油化工,2004,33(6):560-562.LI H,GUAN Y X,XUE X M,et al. Preparation of monodispersed cross-linked polystyrene nano-microspheres by suspension polymierization[J]. Petrochemical Technology,2004,33(6):560-562.
[9]熊颖辉,李红,李慧芝.悬浮共聚法合成功能性微米级单分散交联聚苯乙烯微球[J].石油化工,2008,37(5):502-509.XIONG Y H,LI H,LI H Z. Preparation of functional micron-sized monodispersed cross-linking polystyrene microspheres by suspension copolymierization[J]. Petrochemical Technology,2008,37(5):502-509.
[10]龚小燕,袁桂梅,陈胜利.微米级单分散聚苯乙烯微球的制备[J].中国粉体技术,2010,16(2):4-7.GONG X Y,YUAN G MCHEN S L. Synthesis of microsized monodisperse polystyrene icrospheres[J]. China Powder Science and Technology,2010,16(2):4-7.
[11] MA G H. Control of polymer particle size using porous glass membrane emulsification[J]. China Particuology,2003,1(3):105-114.