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研究生： 翁啟洋
Chi-Yang Weng
論文名稱： 分散聚合法製備均一粒徑聚苯乙烯微米球
指導教授： 陳暉
Hui-Chen
口試委員:
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程與材料工程學系
Department of Chemical & Materials Engineering
論文出版年： 2016
畢業學年度： 104
語文別： 中文
論文頁數： 101
中文關鍵詞： 分散聚合法 、聚苯乙烯微球 、單分散性
外文關鍵詞： Dispersion polymerization, Polystyrene microsphere, Monodisperse
相關次數： 點閱：15  下載：0 
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    • 本研究以分散聚合法製備均一粒徑聚苯乙烯(PS)微米球，並對反應條件溶劑、反應溫度、起始劑偶氮二異丁腈(AIBN)用量、穩定劑聚乙烯基吡咯烷酮(PVP)用量進行探討。
    以異丙醇為反應溶劑時，因為異丙醇和穩定劑PVP相溶性不佳，核與核之間劇烈碰撞，造成PS微球之粒徑均一度差。而以乙醇或甲醇為反應溶劑時則能成功製備均一粒徑PS微米球。
    PS微米球之平均粒徑，隨反應溫度、起始劑AIBN用量增加而大；隨穩定劑PVP用量增加而變小。以乙醇和甲醇為反應溶劑時，所能製備得最大粒徑分別為2.52μm和2.92μm。此外，在乙醇或甲醇溶劑下可以藉由微量(≤5%)添加共溶劑(甲苯或丁酮)來增加PS微米球粒徑。這是因為共溶劑可以增加臨界鏈長(Critical chain length)進而增加PS微球粒徑。

    The preparation conditions , solvents, reaction temperature, the amount of initiator 2,2'Azobisisobutyronitrile(AIBN) and stabilizer Polyvinylpyrrolidone(PVP),of monodisperse polystyrene (PS) microspheres by dispersion polymerization were
    investigated.
    When isopropyl alcohol (IPA) was used as reaction solvent, the compatibility between IPA and PVP was poor. The nuclei collided intensely. So the particle size of
    PS microspheres was not uniform. On the other hands, monodisperse PS particle was obtained by using ethanol (EtOH) or methanol (MeOH) as solvents.
    PS particle size was increased with increasing reaction temperature and amount of AIBN and with decreasing amount of PVP. The maximum size of monodispersemicrospheres prepared by EtOH and MOH were 2.52μm and 2.92μm, respectively. In
    addition, the PS particle sizes were increased by adding few amount (≤5%) of co-solvent (toluene or methyl ethyl ketone) in EtOH or MeOH solvents, respectively.It was considered that co-solvent was able to increase the critical chain length of PS to increase PS particle size.

    中文摘要.................................................I 英文摘要................................................II 目錄..................................................III 表目錄..................................................V 圖目錄................................................VII 第一章 緒論..............................................1 1-1 均一粒徑高分子球製備方法..............................1 1-2. 分散聚合法機制......................................2 1-3. 分散聚合法文獻回顧..................................3 1-4.研究目的與動機.......................................5 第二章 實驗..............................................8 2-1. 實驗藥品............................................8 2-2. 實驗儀器...........................................10 2-3. 實驗方法...........................................11 2-3-1. 單體精餾.........................................11 2-3-2. 製備均一粒徑苯乙烯微米球..........................11 2-4. 高分子微米球的物性測試..............................13 2-4-1. 掃描式電子顯微鏡(SEM) ...........................13 2-4-2. 高分子微米球粒徑分布分析..........................13 第三章 結果與討論.......................................14 3-1. 異丙醇溶劑製備PS 微米球之研究.......................14 3-1-1. 反應溫度對PS 微米球之影響.........................15 3-1-2. 共溶劑對PS 微米球之影響...........................16 (a). 甲苯/異丙醇共溶劑對PS 微米球之影響...................16 (b). 丁酮/異丙醇共溶劑對PS 微米球之影響...................18 3-1-3. 醇類溶劑對PS 微米球之影響.........................19 3-2. 乙醇溶劑製備PS 微米球之研究.........................30 3-2-1. 反應溫度對PS 微米球之影響.........................30 3-2-2. 起始劑用量對PS 微米球之影響.......................31 3-2-3. 穩定劑用量對PS 微米球之影響.......................32 3-2-4. 75oC下製備均一大粒徑PS 微米球之研究...............33 3-2-5. 共溶劑對PS 微米球之影響...........................34 (a). 甲苯/乙醇共溶劑對PS 微米球之影響....................35 (b). 丁酮/乙醇共溶劑對PS 微米球之影響....................36 3-3. 甲醇溶劑製備PS 微米球之研究.........................53 3-3-1. 反應溫度對PS 微米球之影響.........................53 3-3-2. 起始劑用量對PS 微米球之影響.......................54 3-3-3. 穩定劑用量對PS 微米球之影響.......................55 3-3-4. 共溶劑對PS 微米球之影響...........................56 (a). 甲苯/甲醇共溶劑對PS 微米球之影響....................56 (b). 丁酮/甲醇共溶劑對PS 微米球之影響....................57 3-4. 醇類共溶劑對PS 微米球之影響.........................73 3-4-1 甲醇/異丙醇共溶劑對PS 微米球之影響..................73 3-4-2 甲醇/乙醇共溶劑對PS 微米球之影響...................74 第四章 結論.............................................82 參考文獻................................................84

    [1] R. Lambourne, T. Strivens, Paint and surface coatings: theory and practice, Elsevier1999.
    [2] G. Riess, C. Labbe. "Block copolymers in emulsion and dispersion polymerization." Macromolecular rapid communications 2004. 25. 2: 401-435.
    [3] D. Li, Y. Le, X.-Y. Hou, J.-F. Chen, Z.-G. Shen. "Colored nanoparticles dispersions as electronic inks for electrophoretic display." Synthetic Metals 2011. 161. 13: 1270-1275.
    [4] F. Gritti, I. Leonardis, J. Abia, G. Guiochon. "Physical properties and structure of fine core–shell particles used as packing materials for chromatography: relationships between particle characteristics and column performance." Journal of Chromatography A 2010. 1217. 24: 3819-3843.
    [5] X.B. Ding, Z.H. Sun, G.X. Wan, Y.Y. Jiang. "Preparation of thermosensitive magnetic particles by dispersion polymerization." Reactive and Functional Polymers 1998. 38. 1: 11-15.
    [6] T. Ellingsen, O. Aune, J. Ugelstad, S. Hagen. "Monosized stationary phases for chromatography." Journal of Chromatography A 1990. 535. 147-161.
    [7] A. Tuncel, A. Denizli, D. Purvis, C.R. Lowe, E. Pişkin. "Cibacron Blue F3G-A-attached monosize poly (vinyl alcohol)-coated polystyrene microspheres for specific albumin adsorption." Journal of Chromatography A 1993. 634. 2: 161-168.
    [8] J. Singer, The use of polystyrene latexes in medicine, Future directions in polymer colloids, Springer1987, pp. 371-394.
    [9] H. Fritz, M. Maier, E. Bayer. "Cationic polystyrene nanoparticles: preparation and characterization of a model drug carrier system for antisense oligonucleotides." Journal of colloid and interface science 1997. 195. 2: 272-288.
    [10] J. Wang. "Nanomaterial‐based amplified transduction of biomolecular interactions." small 2005. 1. 11: 1036-1043.
    [11] G. Réthoré, A. Mathew, H. Naik, A. Pandit. "Preparation of chitosan/polyglutamic acid spheres based on the use of polystyrene template as a nonviral gene carrier." Tissue Engineering Part C: Methods 2009. 15. 4: 605-613.
    [12] M. Nakazawa, S. Nakahara, T. Hirooka, M. Yoshida, T. Kaino, K. Komatsu. "Polymer saturable absorber materials in the 1.5 μm band using poly-methyl-methacrylate and polystyrene with single-wall carbon nanotubes and their application to a femtosecond laser." Optics letters 2006. 31. 7: 915-917.
    [13] K. Hara, Polarizing element, optical element, and liquid crystal display, Google Patents, 2003.
    [14] B.J. de Gans, E. Kazancioglu, W. Meyer, U.S. Schubert. "Ink‐jet Printing Polymers and Polymer Libraries Using Micropipettes." Macromolecular Rapid Communications 2004. 25. 1: 292-296.
    [15] K. Kaewtatip, V. Tanrattanakul. "Preparation of cassava starch grafted with polystyrene by suspension polymerization." Carbohydrate Polymers 2008. 73. 4: 647-655.
    [16] C. Chern. "Emulsion polymerization mechanisms and kinetics." Progress in polymer science 2006. 31. 5: 443-486.
    [17] Y.S. Choi, M.H. Choi, K.H. Wang, S.O. Kim, Y.K. Kim, I.J. Chung. "Synthesis of exfoliated PMMA/Na-MMT nanocomposites via soap-free emulsion polymerization." Macromolecules 2001. 34. 26: 8978-8985.
    [18] J. Lee, C.K. Hong, S. Choe, S.E. Shim. "Synthesis of polystyrene/silica composite particles by soap-free emulsion polymerization using positively charged colloidal silica." Journal of colloid and interface science 2007. 310. 1: 112-120.
    [19] M. Yasuda, M. Kobayashi, T. Kotani, K. Kawahara, H. Nikaido, A. Ueda, H. Ogino, H. Ishikawa. "Synthesis of amphiphilic polymer particles by seed polymerization and their application for lipase immobilization." Macromolecular Chemistry and Physics 2002. 203. 2: 284-293.
    [20] F. Baines, S. Dionisio, N. Billingham, S. Armes. "Use of block copolymer stabilizers for the dispersion polymerization of styrene in alcoholic media." Macromolecules 1996. 29. 9: 3096-3102.
    [21] G. Bosma, C. Pathmamanoharan, E.H. de Hoog, W.K. Kegel, A. van Blaaderen, H.N. Lekkerkerker. "Preparation of monodisperse, fluorescent PMMA–latex colloids by dispersion polymerization." Journal of colloid and interface science 2002. 245. 2: 292-300.
    [22] M. Cho, K. Yoon, B. Song. "Dispersion polymerization of acrylamide in aqueous solution of ammonium sulfate: synthesis and characterization." Journal of applied polymer science 2002. 83. 7: 1397-1405.
    [23] D. Horák, P. Shapoval. "Reactive poly (glycidyl methacrylate) microspheres prepared by dispersion polymerization." Journal of Polymer Science Part A: Polymer Chemistry 2000. 38. 21: 3855-3863.
    [24] S.M. Klein, V.N. Manoharan, D.J. Pine, F.F. Lange. "Preparation of monodisperse PMMA microspheres in nonpolar solvents by dispersion polymerization with a macromonomeric stabilizer." Colloid and Polymer Science 2003. 282. 1: 7-13.
    [25] M. Okubo, S. Fujii, H. Maenaka, H. Minami. "Production of submicron-sized poly (methyl methacrylate) particles by dispersion polymerization with a poly (dimethylsiloxane)-based azoinitiator in supercritical carbon dioxide." Colloid and Polymer Science 2002. 280. 2: 183-187.
    [26] J.-S. Song, M.A. Winnik. "Cross-linked, monodisperse, micron-sized polystyrene particles by two-stage dispersion polymerization." Macromolecules 2005. 38. 20: 8300-8307.
    [27] J. Yuan, M. Antonietti. "Poly (ionic liquid) latexes prepared by dispersion polymerization of ionic liquid monomers." Macromolecules 2011. 44. 4: 744-750.
    [28] D. Horák, M. Kryštůfek, J. Spěváček. "Effect of reaction parameters on the dispersion polymerization of 1‐vinyl‐2‐pyrrolidone." Journal of Polymer Science Part A: Polymer Chemistry 2000. 38. 3: 653-663.
    [29] K. Takahashi, S. Miyamori, H. Uyama, S. Kobayashi. "Preparation of micron‐size monodisperse poly (2‐hydroxyethyl methacrylate) particles by dispersion polymerization." Journal of Polymer Science Part A: Polymer Chemistry 1996. 34. 2: 175-182.
    [30] K. Cao, J. Yu, B.-G. Li, B.-F. Li, Z.-R. Pan. "Micron-size uniform poly (methyl methacrylate) particles by dispersion polymerization in polar media: 1. Particle size and particle size distribution." Chemical Engineering Journal 2000. 78. 2: 211-215.
    [31] M. Awan, V. Dimonie, M. El‐Aasser. "Anionic dispersion polymerization of styrene. I. Investigation of parameters for preparation of uniform micron‐size polystyrene particles with narrow molecular weight distribution." Journal of Polymer Science Part A: Polymer Chemistry 1996. 34. 13: 2633-2649.
    [32] N.M. Smeets, R.A. Hutchinson, T.F. McKenna. "Determination of the critical chain length of oligomers in dispersion polymerization." ACS Macro Letters 2011. 1. 1: 171-174.
    [33] S. Kawaguchi, K. Ito. "Dispersion polymerization." Polymer Particles 2005. 299-328.
    [34] K.E. Barrett, Dispersion polymerization in organic media, Wiley1975.
    [35] Y. Almog, S. Reich, M. Levy, Brit Polym J 1982, 14, 131, Wiley Online Library| CAS| Web of Science® Times Cited.12: 3104-3109.
    [36] A.J. Paine. "Dispersion polymerization of styrene in polar solvents. 7. A simple mechanistic model to predict particle size." macromolecules 1990. 23. 12: 3109-3117.
    [37] K. Sparnacci, M. Laus, L. Tondelli, L. Magnani, C. Bernardi. "Core–shell microspheres by dispersion polymerization as drug delivery systems." Macromolecular Chemistry and Physics 2002. 203. 10‐11: 1364-1369.
    [38] L. Guo, G.-L. Pei, T.-J. Wang, Z.-W. Wang, Y. Jin. "Polystyrene coating of Fe 3 O 4 particles using dispersion polymerization." Colloids and Surfaces A: Physicochemical and Engineering Aspects 2007. 293. 1: 58-62.
    [39] C. Tseng, Y. Lu, M. El‐Aasser, J. Vanderhoff. "Uniform polymer particles by dispersion polymerization in alcohol." Journal of Polymer Science Part A: Polymer Chemistry 1986. 24. 11: 2995-3007.
    [40] Y.-Y. Lu, M. El‐Aasser, J. Vanderhoff. "Dispersion polymerization of styrene in ethanol: monomer partitioning behavior and locus of polymerization." Journal of Polymer Science Part B: Polymer Physics 1988. 26. 6: 1187-1203.
    [41] Y.-S. Cho, C.H. Shin, S. Han. "Dispersion Polymerization of Polystyrene Particles Using Alcohol as Reaction Medium." Nanoscale research letters 2016. 11. 1: 1-9.
    [42] K.P. Lok, C.K. Ober. "Particle size control in dispersion polymerization of polystyrene." Canadian journal of chemistry 1985. 63. 1: 209-216.
    [43] D. Horák, O. Chaykivskyy. "Poly (2‐hydroxyethyl methacrylate‐co‐N, O‐dimethacryloylhydroxylamine) particles by dispersion polymerization." Journal of Polymer Science Part A: Polymer Chemistry 2002. 40. 10: 1625-1632.
    [44] X. Zhang, S. Shen, L. Fan. "Uniform polystyrene particles by dispersion polymerization in different dispersion medium." Polymer Bulletin 2008. 61. 1: 19-26.
    [45] Y. Almog, M. Levy. "Effect of inititiator on the molecular weight distribution in dispersion polymerization of styrene." Journal of Polymer Science: Polymer Chemistry Edition 1980. 18. 1: 1-11.
    [46] E. Bourgeat-Lami, J. Lang. "Encapsulation of inorganic particles by dispersion polymerization in polar media: 1. Silica nanoparticles encapsulated by polystyrene." Journal of Colloid and Interface Science 1998. 197. 2: 293-308.
    [47] J. Lee, J.U. Ha, S. Choe, C.-S. Lee, S.E. Shim. "Synthesis of highly monodisperse polystyrene microspheres via dispersion polymerization using an amphoteric initiator." Journal of colloid and interface science 2006. 298. 2: 663-671.
    [48] H. Adelnia, H. Riazi, Y. Saadat, S. Hosseinzadeh. "Synthesis of monodisperse anionic submicron polystyrene particles by stabilizer-free dispersion polymerization in alcoholic media." Colloid and Polymer Science 2013. 291. 7: 1741-1748.
    [49] A.J. Paine, W. Luymes, J. McNulty. "Dispersion polymerization of styrene in polar solvents. 6. Influence of reaction parameters on particle size and molecular weight in poly (N-vinylpyrrolidone)-stabilized reactions." Macromolecules 1990. 23.
    [50] C.H. Ho, S.A. Chen, M.D. Amiridis, J. Van Zee. "Dispersion polymerization of styrene in alcohol media: effect of initiator concentration, solvent polarity, and temperature on the rate of polymerization." Journal of Polymer Science Part A: Polymer Chemistry 1997. 35. 14: 2907-2915.
    [51] J.M. Sáenz, J.M. Asua. "Dispersion polymerization in polar solvents." Journal of Polymer Science Part A: Polymer Chemistry 1995. 33. 9: 1511-1521.
    [52] W. Yang. "l. Yang D, Hu JH, el a1." J. Polym. Sci. Polym. Chem. Ed 2001. 39. 4: 555.
    [53] J. Hong, C.K. Hong, S.E. Shim. "Synthesis of polystyrene microspheres by dispersion polymerization using poly (vinyl alcohol) as a steric stabilizer in aqueous alcohol media." Colloids and Surfaces A: Physicochemical and Engineering Aspects 2007. 302. 1: 225-233.
    [54] J.N. Gavgani, M. Shahrousvand, M.M. Aslzadeh. "Monitoring the effects of homogeneity methanol/water/monomer on the mode of polymerization of styrene: dispersion polymerization versus emulsion polymerization." Colloid and Polymer Science 2013. 291. 10: 2299-2309.
    [55] L. Jinhua, Z. Guangyuan. "Polystyrene Microbeads by Dispersion Polymerization: Effect of Solvent on Particle Morphology." International Journal of Polymer Science 2014. 2014.

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