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Received November 19, 2009
Accepted January 17, 2010
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Dispersion polymerization of N-vinyl caprolactam in supercritical carbon dioxide
School of Chemical and Biological Engineering and Institute of Chemical Processes, Seoul National University, 559, Gwanang-ro, Gwanak-gu, Seoul 151-744, Korea 1R&D Institute, Miwon Specialty Chemical Co., Ltd., 405-3, Moknae-dong, Ansan-si, Gyeonggi-do 425-100, Korea
Korean Journal of Chemical Engineering, September 2010, 27(5), 1613-1620(8), 10.1007/s11814-010-0255-y
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Abstract
Dispersion polymerization of N-vinyl caprolactam (NVCL) was carried out in supercritical carbon dioxide (scCO2) using three surfactants. The polymerization was performed in the presence of fluorine-based poly(heptadecafluorodecyl acrylate) (PHDFDA), poly(heptadecafluorodecyl methacrylate) (PHDFDMA) or siloxane-based PDMSg-pyrrolidonecarboxylic acid (Monasil PCA) as a surfactant. FE-SEM and image analyzer were used to characterize particle morphology, size, and size distribution. When fluorine-based surfactants were used, spherical PVCL particles_x000D_
were obtained. Using Monasil PCA resulted in agglomerated and irregular polymer particles. The effect of concentration of surfactants, initiators, and monomer, and reaction pressure on the particle morphology, average particle size and particle size distribution (PSD) was also investigated with fluorine-based surfactant, PHDFDA or PHDFDMA.
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References
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Verbrugghe S, Bernaerts K, Filip E, Macromol. Chem. Phys., 204, 1217 (2003)
Kirsh YE, Yanul NA, Kalninsh KK, Eur. Polym. J., 35, 305 (1999)
Mikheeva LM, Grinberg NV, Mashkevich AY, Grinberg VY, Thanh LT, Makhaeva EE, Khokhlov AR, Macromolecules, 30(9), 2693 (1997)
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Shin J, Oh KS, Bae W, Lee YW, Kim H, Ind. Eng. Chem. Res., 47(15), 5680 (2008)
Shin J, Bae W, Lee YW, Kim H, J. Chem. Eng. Data., 51, 1571 (2006)
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Kwon S, Lee K, Bae W, Kim H, J. Supercrtit. Fluids., 30, 127 (2008)
Kwon S, Bae W, Kim H, J. Chem. Eng. Data., 50, 1560 (2005)
Paine AJ, Luymes W, McNulty J, Macromolecules., 23, 3104 (1990)
Ober CK, Hair ML, J. Polym. Sci.: Part A: Polym. Chem. Ed., 25, 1395 (1987)
Shen S, Sudol ED, El-Aasser MS, J. Polym. Sci.: Part A:Polym. Chem. Ed., 31, 1393 (1993)
Horak D, Krystufek M, Spevacek J, J. Polym. Sci. A: Polym. Chem., 38(3), 653 (2000)
Hsiao YL, Maury EE, Desimone JM, Mawson S, Johnston KP, Macromolecules, 28(24), 8159 (1995)
Carson T, Lizotte J, Desimone JM, Macromolecules, 33(6), 1917 (2000)