화학공학소재연구정보센터
홈 로그인 로그아웃 연락처 사이트맵
Macromolecular Research, Vol.16, No.2, 120-127, February, 2008
Export Citation
GMA-Functionalized Reactive Stabilizer for Polymerization of Methyl Methacrylate in Supercritical CO2: Effect of Stabilizer, Initiator and Monomer Concentrations
Sang-Hun Han, Kyung-Kyu Park, and Sang-Ho Lee†
  • Department of Chemical Engineering, Dong-A University, Busan 604-714, Korea
E-mail:
Glycidyl methacrylate linked poly(dimethylsiloxane) (GMA-PDMS) was synthesized and used as a stabilizer for the dispersion polymerization of methyl methacrylate (MMA) in supercritical CO2. This study examined the effect of the concentrations of the stabilizer, 2,2’-azobisisobutyronitrile (AIBN) initiator, and MMA on the yield, molecular weight, and morphology of the poly(methyl methacrylate) (PMMA) product. PMMA was obtained in 94.6% yield using only 0.87 wt% GMA-PDMS. When the AIBN concentration was increased from 0.25 to 1.06 wt%, the molecular weight and particle size of the PMMA decreased from 56,600 to 21,600 and from 4.1 to 2.7 μm, whereas the particle size distribution increased from 1.3 to 1.9. The Mn of the PMMA product ranged from 41,600 and 55,800 under typical polymerization conditions. The PMMA particle diameter ranged from 1.8 to 11.0 μm and the particle size distribution ranged from 1.4 to 1.8.
Keywords:polymerization;supercritical CO2;macromonomer
  1. DeSimone JM, Guan Z, Elsbernd CS, Science, 257, 945 (1992)
  2. Smith SD, DeSimone JM, Huang H, York G, Dwight DW, Wilkes GL, McGrath JE, Macromolecules, 25, 2575 (1992)
  3. Adamsky FA, Beckman EJ, Macromolecules, 27(1), 312 (1994)
  4. Romack TJ, Combes JR, Desimone JM, Macromolecules, 28(5), 1724 (1995)
  5. Romack TJ, Maury EE, Desimone JM, Macromolecules, 28(4), 912 (1995)
  6. Kapellen KK, Mistele CD, Desimone JM, Macromolecules, 29(1), 495 (1996)
  7. Canelas DA, Desimone JM, Macromolecules, 30(19), 5673 (1997)
  8. Park JY, Shim JJ, J. Supercrit. Fluids, 27(3), 297 (2003)
  9. Desimone JM, Maury EE, Menceloglu YZ, Mcclain JB, Romack TJ, Combes JR, Science, 265(5170), 356 (1994)
  10. Hsiao YL, Maury EE, Desimone JM, Mawson S, Johnston KP, Macromolecules, 28(24), 8159 (1995)
  11. Lepilleur C, Beckman EJ, Macromolecules, 30(4), 745 (1997)
  12. Woods HM, Nouvel C, Licence P, Irvine DJ, Howdle SM, Macromolecules, 38(8), 3271 (2005)
  13. Christian P, Giles MR, Griffiths RMT, Irvine DJ, Major RC, Howdle SM, Macromolecules, 33(25), 9222 (2000)
  14. Rosell A, Storti G, Morbidelli M, Bratton D, Howdle SM, Macromolecules, 37(8), 2996 (2004)
  15. Giles MR, Griffiths RMT, Aguiar-Ricardo A, Silva MRCG, Howdle SM, Macromolecules, 34(1), 20 (2001)
  16. Shaffer KA, Jones TA, Canelas DA, Desimone JM, Wilkinson SP, Macromolecules, 29(7), 2704 (1996)
  17. O'Neill ML, Yates MZ, Johnston KP, Smith CD, Wilkinson SP, Macromolecules, 31(9), 2838 (1998)
  18. O'Neill ML, Yates MZ, Johnston KP, Smith CD, Wilkinson SP, Macromolecules, 31(9), 2848 (1998)
  19. Giles MR, Hay JN, Howdle SM, Winder RJ, Polymer, 41(18), 6715 (2000)
  20. Wang RL, Cheung HM, J. Appl. Polym. Sci., 93(2), 545 (2004)
  21. Hanafy GM, Madbouly SA, Ougizawa T, Inoue T, Polymer, 45(20), 6879 (2004)
  22. Approximately 0.2 g of reaction mass was dissolved in 50 mL of dichloromethane and acetic acid (4/1 solution, volume ratio). Enough amount of TBAI was added and dissolved. Afterwards, the conversion of the addition reaction was checked by titration of the above sample with 0.1 M-Perchloric acid
  23. Lee SH, LoStracco MA, Hasch BM, McHugh MA, J. Phys. Chem., 98(15), 4055 (1994)
  24. Lee SH, J. Appl. Polym. Sci., 95(1), 161 (2005)
  25. Kwon HS, Lee SH, Macromol. Res., 11(4), 231 (2003)
  26. Lora M, McHugh MA, Fluid Phase Equilib., 157(2), 285 (1999)
  27. Klein SM, Manoharan VN, Pine DJ, Lange FF, Colloid Polym. Sci., 282, 7 (2003)