Elastomers and Composites

The Rubber Society of Korea (한국고무학회)
권호 표지

Preparation and Characterization of $CaCO_3$ Encapsulation by PMMA Core-Shell latex

PMMA와 캡슐화된 $CaCO_3$ Core-Shell 라텍스 제조와 물성연구

  • Lim, Jong-Min (Department of Chemical Engineering, Dong-A University) ;
  • Seul, Soo-Duk (Department of Chemical Engineering, Dong-A University)
  • 임종민 (동아대학교 공과대학 화학공학과) ;
  • 설수덕 (동아대학교 공과대학 화학공학과)
  • Published : 2003.12.31
Download PDF
⟨ Previous Next ⟩

Abstract

Inorganic/organic composite particles were also synthesized by changing an initiator an it's concentration, concentration of an adsorbed surfactant, reaction temperature, and agitation speed in the presence of $CaCO_3$ adsorbed SDBS. The polymerization conditions were optimized according to the conversion of the core-shell composite particles. In the inorganic/organic core-shell composite particle polymerization, $CaCO_3$ absorbed surfactant SDBS of 0.5 wt % was prepared first and then core $CaCO_3$ was encapsulated by sequential emulsion polymerization using MMA, concentration of APS $3.16{\times}10^{-3}mol/L$ to minimize the formation of new PMMA particle during MMA shell polymerization. The structure characterization of the inorganic/organic core-shell particles was verified by measuring the decomposition degree of $CaCO_3$ using HCl solution. It was found that $CaCO_3$ was encapsulated by shell PMMA due to having excellent dispersion in the epoxy resin, smooth surface distinctly from spindle shape, and broad particle distribution after the capsulation.

계면활성제가 흡착된 $CaCO_3$를 제조하여 흡착된 유화제의 농도, 개시제의 종류와 농도, 교반속도 및 반응온도에 따라 무기/유기계 core-shell 입자를 제조하였다. 제조된 복합입자의 전환율을 측정하여 중합의 최적조건과 분자량측정, 가수분해도, 필름형성온도, 유리전이온도, 입자경 측정 그리고 입자의 형태를 고찰하여 다음과 같은 결론을 얻었다. 무기/유기 core-shell 입자의 합성의 경우에는 유화제인 SDBS를 0.5 wt% 첨가한 $CaCO_3$를 core로 하여 MMA와 $3.16{\times}10^{-3}mol/L$ 농도의 APS를 단계적으로 주입하여 중합함으로서 $CaCO_3$ 입자 표면에서 MMA의 중합을 잘 유도할 수 있었으며 중합 도중 새로운 폴리머 입자의 생성이 적었다. 무기/유기계의 core-shell 입자의 경우는 염산에 의한 $CaCO_3$ 분해를 이용하여 캡슐화를 조사하고 시차주사열량계(DSC)에 의한 유리전이온도와 열분해 감소중량을 측정한 결과 외부의 유기 폴리머만 분해되는 특성, 에폭시 수지에서의 분산이 캡슐화 되지 않은 $CaCO_3$보다 우수한 특성, 입자경 분포도 측정 결과 입자경 분포도가 고르지 않고 그리고 전자 현미경에 의한 입자모양이 구형화된 특성등으로 core-shell 입자의 구조와 특성을 확인하였다.

Keywords

References

  1. R. Patsiga, M. Litt, and V, Stannett. 'The emulsion polymerization of vinyl acetate. Part I', J. Phys. Chem., 64, 801 (1960) https://doi.org/10.1021/j100835a024
  2. L, J. Hughes and G. L, Brown, 'Heterogenous polymer systems. I. torsional modulus studies', 1. Appl. Polym Sci., 5, 580 (1961) https://doi.org/10.1002/app.1961.070051713
  3. R. F. Mausser, 'The Vanderbilt Latex Handbook', 3rd. Ed., R. T Vanderbilt Company Inc, 1987
  4. H. Warson, 'The Application of Synthetic Resin Emulsion, Emst Benn Ltd', London, 1978
  5. V. I. Eliseeva, 'Morphology and phase structure of latex particles. Their influence on the properties of latices and film', Prog. Org Coatings, 13, 195 (1990) https://doi.org/10.1016/0033-0655(85)80026-1
  6. M. Devon, J, Gardon, G. Roberts, and A, Rudin, 'Effects of core-shell latex morphology on film forming behavior', 1. Appl. Polym. Sci, 39, 2119 (1990) https://doi.org/10.1002/app.1990.070391007
  7. R. Blankenship, A, Kowalski, 'Production of core-sheath polymer particles containing voids, resulting product and use', U, S. Patent, 4, 594, 363 (1986)
  8. L. E. Nielsen, 'Mechanical Properties of Polymers and Composits', 2, Marcel Dekker Inc, 1974
  9. T. Yamaguchi, T. One, M. Sekine, T. Iwai, and T. Okaea, '實在機化合物粉存在下のメ夕夕リル酸メチルの 重合 みにおけるヵプセ 化機構', Kobunslu Ron-bunshu, 40, 259 (1983)
  10. M. Hasegawa, K. Arari, and S. Saito, 'Uniform encapsulation of fine inorganic powder soapless emulsion polymerization', 1. Ploym. Sci, Polym. Chem. Ed., 25, 3117 (1987)
  11. T. Yamaguchi, T. One, and H, Ito, 'Polymerization of vinyl monomers in the presence substance', Angew. Makromol Chem., 32, 177 (1973) https://doi.org/10.1002/apmc.1973.050320115
  12. T Yamaguchi, T. Ono amd Y. Saito, 'Polymerisation of methyl methacrylate in the presence of graphite', Chem. Ind., 783 (1974)
  13. T. Yamagcuhi, H. Tanaka, A, B. Moustafa, T. Ono H. Ito, O Itabashi, M. Endo, Moustsfa, T. Ono, H. Ito, O. ltabashi, M. Endo, M, Ohuchi, and L. Satio, 'Polymerisation of methly methacrylate In the presence of various metal oxides', Chem. Ind, 619 (1974)
  14. T. Yamagcuhi, T. Ono, and H, Hasegawa, 'Coating og metal powder surface with polymethly methacrylate', Chem. Ind, 748 (1975).
  15. T. Yamaguchi, H, Tanaka, T. Ono, M. Endo, and O. Itabashi, '假化誠布在下にゎけるメ夕クリル骸 メチルの 重合', Kobunshi Ronbunshu, 32, 120 (1975)
  16. T. Yamaguchi, H, Tanaka, T. Oni, O. Itabashi, and H, Ito, '高爐スラフ存在下にゎけるメ夕クリル酸メ千 メ重合', Kobunshi Ronbunshu,, 32, 126 (1975)
  17. T. Yamaguchi, T. Ono, and S, Ohara, '金屬流化物存在 下にゎけるヒニルモノマーの重合', Kobunshi Ronbunshu,, 34, 413(1977)
  18. T. Yamaguchi, T. Ono, M. Nozawa, and M. Sekine,'硫酸パリウ厶 紛存在存在下 のメ夕クリル酸 メチルの 合仁打l于毛力ブ七ル 化機構', Kobunshi Ronbunshu, 38, 435(1981)
  19. Wolf-Dieter Hergeth, P. Starre, K. Schmutzler, and S, Wartewing, 'Polymerization in the presence of seeds: 3. emulsion polymerization of vinyl acetate in the presence of quartz powferm', Polymer, 29, 1323 (1988)
  20. K. Furusawa, Y. Ki,ura, and T, Tagawa, 'Syntheses of composit polystyrene latices with silica particles in the core', J. Colloid Interface Sci, 109, 69 (1896) https://doi.org/10.1016/0021-9797(86)90282-1
  21. M. Arai, K, Arai, and S. Saito, 'Studies on suspension and emulsion. Ll. peculoar morphology of composite polymer particles produced by seeded emulsion polymerization', J. Polym. Sci, 20, 1021 (1982)
  22. M. Konno, K. Shimizu, K. Arai, and S. Saito, 'Soapless emulsion polymerization of methyl metha-crylate in water in the presence of barium sulfate', J. Polym. Sci, 25, 223 (1987)
  23. M. Hasegawa, K. Arai, and S. Saito, 'Effect of surfactant adsorbed on encapsulation of fine inoranic powder with soapless emulsion polymerization', J. Polym. Sci, 25, 3231 (1987)
  24. M. Hasegawa, K. Arai, and S. Saito, 'Selective adsorption of polymer on freshly ground solid sur-faces in soapless emulsion polymerization', J. Appl. Polym, Sci, 33, 411 (1978)
  25. Kissinger, H. E., Anal. Chem., 21, 1702 (1957)
  26. Murray, P. and White, J., Trans. Brit. Ceram. Soc., 54, 204 (1955)
  27. M. Hasegawa, K. Arai, and S. Saito, Trans. Brit. Ceram. Soc, 25, 3231 (1987)
  28. M. Hasegawa, K. Arai, and S. Saito, J. Appl. Polym. Sci., 33, 411 (1987)
  29. H. F. Mark, Bikales, C. G. Overberger, Georg Menges, 'Encyclopedia of Polymer Sci. and Engineering', Vol 8, 2nd. Ed., John Wiley & Sons Inc.(1988)
  30. M. Konno, K. Shimizu, K. Arai, and S. Saito, John Wiley & Sons Inc ,25, 223 (1987). Elastomer