Elastomers and Composites

The Rubber Society of Korea (한국고무학회)
권호 표지
DOI QR코드

DOI QR Code

Determination of Epoxy/Anhydride Mixing Ratio for the Highly Silica Filled Compounds with Chromium (III) Octoate Catalyst

  • Lee, Noori (Department of Chemical Engineering, Pusan National University) ;
  • Lee, Dong-Hoon (Department of Chemical Engineering, Pusan National University) ;
  • Lee, Jung Hoon (Composites & Communication Device Materials Business Division, Kukdo Chemical, Co., Ltd.) ;
  • Min, Kyeong-sik (Composites & Communication Device Materials Business Division, Kukdo Chemical, Co., Ltd.) ;
  • Kang, Sung Yun (Research & Development Institute, Hanwha Corporation) ;
  • Seo, Seungkil (Research & Development Institute, Hanwha Corporation) ;
  • Rho, Byung Lae (Defense Industry Technology Center, Agency for Defense Development) ;
  • Kim, Wonho (Department of Chemical Engineering, Pusan National University)
  • Received : 2015.03.23
  • Accepted : 2015.05.18
  • Published : 2015.06.30
Download PDF
⟨ Previous Next ⟩

Abstract

In this study, epoxy/anhydride mixing ratio for the highly silica filled compounds with chromium (III) octoate catalyst was investigated at a low curing temperature ($71^{\circ}C$ for 40 hr) by evaluating the compressive strength with the weight ratio ranges from 0.3/1.0 to 1.0/1.0 of epoxy part (Part A)/anhydride part (Part B). In case of epoxy/anhydride compounds used surface unmodified silica by coupling agent, these compounds need excess anhydride unlike the weight ratio in the conventional epoxy/anhydride compounds. In curing behavior, the epoxy/anhydride compounds containing chromium (III) octoate showed high conversions at $71^{\circ}C$ for 40 hr, even if a dipropylene glycol (DPG) was not used as a polymerization initiator. Also, DPG leads to a poor epoxy network structure. In conclusion, the appropriate weight ratio of Part A/Part B of highly silica filled epoxy/anhydride compounds with chromium (III) octoate catalyst is 0.5/1.0 and the maximum amounts of silica is 1470 phr of epoxy resin.

Keywords

References

  1. Z. Zhang, E. Beatty, and C. P. Wong, "Study on the Curing Process and the Gelation of Epoxy/Anhydride System for No- Flow Underfill for Flip-Chip Applications", Macromol. Mater. Eng., 288, 365 (2003). https://doi.org/10.1002/mame.200390029
  2. J. D. B. Smith and A. W. Ott, "Pre-Reacted Carboxylic Acid Anhydride Complexes as Low Temperature Curing Agents for Epoxy Resins", U. S. Patent 4,273,914 (1981).
  3. J. J. Miyashiro and A. W. Seiling, "Epoxy Compositions Cured with Carboxylic Acid Anhydrides and Metallic Salt of Acetylacetone", U. S. Patent 3,624,032 (1971).
  4. J. R. Lee and S. J. Park, "Development Trend of Matrix Resins in Polymer Composites", Polym. Sci. Technol., 10, 35 (1999).
  5. C. H. Lee and K. M. Kim, "A Study on Cure Behavior of an Epoxy/Anhydride System and Silica Filler Effects", J. Adh. Inter., 10, 117 (2009).
  6. N. W. Gregornik and F. D. Swanson, "Low Temperature Epoxy Resin Curing Agent Comprising Blend of an Anhydride Mixture, an Anhydride Half Ester, and Uranyl Salt", U. S. Patent 3,852,245 (1974).
  7. B. Seo, D. H. Lee, N. Lee, K. Do, K. Ma, and W. Kim, "Effect of Metal Complexes as a Catalyst on Curing Behavior and Mechanical Properties of Silica Filled Epoxy-Anhydride Compounds", Elast. Compos., 49, 59 (2014). https://doi.org/10.7473/EC.2014.49.1.59
  8. G. C. Stevens, "Cure Kinetics of a High Epoxide/Hydroxyl Group-Ratio Bisphenol A Epoxy Resin-Anhydride System by Infrared Absorption Spectroscopy", J. Appl. Polym. Sci., 26, 4279 (1981). https://doi.org/10.1002/app.1981.070261226
  9. T. F. Milta, and R. S. Bauer, "Epoxy Resins-Chemistry and Technology", 2nd ed. by C. A. May, p. 465, Marcel Dekker, Inc., New York, 1988.
  10. P. Guerrero, K. De la Caba, A. Valea, M. A. Corcuera, and I. Mondragon, "Influence of Cure Schedule and Stoichiometry on the Dynamic Mechanical Behaviour of Tetrafunctional Epoxy Resins Cured with Anhydrides", Polymer, 37, 2195 (1996). https://doi.org/10.1016/0032-3861(96)85865-4
  11. N. Bouillon, J. P. Pascault, and L. Tighzert, "Influence of Different Imidazole Catalysts on Epoxy-Anhydride Copolymerization and on their Network Properties", J. Appl. Polym. Sci., 38, 2103 (1989). https://doi.org/10.1002/app.1989.070381112
  12. M. A. Corcuera, M. A. Andres, R. Sarasua, and I. Mondragon, "Rheological and Mechanical Behaviour of Tetraglycidyldiaminodiphenylmethane (TGDDM)/Anhydride Epoxy Systems", Polym. Int., 29, 97 (1992). https://doi.org/10.1002/pi.4990290206
  13. W. H. Park and J. K. Lee, "Cure Kinetics of an Epoxy-rich/ Anhydride/Imidazole System", Polymer (Korea), 22, 374 (1998).
  14. J. J. Park, "Long-term and Short-term AC Treeing Breakdown of Epoxy/Micro-Silica/Nano-Silicate Composite in Needle-Plate Electrodes", Trans. Electr. Electron. Mater., 13, 252 (2012). https://doi.org/10.4313/TEEM.2012.13.5.252
  15. H. Y. Jin, Y. Q, Yang, L. Xu, and S. E. Hou, "Effects of Spherical Silica on the Properties of an Epoxy Resin System", J. Appl. Polym. Sci., 121, 648 (2011). https://doi.org/10.1002/app.33315
  16. R. R. Rindone and W. K. Musker, "Reaction Catalyzed by Chromium (III) Carboxylates", U. S. Patent 6,359,147 B1 (2002).