Preparation and Characterization of Layered Silicate Polyethylene Terephthalate Nanocomposite by in Situ Polymerization

Document Type : Research Paper

Authors

1 Research Institute of Petroleum Industry (RIPI)

2 Technology Development of Chemical, Polymeric, and Petrochemical Research Division, Research Institute of Petroleum Industry (RIPI), Tehran, Iran

Abstract

A series of experiments on the synthesis of poly (ethylene terephthalate) (PET)/organo-montmorillonite (MMT) nanocomposites were carried out in a pressurized reactor using alkyl ammonium exchanged smectite clays, (Closite 30B).Given the degradation of organoclay at high temperatures, the in situ polymerization process was carried out at mild temperatures ranging from 210 to 230°C for 40 minutes followed by solid state polymerization (SSP) at 245°C for 30 minutes at a pressure of 5 mbar. The nanocomposites were prepared using different weight percentages (1-5)of organoclay. The reaction completed when the mixing torque ceased to change as recorded by the auto data acquisition system of the pressure reactor. The DSC analysis provided information on the course of the thermal characterization of the PET nanocomposites versus regular PET. As shown by the results of DSC cooling scan, all the PET nanocomposite samples have higher crystallization temperatures (Tc) and faster crystallization rates (HC/t) compared to regular PET. Furthermore, the opposite behavior is observed for t1/2. This is due to the fact that the nucleation of organoclay nanoparticles reduces the crystallite size in the PET nanocomposites. The XRD results indicated that the peaks in the 2θ angle from 1° to 7° were disappeared, which is an indication of an exfoliated MMT.In addition, The atomic force microscope (AFM) results showed broken mirror like lamellae, confirming the exfoliated results of the XRD analysis. The peaks are indexed according to the 2θ angle from 10° to 30° known assignments of the triclinic unit cell dimensions for PET. The comparative crystallite size of the PET nanocomposites samples (1-5%wt organoclay) can be deduced from the peak ratio change of 2θ angle from 10° to 30°. Heat distortion (or deflection) temperature (HDT) was enhanced by increasing the amount of organoclay in PET nanocomposites compared to regular PET. The tensile test results of 2%wt organoclay show an increase of 58% in the tensile strength of this sample. As a result of MMT agglomeration, due to the high temperature instability of Closite 30B, the relative oxygen pressure drop data shows fluctuations. However, as an overall trend, PET nanocomposite gives about 50% greater reduction in O2 pressure drop or relative oxygen permeability compared with a homo structure.

Keywords


            [1]            Ray S. S. and Okamoto M., “Polymer/Layered Silicate Nanocomposites: A Review from Preparation to Processing,” Progress in Polymer Science, 2003, 28, 1539-1641.
      [2]     Gupta B., Lacrampe M-F., Krawczak P., “Polyamide-6/ Clay Nanocomposites, A Critical Review,” Polymer and Polymer Composites, 2006, 14, 13-38.
      [3]     Lee W. D. and. Im S. S, “Dispersibility of Clay and Crystallization Kinetics for In Situ Polymerized PET/Pristine and Modified Montmorillonite Nanocomposites,” Journal of Polymer SciencePart B: Polymer Physics, 2007, 28, 45-53.
      [4]     Hwang S. Y., Lee W. D., Lim J. S., Park K. H, et al., “Dispersibility of Clay and Crystallization Kinetics for In Situ Polymerized PET/Pristine and Modified Montmorillonite Nanocomposites,Journal of Polymer SciencePart B: Polymer Physics, 2008, 46, 1022-1035.
      [5]     Mainar K. K., “Polymeric Nanocomposites a Review, Polymer-Plastics Technology and Engineering, 2004, 43, 427-443.
            [6]            Chang J.H., Kim S. J., Joo Yong L., and Im S., "Poly Ethylene Terephthalate Nanocomposites by in Situ Interlayer Polymerization, Polymer, 2004, 45, 919-926.
      [7]     Ke Y., Long Ch., and Qi Z., “Crystallization, Properties, and Crystal and Nanoscale Morphology of PET-Clay Nanocomposites,” Journal of Applied Polymer Science, 1999, 71, 1139-1146.
      [8]     Costache M. C., Heidecker M. J., Manias E., and Wilkie Ch. A., “Preparation and Characterization of Poly (Ethylene Terephthalate)/Clay Nanocomposites by Melt Blending Using Thermally Stable Surfactants,” Polymers for Advanced Technologies, 2006, 17, 764–771.
      [9]     Pavlidoua S. and Papaspyrides C. D., A Review on Polymer Layered Silicate Nanocomposites,” Progress in Polymer Science, 2008, 33, 1119-1198.
    [10]    Esmailzadeh A., et al, “Mechanical and Crystallization Analyses of Layered Silicate Polyethylene Terephthalate Nanocomposites,” Prepared by in Situ Polymerization Asia/Australia Regional Meeting, Kish island, Iran, 2011, 15-17.
    [11]    Ou C.F., Ho M.T., and Lin J.R., Synthesis and Characterization of Poly (Ethylene Terephthalate) Nanocomposites with Organoclay,” Journal of Applied Polymer Science, 2004, 91, 140-145.
    [12]    Patro T. U., Khakhar D. V., and Misra A., “Phosphonium-Based Layered Silicate—Poly (Ethylene Terephthalate) Nanocomposites: Stability, Thermal and Mechanical Properties,” Journal of Applied Polymer Science, 2009, 113, 1720-1732.
         [13]         Chang J. H., Mun M. K., Lee C., “Poly (Ethylene Terephthalate) Nanocomposite Fibers by in Situ Polymerization: The Thermomechanical Properties and Morphology,” Journal of Applied Polymer Science, 2005, 98, 2009-2016.
    [14]    Guan G. H., Li C. C., and Zhang D., “Spinning and Properties of Poly (Ethylene Terephthalate)/Organomontmorillonite Nanocomposite Fibers,” Journal of Applied Polymer Science, 2005, 95, 1443-1447.
    [15]    Guan G., Li C., Zhang D., and Jin Y., “The Effects of Metallic Derivatives Released from Montmorillonite on the Thermal Stability of Poly(EthyleneTerephthalate)/Montmorillonite Nanocomposites, Journal of Applied Polymer Science, 2006, 101, 1692-1699.
    [16]    Jabarin S. A., “Polymeric Materials Encyclopedia,” 1996, 8, CRC press, 6078-6085, 6091-6100.
    [17]    Wiesendanger R., Scanning Probe Microscopy and Spectroscopy,” 1994 (Cambridge: Cambridge University Press).
    [18]    Calcagno C. I. W., Mariani C. M., Teixeira S. R., and Mauler R. S., The Effect of Organic Modifier of the Clay on the Morphology and Crystallization Properties of PET Nanocomposites,” Polymer, 2007, 48, 966-974.
    [19]    Sharma R., Joshi H., and Jain P.,Short Review on the Crystallization Behavior of PET/Clay Nanocomposites,” Journal of Chemical Engineering and Materials Science, 2011, 2, 39-43.
    [20]    Kim T. Y., Lofgren E. A., and Jabarin S. A., “Solid-State Polymerization of Poly (Ethylene Terephthalate). I. Experimental Study of the Reaction Kinetics and Properties,” Journal of Applied polymer Science, 2003, 89, 197-212.
        [21]        Neef C. J. and Ferraris J. P., “Improved Synthetic Procedure and Molecular Weight Control,” Macromolecules, 2000, 33, 2311–2314.
    [22]    Dini M., Carreau P. J., Kamal M.R., Minh-Tan, et al., “Effect Of Organoclay Content In Solid-State Polymerization Of Poly (Ethylene Terephthalate),” Society of Plastics Engineers (SPE) 2014,10,2417
         [23]         Dini M., Carreau P. J., Kamal M. R., Ton-That M. T., et al., “Solid-State Polymerization of Poly (Ethylene Terephthalate): Effect of Organoclay Concentration, Polymer Engineering Science, 2014, First published online: 22 January. doi:10.1002/pen.23853.
    [24]    Chacko A., Sadiku E. R., and Vorster O. C., “The Rheological and Mechanical Properties of Organoclay Nanocomposites, Journal of Reinforced Plastics and Composites, 2010, 29, 4.
    [25]    Guihe L., Zhifeng F., and Ding C., “Study on the Synthesis and Properties of PET Using Hydrotalcite as Catalyst, China Petroleum Processing and Petrochemical Technology, 2013, 15, 65-69
    [26]    Ke Y. C. and Stroeve P., Polymer-Layered Silicate and Silica Nanocomposites,” Radarweg 29 P. O. Box 211, 1000 AE Amsterdam, the Netherlands Elsevier B. V. ISBN: 0-444-51570-4 (1St ed.) 2005 P224, 322.
    [27]    Wang Y., Gao J., Ma Y., and Agarwal U. S., “Study on mechanical properties, thermal stability and crystallization behavior of PET/MMT nanocomposites,” Composites: Part B 37 2006, 399.
    [28]    Yelkovan S., Yılmaz D., and Aksoy K., “A study of organo-modified clay type on pet-clay based nanocomposite properties, Usak University Journal of Material Sciences,2014, 1, 33 –46.
    [29]    Hegde R. R., Bhat G. S., and Deshpande B., “Crystallization Kinetics and Morphology of Melt Spun Poly (Ethylene Terephthalate) Nanocomposite Fibers, Express Polymer Letters, 2013, 7, 821–831.
         [30]         Bushroa A. R., Rahbari b R. G., Masjuki d H. H., and Muhamadc M. R., “Approximation of Crystallite Size and Microstrain Via XRD Line Broadening Analysis, Vacuum 86, 2012, 1107-1112
    [31]    Avolio R., Gentile G., Avella M., Carfagna C., et al. “Polymer–filler interactions in PET/CaCO3 nanocomposites: Chain ordering at the interface and physical properties,European Polymer Journal 2013, 49, 419-427.
         [32]         Carrera M. C., Erdmann E., and H. A. “Destéfanis Barrier Properties and Structural Study of Nanocomposite of HDPE/Montmorillonite,” Journal of Chemistry, 2013, Article ID 679567, 7.
    [33]     Ghorbanzadeh A. M. and Matin N. S., “Methane Conversion to Hydrogen and Higher Hydrocarbons by Double Pulsed Glow Discharge, Plasma Chemistry and Plasma Processing, 2005, 25, 19-29.
    [34]    Hongfei L., Yanying W., Jürgen C., and Haihui W., “Oxidative Coupling of Methane with High C2 Yield by using Chlorinated Perovskite Ba0.5Sr0.5Fe0.2Co0.8O3−δ as Catalyst and N2O as Oxidant,” Heterogeneous & Homogeneous & Bio- & Nano-Chemcatchem Catalysis., 2010, 2, 1539-1542.
    [35]    Darwent B., “Bond Dissociation Energies in Simple Molecules,” U.S. National Bureau of Standards, 1970, 23.
         [36]         Labde R., “Preparation and Characterization of Polyethylene Terephthalate/Montmorillonite Nanocomposites by In-situ Polymerization Method,” Thesis of the Master of ScienceDegree in Chemical Engineering, Entitled University of Toledo, Ohio, United States, May 2010.