Jurnal
Teknologi ProsesMedia Publikasi Karya Ilmiah Teknik Kimia
6(1) Januari 2007: 82 – 84 ISSN 1412-7814
The Thermal Properties of Calcium Carbonate Filled Polypropylene (PP)/
Ethylene Propylene Diene Terpolymer (EPDM) Composites
Salmah
Department of Chemical Engineering, Faculty of Engineering University of Sumatera Utara, Medan 20155
Abstract
The thermal and crystallization behavior of PP/EPDM/CaCO3 composites was studied by thermogravimetry
analysis (TGA) and differential scanning calorimetric (DSC). The results showed that the increasing of filler loading increase the thermal stability and crystallinity of PP/EPDM/CaCO3 composites.
Keywords: paper sludge, calcium carbonate, polypropylene, ethylene propylene diene terpolymer, composites.
Introduction
Thermal analysis of polymers is an important subject as it covers a broad field, ranging from the development of thermoresistant polymers and ablation problem to the stabilization of thermolabile polymers. Thermal analysis is an important analytical method in understanding the structure-property relationship and mastering the technology for molecule design and industrial production of different polymeric materials. Moreover, it is a useful technique to determine the thermal stability of the materials. In addition, it is possible to quantify the amount of moisture and volatiles present which can cause detemoration in the composites.
Thermal analysis studies have been carried out and the effects of crystallinity, orientation and cross-linking haven reported (Daniel et al., 1994, George et al., 2000, Fangling et al., 2004, Joseph et al., 2003).
One of the accepted methods for studying the thermal properties of polymeric materials is
thermogravimetry (TG). Thermogravimetric data indicate a number of stages of thermal breakdown, weight loss of the material in each stage. Threshold temperature, etc. Both TG and derivative thermogravimetry (DTG) will provide information about the nature and extent of degradation of material. In differential scanning calorimetry (DSC), the heat flow rate associated with a thermal event can be measured as a function of time and temperature allowing us to obtain quantitative information about malting and phase transition of the composite system.
Experimental
Materials
Polypropylene homopolymer used in this study was of injection molding grade, from Titan PP polymers (M) Sdn Bhd, Johor, Malaysia (code 6331) with MFI value of 14.0
g/10 min at 2300C. Ethylene propylene diene
Salmah / Jurnal Teknologi Proses 6(1) Januari 2007: 82 – 84 83
Selangor, Malaysia. Calcium carbonate was obtained from Malaysia Calcium Corporation Sdn Bhd., Malaysia, with average size of 4.5µm
(density, 2.7 g/cm3). The formulation of
PP/EPDM/CaCO3 composites used in this study
is shown in Table 1. Tables 2 show the results of semi-quantitative analysis of calcium carbonate used in this study.
Mixing Procedure
Composites were prepared in a Haake
Reomix PolyDrive. Mixing was done at 180 0C
and 50 rpm. EPDM was first charged to start the melt mixing. After 3 min. filler was added followed by PP at the fifth minutes. Mixing was continued for another 5 min. At the end of 10 min, the composites were taken out and sheeted through a laboratory mill at 2.0 mm nip setting. Sample of composites were compression molded in an electrically heated hydraulic press. Hot-press procedures involved preheating at
180 0C for 6 min followed by compressing for 4
min at the same temperature and subsequent cooling under pressure for 4 min.
Thermogravimetry Analysis
Thermogravimetry analysis of the composites was carried out with a Perkin Elmer Pyris 6 TGA analyzer. The samples weight of about 15 – 25 mg were scanned from 50 to 600
0
C using a nitrogen air flow of 50 ml/min and a
heating rate of 20 0C/min. The sample size was
kept nearly the same for all tests.
Differential Scanning Calorimetry
Thermal analysis measurements of selected systems were performed using a Perkin Elmer DSC-7 analyzer. Samples of about 10 – 25 mg
were heated from 20 to 220 0C using a nitrogen
air flow of 50 ml/min and the heating rate of 20
0C/min. The melting and crystallization
behavior of selected composites were also performed using a Perkin Elmer DSC-7. The
crystallinity (Xcom) of composites were
determined using the following relationship:
Xcom (%cryst) = UHf/UHof x 100 … (1)
Where UHf and UHof are enthalpy of fusion
of the system and enthalpy of fusion of
perfectly (100%) crystalline PP, respectively.
For UHof (PP) a value of 209 J/g was used for
100% crystalline PP homopolymer (Greco et
al., 1987). Xcom, which is calculated using this
equation, however, gives only the overall crystallinity of the composites based on the total weight of composites including non-crystalline fractions, and it is not the true crystallinity of the PP phase. The value of
crystallinity for PP phase (Xpp) of the PP
fraction was normalized using Eq. (2) as follow (Shoinake et al., 1998):
Xpp = (Xcom)/Wfpp … (2)
Where Wf pp is the weight fraction of PP in
the composites.
TABLE 1: Formulation of PP/EPDM/CaCO3
composites with different filler loading
Materials Composites Polypropylene (PP) (wt %) 50
EPDM (wt %) 50 Calcium carbonate (wt %) 0, 15, 30,
45, 60
Results and Discussion
Thermogravimetry analysis (TGA) curve of
PP/EPDM and PP/EPDM/CaCO3 at 0,30 and 60
wt % filler loading is show in Figure 1. Table 3
show that the end degradation temperature (Te
deg) and total weight loss of PP/EPDM/CaCO3
at different filler loading. The total weight loss
of PP/EPDM/CaCO3 composites at 60 wt% is
lower than PP/EPDM/CaCO3 at 30% and
PP/EPDM, which might be due to the presence
of large content of inorganic material in CaCO3
with increasing filler loading. This result
indicate that PP/EPDM/CaCO3 composite have
better thermal stability compared PP/EPDM.
TABLE 2: Semi quantitative analysis of Calcium
Carbonate using X- Ray Flourescene Spectrometer Rigaku RIX 3000.
Component Wt %
CaO 56 MgO 1
SiO2 0.13
Al2O3 0.072
Salmah / Jurnal Teknologi Proses 6(1) Januari 2007: 82 – 84
TABLE 3: Percentage weight loss of
PP/EPDM/CaCO3 composites with different filler
loading
Table 4 show the parameter differential scanning calorimetric (DSC) of
PP/EPDM/CaCO3 at different filler loading.
The value of melting temperature (Tm), heat of
fusion of composites (UHf (com)), crystallinity of
composites (Xcom) and crystallinity of PP (Xpp)
also show in Table 2. The results show that the percentage of crystallinity of composites changed with filler loading. It can be seen that
the value of UHf(com) and Xcom decrease with
increasing filler loading. This is due to the decreasing of PP content at higher filler loading. The addition of fillers results in an
increase in Xpp. This behavior is consistent with
the results by reported by Salmah et al., (2005).
-10
FIGURE 1: Thermogravimetric analysis (TGA)
curve of PP/EPDM/CaCO3 composites at 0, 30 and
60 wt % calcium carbonate.
TABLE 4: Parameter DSC of PP/EPDM/CaCO3
composites with different filler loading.
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Daftar Pustaka
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(contoh rujukan jurnal)
Howes, T. & Mackley, M.R. 1990. Experimental axial dispersion for oscillatory flow trough a baffled tube. Chem.Eng.Sci. 45: 1349-1358. (TNR 10pt)
(contoh rujukan prosiding & tahun terbit yang sama) Zuhrina Masyithah & Mohd Sobri Takriff. 2000a.
Interstage backmixing in oscillatory flow in a baffled column. Proc. 2nd International Conference on Advances in Strategic Technologies. 1: 493-498.
Zuhrina Masyithah & Mohd Sobri Takriff. 2000b. Interstage backmixing in oscillatory flow in a baffled column. Jurnal Teknik Mesin. 3(1): 55-60.
(contoh rujukan buku teks)
Fogler, H.S. 1992. Elements of chemical reaction engineering. Ed.2. New Jersey: Prentice-Hall. (contoh rujukan skripsi/tesis/disertasi)
Mohd Sobri Takriff. 1996. Column flooding, gas holdup and interstage backmixing in an aerated multistage, mechanically-agitated, compartmented column. Ph.D Dissertation. University of Arkansas.
(contoh rujukan internet)
Elsevier. 2002. Pedoman penulisan kertas kerja.
http://www.elsevier.com (26 Agustus 2002). (catatan: 26 Agustus 2002 adalah tanggal saat situs
tersebut dirujuk).