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composite
Taranitharan Thiruselvan*, Dr. Firuz Zainuddin*
* Polymer Engineering, School of Material Engineering, Universiti Malaysia Perlis (UniMAP),
Kompleks Pusat Pengajian Jejawi 2, Taman Muhibbah, 02600 Jejawi, Arau, Perlis, Malaysia.
Abstract
In this research, polyurethane rigid foam with charcoal filler were prepared and characterized. The
purpose is to use coconut shell charcoal filler which was grinded to obtain powder form to be used as
particulate filler in polyurethane foam to produce a composite with its mechanical strength to be
identified by several testings. Properties of the composite foam were compared with the control PU foam
with four percentage considered (2%, 4%, 6% and 8%). Two batch were produced with different
procedures where the first batch the filler were mixed with polyol first them MDI while for the second
batch is where the filler were mixed with MDI then polyol. Compression test was executed to compare
the modulus and the compressive strength of the filled foam. Density test were also carried out to
determine the effect of filler loading on the PU foam. The density does not vary much when more filler is
added due to the characteristic structure of the charcoal filler. Morphology of the foam surface that
undergone the compression test were probed using Scanning Electron Microscopy. The images obtained
shows the ruptured closed cells and the difference in average cell size upon filler loading. The
spectroscopy behavior of the charcoal composite PU foam was analyzed using the Fourier Transform
Infrared (FTIR) spectroscopy. The chemical structure and functional groups were inspected from the peak
analysis of the sample tested.
3
peed trrer wth 2000 rpm n 20 seconds. fter 2.3.4. Morphology (cnnng Electron Mcrocopy)
mxng polyol wth chrcol powder the docynte
dded nd mxed for 20 econds at 2000rpm untl fter the pecmen w deformed, EM mchne
the mxture blended well together homogeneouly model JOEL-JM-6460-L ued to exmne the
untl the mxture relee het ndctng the urfce morphology. The pecmen w cut nto
ntton of the chemcl recton. nother et of mll ze whch 10 mm x 10 mm x 10mm to
mxng done wth lght chnge n procedure undergo EM. EM h n dvntge n uffcently
where chrcol powder frt mxed wth produce cler enlrgement of the mge to vew
docynte before ddng n the polyol. The the cell nd t functon by cnnng the pecmen
mxture wll be poured nto the cloed mold wth wth hgh energy bem of electron.
dmenon of 250mm x 190mm x 75mm. fter
pourng the mxture, the mold h to cloe ft
before the mxture rng nd overflow. The mold 4,4- methylene
Polyol + Coconut
wth polyurethne fom plced n room shell charcoal dphenyl
temperture nd cured for 1 hour and post cured in powder dsocynte +
oven at 800C with the mold for another 1 hour. fter Coconut shell
curng the mple tken out from the mold. The charcoal
Mix (2000 rpm in powder
overall flow chart is as shown in Figure 1 . for 20 sec)
Mix (2000 rpm in
for 20 sec)
2.3. Characterization of Samples
4,4- methylene
dphenyl Polyol
2.3.1. Denty Meurement
Denty the m per unt volume of ubtnce, Mixing process (2000 rpm for
the ymbol ued for denty (Greek letter rho)
nd t unt re kg/m3. Where volume meure
Casting into mould
of the pce occuped by old nd meured by
multply length by length, f the length n meter
the unt of volume cubc meter (m3) nd m Curing at room temperature for 1
the mount of mtter n body nd t meured n
klogrm (kg). From the bulk fom produced 5 cube Postcured in oven for another 1 hour at
mple wth dmenon of 50mm x 50mm x 50mm
cut nd teted for t denty nd the verge
denty wll be recorded for ech type of Rigid Polyurethane foam filled
formulton. with coconut shell charcoal
composite
2.3.2. Compreon Tet
4
lower viscosity and can mix faster accordingly to the
0.7
reaction to produce the foam and ease the process
0.6 and there is also less chances of the charcoal filler to
dispense. Thus, the filler is much well dispersed in
0.5 this polyurethane foam matrix and shows the
FILLER MIXED WITH POLYOL THEN enhance in strength.
0.4 MDI
5
Fig. 3: Variation of compression modulus over Fig. 4: Variation of density over filler loading based
charcoal filler loading. on two mixing method.
3.3. Density Test However, the decrease is not much as and varies
a lot in raw data obtained this is caused by the
Density test is done by dividing the mass of the natural characteristic of the charcoal particles itself
particles in a material by the overall volume as they have millions of pores to absorbs air
occupied by it. The overall volume sum is including molecules [10]. This is because during the charcoal
inter-particle voids volume, particles volume and making process the charcoal will be treated with
the internal volume of the pores [8]. For foam oxygen which then increases its adsorbent
produced in closed molds the density seems to tally characteristics. Hence as this occluded air molecules
with the compressive strength value as filler loading increases; the bulk density tends to decrease.
amount varies. The density change can be observed
through the morphology of the cell itself. In Fig. 4, 3.4. Morphology (SEM)
the graph shows that the highest density value is
shown by the foam loaded with 4% of charcoal fillers Scanning electron microscopy result were shown
with the 2nd batch showing slightly higher value than in the following Fig. 5 to Fig. 8 according to the
1st batch. percentage of filler added. The accelerated voltage
used was 10 kV. The scanned cross-sectional
This is mainly due to the mixing method, where surfaces are showing ruptured cells as the foam
the viscosity play its role as explained in third were scanned after the compression testing were
paragraph in section 3.1. On the other hand, for the done. It can be noticed that some unruptured cells
lowest density is shown by the 8% filler loaded are almost spherical in shape with many windows
foam. As filler increases during the mixture it is very which shows that they are closed cells [11]. The size
hard to ensure that the dispersion of filler is well and of the foaming cell decreases as the percentage of
uniform, thus leading to agglomeration of the filler fillers added increases [12]. From the result of SEM
[9]. itself there is a gradual change in cell size averagely
from Fig. 5 to Fig. 8.
55
However, to be precise the uniformity of the cell
54 size is varied when filler added this is because the
dispersion of fillers in the matrix during the foaming
53 will cause difference in force to get the foaming
FILLER MIXED WITH POLYOL FIRST THEN MDI done. Thus, causing it to be smaller as the more
(1st Batch) 52
filler is added more force needed for foaming with
DENS ITY (kg/m^3) 51 the filler incorporated on the cells and vice versa.
[12]. As more filler added its seems the rigidity will
50 increase due to the filler to fill up the spaces in the
49 foam causing a much dense yet rigid structure.
FILLER MIXED WITH MDI FIRST THEN POLYOL Thus, adding too much of fillers could cause drop of
(2nd Batch) 48 foam properties and the right amout of charcoal
filler percentage for filling the PU foam is around 4%.
6
addition from 2%, 4%, 6% to 8% there is gradual Then for there is a peak identified after the
change in average cell size accordingly from 450 charcoal filler is incorporated with the PU foam. This
m, 400 m, 380 m to 300 m. region indicates the hydrogen-bonded O-H stretch
as noted it may obscure other peaks in this region.
Particularly, the newly marked peak in this region
which lays in the range of 2820-2780 show the
functional group, N-CH3 the methylamino radical.
Cont rol
2517.84
2951.57 2168.61 928.80
3632.51
3313.78 2878.71 2028.57 1605.81
1394.21
1302.24 755.22
1709.64
2% P olyol
1517.75 1216.91 1075.77
1077.35
8% P olyol 1517.83 1217.23
2807.61 1080.46
1517.13
2987.99 2350.49 2026.18 1217.17
3631.96 3299.74 2879.04 2164.26 1604.87
1394.22
1711.02 1302.36 757.77
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650.0
cm-1
Control
2517.84
2951.57 2168.61 928.80
3632.51
3313.78 2028.57 1605.81
2878.71 1394.21
2% MDI
1517.75 1216.91 1075.77
2806.91
2987.09 2349.05 2028.38 928.42
3633.49
3303.10 2878.83 2168.08 1605.62
1394.02
1302.53 756.96
1710.84
1217.78 1080.57
8% MDI 1518.51
1517.13 1217.36
2987.28 2808.65 2347.41 2027.29 930.72
3632.01 3303.25 2879.17 2167.62 1605.09
1394.17
1302.38 1079.75 757.02
1709.94
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650.0
cm-1
Fig. 8: PU foam filled with 8% charcoal filler. Fig. 9: FTIR spectrum of Control PU foam and 1st
3.5. Fourier transform infrared spectroscopy (FTIR) batch charcoal filler mixed composite foam
7
the charcoal filler 2% and 4% f filler content the References
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Acknowledgment polyurethane foams reinforced with fillers:
microspheres and nanoclay. International
I would like to express my deepest gratitude to Journal of Polymer Science, 2012.
my project supervisor Dr. Firuz Zainuddin for
opportunities she had gave me to learn and to
complete the project under her supervision. I also
would like to thank both the master students under
my supervisor Suhaili and Hazmi for their guidance
that really helped me in solving most of the problem
on the study.