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<div class="articledetails article-header clearfix">
<p class="art-type">Research Article</p>
<p class="art-title">Effect of pyrolysis temperature on gas permeation
characteristics of poly(p-phenylene oxide) derived
hollow fiber carbon membranes</p>
<p class="art-author"><?php $authors="Jaya M.A.T<sup>1,2</sup>, Harun W.M.H.W<sup>1</sup>, Yusop M.F.M<sup>1</sup>, Ismail A.F<sup>3</sup> and Mohd Azmier Ahmad<sup>1,4*</sup>"; echo (stristr($authors,$coauthor))?str_replace($coauthor,"<a href='".$extpath."authors/".$courl."' target='_blank'>".$coauthor."</a>",$authors):$authors; ?></p>
<p class="art-affl">
<sup>1</sup>School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia<br>
<sup>2</sup>Membrane Science and Technology Cluster, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia<br>
<sup>3</sup>Advanced Membrane Technology Research Centre, Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia<br>
<sup>4</sup>Solid Waste Management Cluster, Science & Engineering Research Centre, Engineering Campus, Universiti Sains Malaysia, Nibong
Tebal, Penang, Malaysia</p>
<p class="art-aff"><b>*Corresponding author: <?php $corresponding_author="Mohd Azmier Ahmad"; echo ($coauthor!="" && $coauthor==$corresponding_author)?"<a href='".$extpath."authors/".$courl."' target='_blank'>".$coauthor."</a>":$corresponding_author;?></b>, Associate Professor, School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 NibongTebal, Penang, Malaysia, E-mail: <a href="mailto:chazmier@usm.my">chazmier@usm.my</a>
</p>
<p class="art-aff"><b>Received:</b> February 24, 2017 <b>Accepted:</b> March 31, 2017 <b>Published:</b> April 7, 2017</p>
<p class="art-aff"><b>Citation: </b> Jaya MAT, Harun WMHW, Yusop
MFM, Ismail AF, Ahmad MA. Effect of pyrolysis
temperature on gas permeation characteristics
of poly(p-phenylene oxide) derived hollow
fiber carbon membranes. <i>Int J Petrochem Res.</i> 2017; 1(1): 12-14. doi: <a href="https://doi.org/10.18689/ijpr-1000103">10.18689/ijpr-1000103</a></p>
<p class="art-aff"><b>Copyright:</b> &copy; 2017 The Author(s). This
work is licensed under a Creative Commons
Attribution 4.0 International License, which
permits unrestricted use, distribution, and
reproduction in any medium, provided the
original work is properly cited.</p>
<p><a href="<?php echo $extpath;?><?php echo $jres['journal_link'];?>/ijpr-1000103.pdf" class="btn btn-danger pull-right" target="_blank">Download PDF</a></p>
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<div class="articlecontent">
<p class="art-subhead">Abstract</p>
<p class="art-para">Hollow fiber carbon membranes derived from poly(p-phenylene oxide) were
subjected to different pyrolysis temperatures and their corresponding gas permeation
characteristics were studied. Carbon membrane produced using pyrolysis temperature
of 500&#176;C was low in H<sub>2</sub>, O<sub>2</sub>, N<sub>2</sub> and CH<sub>4</sub> permeabilities, as well as H<sub>2</sub>/N<sub>2</sub> and O<sub>2</sub>/N<sub>2</sub> ideal
selectivities. The highest permeabilities and ideal selectivities were obtained at 600&#176;C. Different trend was shown by the CO<sub>2</sub> permeability which increased with pyrolysis
temperature before decreased at 700&#176;C. The CO<sub>2</sub>/CH<sub>4</sub> ideal selectivity consistently
increased with increasing pyrolysis temperatures.</p>
<p class="art-para">Keywords: Poly(p-phenylene oxide), Hollow fiber, Carbon membrane, Pyrolysis temperature, Gas separation.</p>
<p class="art-subhead">Introduction</p>
<p class="art-para">Carbon membranes possess the capability of discriminating gas molecules with
similar kinetic diameters such as O<sub>2</sub> and N<sub>2</sub> <a href="#1">[1]</a>. This feature has attracted many researchers
to investigate and further develop the carbon membranes into commercially acceptance. Currently, the carbon membrane development focuses on finding new precursors and
modification of the existing precursors. The precursors were mostly polyimides which is
economically unattractive, thus non-polyimide polymers such as phenolic resin <a href="#2">[2]</a>, cellulose acetate <a href="#3">[3]</a> and poly(furfuryl alcohol) <a href="#4">[4]</a> were extensively introduced. The
current study reports interesting findings on the ideal gas separation characteristics of
hollow fiber carbon membrane produced from poly(p-phenylene oxide) (PPO) using
different pyrolysis temperature.</p>
<p class="art-subhead">Methods</p>
<p class="art-para">The hollow fiber PPO and carbon membranes were synthesized according to the
previous work <a href="#5">[5]</a>. Heat treatments which were thermostabilization and pyrolysis, were
applied to convert the PPO membrane into carbon membrane. The thermostabilization
temperature was 240&#176;C and held for 1 hour before proceeding to pyrolysis treatment at
varied temperatures. A constant pressure/variable-volume system and a soap-bubble
flow meter were used to measure the membrane flow rate. The membrane module was open/close-ended in which gas was fed from the membrane
bore side. The order of the feed was H<sub>2</sub>, N<sub>2</sub>, CO<sub>2</sub>, CH<sub>4</sub> and CO<sub>2</sub>
to prevent strong adsorbing gases from influencing the
measurement of the proceeding gases <a href="#6">[6]</a>. The morphology of
the carbon membrane was captured using scanning electron
microscope (SEM, Model Quanta FEG 450, FEI, USA).</p>
<p class="art-subhead">Results and discussions</p>
<p class="art-para">Fig. 1 (a&#8211;b) and (c&#8211;d) shows the cross-sectional morphology
of PPO and carbon membranes, respectively. Both membranes
exhibited homogeneous, symmetric, and nonporous structure. The PPO and carbon membranes were approximately 15.4 and
14.7 &#181;m thick. The non-porous structure of the PPO membrane (PPOM) stemmed from the delayed phase inversion between the
polymer solution and ethanol bore fluid and bath. The diameter
and thickness of the membrane decreased after pyrolysis because
of thermal shrinkage and decomposition. The change in surface
morphology also suggested structure rearrangement during
pyrolysis.</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-103.g001.gif" class="img-responsive center-block"/></div>
<p class="text-center"><b>Figure 1: </b> SEM images of cross-sectional views of PPO membrane (a, b) and carbon membrane (c, d)</p>
<!-- Table -->
<p class="art-para">Figure 2 shows the permeabilities of H<sub>2</sub>, CO<sub>2</sub>, O<sub>2</sub>, CH<sub>4</sub> and
N<sub>2</sub> for carbon membranes pyrolyzed at 500&#176;C (CM500), 600&#176;C (CM600) and 700&#176;C (CM700) with heating rate and thermal
soak time of 1&#176;C/min and 15 mins, respectively. PPOM
permeabilities was included for comparison purpose. The
permeabilities of H<sub>2</sub>, O<sub>2</sub>, N<sub>2</sub> and CH<sub>4</sub>dropped significantly
when the sample was pyrolyzed to 500&#176;C. Similar trend was
followed by their corresponding ideal selectivities of O<sub>2</sub>/N<sub>2</sub>
and H<sub>2</sub>/N<sub>2</sub>. In contrast, the CO<sub>2</sub> permeability and CO<sub>2</sub>/CH<sub>2</sub>
ideal selectivity increased. As the pyrolysis temperature was
increased to 600&#176;C, all the gas permeabilities and ideal selectivities
increased significantly. The ideal separation performances of
the gases, except CO<sub>2</sub>/CH<sub>4</sub> ideal selectivity, decreased again as
the pyrolysis temperature was further increased to 700&#176;C.</p>
<p class="art-para">According to the values of permeabilities and ideal
selectivities, particularly O<sub>4</sub>/N<sub>4</sub>, of the hollow fiber carbon
membrane, the transport mechanism of the gases was most
probably dominated by the molecular sieving in which it
suggested that the membranes possessed micropore structure
with pore size less than 2 nm <a href="#7">[7]</a> <a href="#8">[8]</a>. When the thermostabilized
PPO membrane was subjected to pyrolysis treatment, slow
decomposition of the polymer structure took place. At the
same time, thermal shrinkage and structural rearrangement
also occurred. The amorphous structure originated from the
thermostabilized PPO membrane gradually collapsed during
the pyrolysis and chaotically rearranged as amorphous
carbon.<br>
<br>
At 500&#176;C the decomposition was not sufficient to develop
highly porous membrane structure and the newly-developed
pores were constantly decreased in size due to the thermal
shrinkage. The decomposition to thermal shrinkage ratio
might have increased significantly at pyrolysis temperature of
600&#176;C as suggested by the substantial increases of the gas
permeabilities. The decomposition rate reduced as the
decomposable structure of the membrane not much left, resulting the dominance of structural densification when the
pyrolysis temperature was further increased to 700&#176;C. The
pores of carbon membrane might have collapsed and given
away for the initiation of carbon graphitization which had
higher density, tighter packaging and higher ordered structure
<a href="#9">[9]</a>. </p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-103.g002.gif" class="img-responsive center-block"/></div>
<p class="text-center"><b>Figure 2: </b> Permeabilities and ideal selectivities of PPO (PPOM) and
PPO-derived hollow fiber carbon membrane (CM500, CM600 and
CM700) prepared at different pyrolysis temperatures</p>
<!-- Table -->
<p class="art-para">The slightly higher CO<sub>2</sub> permeabilities than their H<sub>2</sub>
counterparts as shown by the CM500 and CM700 indicated
the presence of surface diffusion as one of the contributing
transport mechanism besides molecular sieving effect. The
lower H<sub>2</sub> permeability on both membranes indicated that the
resistance into the membrane was high most probably due to
smaller openings than that of CM600. At the same time, this
pore resistance also accelerated the accumulation of the
highly adsorbable CO<sub>2</sub> at the narrow opening which eventually
provided suitable environment to produce surface diffusion
effect that increased the CO<sub>2</sub> permeability.<br>
<br>
The affinity between the CO<sub>2</sub> and carbon membrane pore
wall suggested that kinetic diameter was not the sole factor in
determining the magnitude of the gas permeabilities, but also
the affinity of the diffusing molecules towards the carbon
membrane pore wall <a href="#10">[10]</a>. This affinity is originated from the van der Waal's forces produced by quadrupole moment of
the symmetrical CO<sub>2</sub> that established weak attraction towards
the carbon pore walls which occupied with delocalized
electrons from its turbostratic structure.</p>
<p class="art-subhead">Conclusion</p>
<p class="art-para">The morphology of the PPO-derived hollow fiber carbon
membrane was dense, homogenous, thin and symmetric. Each stage of pyrolysis temperature has significant impact on
the PPO-derived carbon membrane structures. The highest
permeabilities and ideal selectivities were obtained at 600&#176;C. In exception of CO<sub>2</sub> permeability and CO<sub>2</sub>/CH<sub>4</sub> ideal selectivity, all permeabilities and ideal selectivities were very low when
pyrolysis temperature of 500&#176;C was used. The transport
mechanism through the carbon membranes was highly
affected by molecular sieving and surface diffusion. The
surface diffusion transport mechanism was highly dominating
when the carbon membranes possessed very small pore sizes.</p>
<p class="art-subhead">Acknowledgements</p>
<p class="art-para">The authors are grateful for the funding from Solid Waste
Management Cluster (1001/CKT/870023), Membrane Science
and Technology Cluster (1001/PSF/8610011), Postgraduate
Research grant of Universiti Sains Malaysia and Mybrain 15
fellowship of Ministry of Higher Education, Malaysia.</p>
<div style="clear:both"></div>
<p class="art-subhead">References</p>
<ol> 
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