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Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

Temperature Effect on the Characterization of Pyrolysis Products from Oil Palm Fronds A. Abdul Rahman*, N. Abdullah, F. Sulaiman School of Physics, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia *[email protected]; [email protected]; [email protected] Abstract The oil palm fronds (OPF) have the great potential in satisfying the energy demand due to its abundant availability. Due to limited usage and commercialization, lack of research work attempted on the OPF as compared with other oil palm wastes. Thermal conversion process, pyrolysis was performed on the OPF in the range between of 300-500OC for two hours at a constant heating rate of 10OC/min. The setup of fixed bed reactor and liquid collecting system was build up to collect and determine the yield of bio-char, pyrolysis oil and gases. The maximum yield of OPF bio-char was obtained at 300OC with 50.95 wt% meanwhile, pyrolysis oil yield was observed to be initially increased until the maximum yield was reached at 400OC with 47.41 wt%, and then decreased with the increment of temperature from 400-500OC. The bio-char obtained from this work consisted of high amount of HHV within the range of 18.80 to 19.40 MJ/kg, but contained high ash content with the maximum around 4.52 mf wt% after pyrolyzed at 500OC. Pyrolysis oils were found to be more acidic, higher ash content and decrement of HHV as temperature increased; furthermore, they were separated into two phases, tarry and an aqueous fraction. Keywords Oil Palm Fronds; Pyrolysis; Bio-Char; Pyrolysis Oil

Introduction The oil palm fronds (OPF) are harvested annually about 24.4 million metric tons in Malaysia from its quarter millions hectare of oil palm fields [Bengaly, Liang, Jelan, Ho and Ong, 2010]. However, the OPF has a very limited usage and research work as compared to the other oil palm wastes such as empty fruit bunches (EFB) and oil palm shell (OPS). The OPF is usually decomposed naturally on the ground for soil fertilization, erosion control and nutrient recycling [Sulaiman, T. Ahmad and Atnaw, 2011]. Energy from biomass, in particular OPF has great potential in satisfying the energy demand due to its abundant availability. Thermochemical conversion of biomass, the pyrolysis is an alternative route to overcome limited supply of fossil fuels in sustainable basis [Yan, Acharjee, 14

Coronella and Vasquez, 2009]. It is also potential as alternative to the open burning disposal of biomass to reduce air pollution nowadays. Knowledge of the major chemical components of lignocellulosic biomass is necessary to foresee the efficiency of biomass conversion process. Generally, the biomass mainly consists of three types of carbohydrate polymers, namely, cellulose, hemicelluloses and lignin [Carrier, Loppinet-Serani, Denux, Lasnier, Ham-Pichavant, Cansell and Aymonier, 2011]. These components have influence on their chemical reactivities respectively. Knowing deeper into these three major complex lignocellulosic compositions could expose the better understanding on commercialization in converting biomass into sustainable fuels or valuable chemical products usage. The OPF has been reported consisting of 38.8% cellulose, 36.4% hemicelluloses and 19.3% lignin [Khor and Lim, 2006]. Various biomasses have different lignocellulosic wastes structure and composition as presented in Table 1. This inconsistency of biomass chemical composition could lead to unpredictable final yield of pyrolysis during thermal degradation process respectively. TABLE 1 THE CHEMICAL COMPOSITION OF VARIOUS TYPES OF BIOMASS

Biomass

References

Khor and Lim, [2006] Rice husks Li et al. [2011] Corn Stover Mullen et al. [2010] Corn cobs Soft-wood Garcia-Perez Hard-wood et al. [2007] OPF

Chemical Composition (wt%) Cellulose Hemi-celluloses Lignin 38.8

36.4

19.3

35.86 47.5 29.8 19.0 40.1

18.20 28.6 38.3 18.9 27.8

24.52 6.3 3.3 44.8 23.1

The pyrolysis system designs and operating conditions are few clear factors influencing thermal conversion process respectively. These factors effected the optimum production of pyrolysis yields (bio-char, bio-oil and gas) and its characteristics. A simple pyrolysis design consisted of fixed bed reactor and two condensers for liquid collection were used by Natarajan and GanapathySundaram [2009] in obtaining optimum process conditions for maximizing the liquid yield of

Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

the rice husk. The design has produced maximum liquid yield of 31.78% at the optimum condition. The optimum operating conditions of pyrolysis were 500OC, heating rate of 60OC/min and the reactor length of 300 mm. However, the pyrolysis liquid obtained from their work required some upgrading to improve its stability and heating values. Addition of N2 gas flow and ice-cooled trapper was purposed by Ertas and Hakki Alma [2010] for fixed bed reactor and liquid collecting system to produce and characterize the biochar and bio-oil from laurel (Laurusnobilis L.). Based on their results, the maximum bio-oil yield was found to be around 21.91% at optimum pyrolysis temperature of 500OC under flow rate of gas N2 about 100 mL/min. However, bio-char yield decreased with increasing temperature. The flow of nitrogen is mainly regarded as sweeping gas and beneficial to remove the pyrolysis volatiles where secondary reactions such as thermal cracking and repolymerization took place. The pyrolysis vapours are highly condensed at low purge of nitrogen around 50 and 100 mL/min, but started to decrease with increase in flow rate up to 400 mL/min. The possible reason to have such situation was due to insufficient cooling apparatus used throughout the experiment. No clear distinction on bio-char yield under influenced of nitrogen flow rate from 100-400 mL/min since only 28.48 to 27.21wt% was observed. The bio-oil and its fraction were characterized and found to have high potential as transport fuels, while the porosity of bio-char increased with pyrolysis temperature. Abdullah and Bridgwater [2006] have performed fast pyrolysis experiment in a fluidized bed pyrolysis system which consists of three main parts which are feeder, reactor and condensate collection. The fluidizing gas (N2) was flown through the char into char pot while the vapours were condensed along the liquid collecting systems. Presence of electrostatic precipitator (EP) in the cooling systems could trap and capture the vapours effectively. In the research, optimum organic liquid yields obtained were about 55.15 mf wt% at fluidized bed temperature of 450OC with residence time of 1.03s. However, the obtained liquid existed in two forms which are viscous tar and aqueous liquid. The liquid could be upgraded either with chemical solvent or to pre-treat the feedstock with water or acid before being pyrolysed to increase the liquid homogeneity. Materials and Methodology Raw Material The OPF was used in this study and collected from the

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oil palm field in NibongTebal, Penang, Malaysia. Prior to the experiments, the OPF was oven dried by conventional oven at 105OC until moisture content was approximately less than 10 mf wt%. The purpose of drying process was to prevent the growth of microorganism or fungus [Sulaiman and Abdullah, 2011]. OPF was then cut into small piece around 6–8 cm in length as in Fig. 1 before packed and stored for further analysis.

FIG. 1 SMALL PIECES OF FRESH OPF

Experimental The pyrolysis of OPF was conducted using the fixed bed reactor consisting of cylindrical stainless-steel pyrolyzer and equipped together with the liquid collecting system. The pyrolyzer with length of 15 cm and an internal diameter of 6.5 cm, was heated externally in a muffle furnace. Bio-char from each pyrolysis was collected from the pyrolyzer, meanwhile, pyrolysis oil was obtained from the collective of condensate gases in the oil pot. Vapours emission from pyrolysis process was condensed along the liquid collecting system. Features of a condenser, electrostatic precipitator (EP) and cotton wool filter could produce greater collection of liquid yield. In this work, the heating rate of 10OC/min was kept constant throughout the experiments. Bunch of OPFs was packed inside the pyrolyzer as compact as possible to minimize any presence of air. The OPF was pyrolyzed initially at 300OC until final temperature of 500OC for two hours respectively. The weight of dry raw OPF used was determined for pyrolysis yield calculation. The bio-char was weighed after the pyrolyzer was cooled for at least 24 hours in desiccators, but the pyrolysis oil was determined immediately after each pyrolysis. Non-condensable gas was just allowed to release or flow outside the workstation through fume cupboard. In this work, all the yields were calculated basically on dry basis, and each yield basically averaged at least on three times of

15

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Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

experiment. The percentage of char and liquid yields were defined as [Khor, Lim and Zainal Alimuddin, 2010]: 𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤ℎ𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡ℎ𝑎𝑎𝑎𝑎/𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙 (𝑔𝑔) × 100% 𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤ℎ𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 (𝑔𝑔)

Since non-condensable gas not experimentally measured, percentage of gas was calculated from the difference between percentage of char and liquid yields from the total percentage of 100%. Raw, Bio-Char and Pyrolysis Oil of OPF Analysis

Thermogravimetric analysis of raw OPF was performed by using thermogravimetricanalyzer (Perkin-Elmer Pyris 1). Basically, this analysis was applied to determine thermal degradation behaviour of biomass weight to the changes in temperature. Structure degradation of OPF could be presented and analyzed in such two ways; based on the thermogravimetric (TG) and derivative thermogravimetric (DTG) curves. Proximate analysis, ultimate analysis and higher heating value (HHV) were done to define the optimum quality of pyrolysis products. These analyses are employed on the raw, bio-char and pyrolysis oil of OPF according to the ASTM standard procedures. The HHV of raw and pyrolysis products of OPF were determined using adiabatic bomb calorimeter, Nenken 1013-B. Proximate analysis was experimentally done on raw and bio-char of OPF covering studies of moisture content (MC), ash content (AC), volatile matter (VM) and fixed carbon (FC). Furthermore, ultimate analysis basically determined the elementals

composition of raw OPF, carbon (C), hydrogen (H), nitrogen (N), sulphur (S) and oxygen (O) contents. Elemental contents were analyzed by Perkin Elmer 2400 Series II CHN Elemental Analyzer. Percentages of those elements were determined by peak areas as identified in reference to standard calibration [Sukiran, Loh, Abu Bakar and Choo, 2011]. For pyrolysis oil, digital pH meter, Acumet AB 15/15+ bench-top meter, was prepared to measure the pH value of each produced pyrolysis liquid. Finally, the ash content of pyrolysis liquid was analyzed by following standard test method, ASTM D 482-07. Moisture free weight percent (mf wt%) represented the unit for most product composition value especially in proximate and ultimate analysis. Results and Discussions Fig. 2 shows the representative profiles of TG and DTG on OPF. Generally, it is assumed that biomass consists of three major components; cellulose, hemicelluloses and lignin. Thermogravimetric analysis could distinguish the temperature range of each component to be decomposed. The heat started to propagate at 30OC until the end of devolatization process around 700OC under heating rate of 10OC/min. First drop of weight loss of OPF is seen on TG curve at 100OC, which is mainly due to the removal of inherent moisture within the biomass. Decomposition of hemicellulose and cellulose is expected to occur in temperature range of 200-400OC, meanwhile lignin is decomposed throughout the temperature range 0.08

120

Weight Loss (wt%)

0.06

TG

80

0.05

DTG

0.04

60

0.03

40

0.02 20

0.01

0

0.00 0

100

200

300

400

500

600

Temperature (oC) FIG. 2 THE TG AND DTG PROFILES FROM THERMOGRAVIMETRIC ANALYSIS OF OPF

16

Derivative Weight Loss (wt%/min)

0.07

100

Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

between 200-900OC [Khor, Lim, Zainal and Mah, 2008]. Two distinct peaks are seen at temperatures around 280OC and 320OC which highly correspond to decomposition of hemicelluloses and cellulose. Both peaks are located in two main regimes of weight loss as mentioned by Khor et al. [2009]. The lower temperature regime (200-300OC) is correlated with hemicelluloses decomposition while the upper temperature regime (300-400OC) with cellulose decomposition. Omar et al. [2011] also agreed with these regimes by mentioning that hemicelluloses degraded at lower temperature compared to cellulose. Devolatization process is considered complete at a temperature of 600OC as weight loss of OPF is almost constant, and the residue left is about 25 wt%. TABLE 2 THERMOCHEMICAL CHARACTERISTICS OF

Analysis Proximate (mf wt%) Moisture Ash Volatile Matter Fixed Carbon Ultimate (mf wt%) Carbon Hydrogen Nitrogen Sulphur Oxygen Heating Value (MJ/kg) HHV

OPF

OPF 3.82 4.20 76.26 19.54 43.35 4.71 0.38 0.37 51.19 15.78

Table 2 summarises the main thermochemical characteristics of OPF. The OPF has high percentage of volatile matter around 76.26 mf wt% which is close to those obtained in previous study as reported by

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Trangkaprasith and Chavalparit [2011] with 72.53 wt% and Xiao and Andresen [2011] with 70.2 wt%. Ash content of OPF is considerably low around 4.20 mf wt% as compared with other oil palm wastes such as EFB with 5.43 wt% [Sia, Lim and Teng, 2009] and OPS with 6.7 wt% [Kim, Jung and Kim, 2010]. High volatility and low amount of ash are desirable for thermal conversion process in order to release more vapours emission while producing remain solid residue (char) with less ash, high fixed carbon and enhancing the heating value of products. Furthermore, the HHV of OPF is considerably 15.78 MJ/kg. This is probably due to high amount of oxygen content in OPF. It is necessary to remove oxygen which leads to presence of oxygenated liquid products after pyrolysis reactions for obtaining higher fuel grade product. The amount of nitrogen and sulphur is small, therefore OPF is environmental friendly and suitable to be feedstock especially for thermochemical conversion process. The pyrolysis was performed on OPF between 300500OC under heating rate of 10OC/min. The reaction proceeds at different temperatures to obtain optimum pyrolysis yield of bio-char, pyrolysis oil and gases. Fig. 3 presents the distribution of pyrolysis yield at different temperatures. The highest production of biochar was obtained at temperature of 300OC with 50.95 wt% while the lowest bio-char yield was produced around 28.28 wt% at temperature of 500OC. Such trend of bio-char yield is similar to that reported by previous research [Sukiran, Loh, Abu Bakar and Choo, 2011; Capunitan and Capareda, 2012]. The maximum biochar yield was obtained at lower temperature probably

70

Pyrolysis Yield (wt%)

60

Bio-Char (± 1.01 - 2.04 wt%)

Pyrolysis Oil (± 0.74 - 2.71 wt%)

Gas (± 0.68 - 1.48 wt%)

50 40 30 20 10 0 300

350

400

450

500

Temperature (OC) FIG. 3 THE PYROLYSIS YIELD OF OPF AT DIFFERENT TEMPERATURE

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Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

80

19.5

70

19.4

60

HHV VM

50

AC

40

FC

19.3 19.2 19.1 19.0 18.9

30

18.8

20

18.7

10

18.6

0

18.5 300

400

High Heating Value (MJ/kg)

Weight Percent (mf wt%)

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500

Temperature

(OC)

FIG. 4 HHV, VM, AC AND FC OF OPF BIO-CHAR AT DIFFERENT TEMPERATURES

due to incomplete decomposition of OPF structure. Then, decomposition of hemicelluloses, cellulose and lignin was gradually enhanced as the temperature was increased up to 500OC. The relationships between the pyrolysis oils with increment of temperature were observed and the yield increased and reached the maximum at 400OC, but then decreased after being further pyrolyzed to 500OC. Maximum pyrolysis oil is found at 400OC with 47.41 wt%. The decrease in liquid at higher temperature might be due to secondary cracking of the pyrolysis oil into gaseous products. Increment of temperature has made the rate of thermal cracking reaction of the pyrolysis vapours become faster, thus resulting in the release of high non-condensable compounds. Volatile matter (VM), ash content (AC), fixed carbon (FC) and higher heating value (HHV) of OPF bio-char wereanalyzed to evaluate the optimum quality. The bio-char collected from pyrolysis at 300, 400 and 500OC were chosen to examine the effect of temperature variations. Fig. 4 shows the HHV, VM, AC and FC of bio-char at different temperatures. The VM of the biochar decreased from 46.29 mf wt% to 25.05 mf wt% as temperature increased. Significantly, the VM in those bio-chars was lower than that in dry raw OPF, and mostly possible due to derivation of constituents in the biomass. AC was found highest for bio-char pyrolyzed at 500OC with 4.52 mf wt% as compared with other bio-char at 300OC (2.34 mf wt%) and 400OC (4.00 mf wt%). This trend might occur due to the reduction of elements composition such as carbon, nitrogen, hydrogen and nitrogen contents. These elements lose 18

their bonding easier as compared to volatize inorganic salts, thus contributing to high AC percentage at higher temperature [Maiti, Dey, Purakayastha and Ghosh, 2006]. Presence of high AC was not preferable in bio-char. It may reduce the heating value owned by bio-char, thus impotency for solid fuel applications. The highest HHV of bio-char was observed at 300OC with 19.37 MJ/kg, but then started to decrease as temperature increased. No significant difference was seen as compared with other bio-char, but clear distinction was found when compared with dry raw OPF (15.78 MJ/kg). FC could be referred to as remained constituents after the release of volatiles. From the results, fixed carbon content of bio-char was approximately around 51.37 mf wt% at 300OC, but then increased up to 60.45 mf wt% and 70.43 mf wt% at 400OC and 500OC. Haiqing and Kuichuan [2012] found an intercorrelation between VM and FC and indicated that gasification of VM at high temperature will lead to the increase of FC content. TABLE 3 PROPERTIES OF PYROLYSIS OIL FROM

OPF AT DIFFERENT

TEMPERATURES

Properties Odour Colour pH Ash (mf wt%) HHV (MJ/kg)

300OC Acrid smoky Black 2.60 0.35 19.84

400OC Acrid smoky Black 2.01 0.40 19.82

500OC Acrid smoky Black 1.98 0.52 19.79

The characteristics of pyrolysis oil from OPF at different temperatures are presented in Table 3. Pyrolysis oils collected from the oil pot were seen nonhomogenous at room temperature with two fractions, oily brownish aqueous phase and viscous tar. Presence

Advances in Energy Engineering (AEE) Volume 2 Issue 1, January 2014

of oxygenated compound could cause the pyrolysis oil to be separated from hydrocarbons [Khor, Lim, Zainal and Mah, 2008]. Thus, upgrading is needed to remove the oxygen and enhanced the pyrolysis oil composition. Abdullah et al. [2011] hasproposed that an addition of polar solvents (methanol or ethanol) could dissolve two phases pyrolysis oil into homogeneous single– phase product with less viscosity and corrosivity. The pH values of the pyrolysis oil ranged between 1.90 and 2.60. Trend of pH value was observed with the most acidic pyrolysis oil obtained at the highest temperature of 500OC with 1.98, and followed by pyrolysis oil of 400OC and 300OC pre of 2.01 and 2.60 respectively. The acidic content in pyrolysis oil could comprise mainly organic acids, such as acetic and formic acids. Chemical treatment is needed to lower the acidity. The treatment is suggested to prevent corrosive on mild steel and aluminium, especially during power generation in engine and turbine [Asadullah, Rahman, Ali, Rahman, Motin, Sultan and Alam, 2007]. The ash content of the pyrolysis oil was found to increase with the temperature: 0.35 mf wt% at 300OC, 0.40 mf wt% at 400OC and 0.52 mf wt% at 500OC. Ash probably flew and condensed together during the release of pyrolysis vapours. This mixture was effectively captured when passing through electrostatic precipitator (EP), and then accumulated and mixed in the oil pot after running down the walls of the EP [Abdullah, Gerhauser and Bridgwater, 2007]. Low amount of ash was really necessary in pyrolysis oil to prevent serious problems, such as erosion, corrosion and gumming problems, in theengine valves respectively [Capunitan and Capareda, 2012]. The HHV was found to be decreased in pyrolysis oil as temperature increased. The pyrolysis oil at 300OC has the highest amount of HHV with 19.84 MJ/kg, while others with 19.82 MJ/kg (400OC) and 19.79 MJ/kg (500OC). However, measured HHV in this work has no obvious distinction between each other at different temperature. These pyrolysis oils just have slightly lower HHV as compared to palm shell (22.1 MJ/kg) and wood (22.124.3 MJ/kg) pyrolysis oil [Islam, Zailani and Ani, 1999], and twice lower as compared to the HHV of diesel (45.00 MJ/kg) [Chaiya, 2011]. Conclusions Pyrolysis of OPF at different temperatures (300, 400 and 500OC) in a fixed bed reactor gave significant variation in the distributions of pyrolysis product (biochar, pyrolysis oil and gases). The highest production of bio-char was obtained at temperature of 300OC with

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50.95 wt% and then started to decrease as temperature increased. High amount of ash measured with increasing temperature could reduce the heating values owned in bio-char. Meanwhile, the pyrolysis oils yield increased and reached maximum value at 400OC with 47.41 wt%, but then decreased after being further pyrolyzed to 500OC. Pyrolysis oils were separated into two phases, tar and aqueous, and upgrading or blending with polar solvents was able to form homogeneous single-phase pyrolysis oil. The HHV of bio-char and pyrolysis oil were measured within the range of 18.86-19.84 MJ/kg, and classified as potential to be used for solid and liquid fuel applications. ACKNOWLEDGEMENT

The authors would like to thank the UniversitiSains Malaysia, Penang by providing the research university grant (1001/PFIZIK/814087) and short term grants (304/ PFIZIK/6310073, 304/PFIZIK/6310087 and 304/PFIZIK/ 6311063) that has made this study possible. REFERENCES

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properties affected by different pyrolysis temperature using visible-near-infrared spectroscopy.” International Scholarly Research Network 2012, doi:10.5402/2012/ 712837. Aizuddin Abdul Rahman received the B. Applied Science degree (Engineering Physic) and M. Science degree (Solid State Physics) from UniversitiSains Malaysia (USM), Penang, Malaysia, in 2009 and 2010 respectively. He is currently a PhD student in energy studies, at USM, with research interest basically in thermochemical energy conversion of biomass for its solid and liquid fuel application. Nurhayati Abdullah received the B. Science degree in Physics and M. Science degree in Solid State Physics from National University of Malaysia (UKM), Selangor and UniversitiSains Malaysia (USM), Penang, Malaysia, in 1987 and 1992, and owned the PhD degree in Chemical

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Engineering from Aston University, Birmingham, United Kingdom in 2005. She has been an academic staff for almost 20 years and recently as senior lecturer in the School of Physics, USM. She has great research intention in energy studies related to research areas including pyrolysis, biomass and bio-energy. FauziahSulaiman received the B. Science degree in Physics from Western Michigan University, Michigan, United State of America (USA) in 1981 and owned M. Science degree in Physics and PhD degree in Mechanical Engineering from Michigan State University, Michigan, USA, in 1985 and 1989 respectively. She is currently an Associate Professor and has been an academic staff for almost 23 years in School of Physics, UniversitiSains Malaysia. Her interest research area includes solar thermal, biomass and bio-energy. She has also published more than 40 research papers, and experience with written and edited chapters in research books.

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