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This article was downloaded by: [New York University] On: 02 June 2015, At: 16:51 Publisher: Taylor & Francis Informa Ltd Registered in England and Wales Registered Number: 1072954 Registered office: Mortimer House, 37-41 Mortimer Street, London W1T 3JH, UK Energy Sources, Part A: Recovery, Utilization, and Environmental Effects Publication details, including instructions for authors and subscription information: http://www.tandfonline.com/loi/ueso20 Fast Pyrolysis of Spent Coffee Waste and Oak Wood Chips in a Micro-tubular Reactor a b c T.-A Ngo , J Kim & S.-S Kim a Department of Chemical Engineering, Ho Chi Minh City University of Technology, Ho Chi Minh City, Vietnam b Department of Chemical Engineering, Kyung Hee University, Yongin, Gyeonggi-do, Korea c Click for updates Department of Chemical Engineering, Kangwon National University, Samcheok, Gangwon-do, Korea Published online: 28 Apr 2015 To cite this article: T.-A Ngo, J Kim & S.-S Kim (2015) Fast Pyrolysis of Spent Coffee Waste and Oak Wood Chips in a Micro-tubular Reactor, Energy Sources, Part A: Recovery, Utilization, and Environmental Effects, 37:11, 1186-1194, DOI: 10.1080/15567036.2011.608779 To link to this article: http://dx.doi.org/10.1080/15567036.2011.608779 PLEASE SCROLL DOWN FOR ARTICLE Taylor & Francis makes every effort to ensure the accuracy of all the information (the “Content”) contained in the publications on our platform However, Taylor & Francis, our agents, and our licensors make no representations or warranties whatsoever as to the accuracy, completeness, or suitability for any purpose of the Content Any opinions and views expressed in this publication are the opinions and views of the authors, and are not the views of or endorsed by Taylor & Francis The accuracy of the Content should not be relied upon and should be independently verified with primary sources of information Taylor and Francis shall not be liable for any losses, actions, claims, proceedings, demands, costs, expenses, damages, and other liabilities whatsoever or howsoever caused arising directly or indirectly in connection with, in relation to or arising out of the use of the Content This article may be used for research, teaching, and private study purposes Any substantial or systematic reproduction, redistribution, reselling, loan, sub-licensing, systematic supply, or distribution in any form to anyone is expressly forbidden Terms & Downloaded by [New York University] at 16:51 02 June 2015 Conditions of access and use can be found at http://www.tandfonline.com/page/termsand-conditions Energy Sources, Part A: Recovery, Utilization, and Environmental Effects, 37:1186–1194, 2015 Copyright © Taylor & Francis Group, LLC ISSN: 1556-7036 print/1556-7230 online DOI: 10.1080/15567036.2011.608779 Fast Pyrolysis of Spent Coffee Waste and Oak Wood Chips in a Micro-tubular Reactor T.-A Ngo,1 J Kim,2 and S.-S Kim3 Downloaded by [New York University] at 16:51 02 June 2015 Department of Chemical Engineering, Ho Chi Minh City University of Technology, Ho Chi Minh City, Vietnam Department of Chemical Engineering, Kyung Hee University, Yongin, Gyeonggi-do, Korea Department of Chemical Engineering, Kangwon National University, Samcheok, Gangwon-do, Korea Fast pyrolysis of spent coffee waste, a major non-cellulosic material, and oak wood chips, a cellulosic material, was carried out in a micro tubular reactor over a temperature range of 550 to 750°C with sweep gas flow rates of 20 and 500 mL/min When the temperature was raised from 550 to 750°C, the gas yields were significantly enhanced, but the liquid yields were reduced The highest liquid yield, 63.4 wt%, was obtained after pyrolysis of spent coffee waste at 550°C at a sweep gas rate of 500 mL/ The highest gas yield, 65.74 wt%, was obtained after pyrolysis of the oak wood chips at 750°C at a sweep gas flow rate of 20 mL/min The gas products primarily included considerable amounts of CO, CO2, and hydrocarbon-rich gases but no hydrogen Furthermore, regardless of the biomass source, the hydrocarbon-rich gases were qualitatively similar and largely consisted of methane, ethane, ethylene, propane, and propylene The gas chromatography-mass spectrometry analysis of the pyrolyzed bio-oils demonstrated that the major compounds were phenol derivatives, aldehydes, ketones, acids, and alcohols Keywords: biomass, cellulosic biomass, fast pyrolysis, non-cellulosic biomass, tubular reactor INTRODUCTION Recently, there has been an increased interest in studies on biomass conversion into fuel Various methods have been, such as fermentation (Lin and Tanaka, 2006), hydrolysis (Sun and Cheng, 2002), and pyrolysis (Raveendran et al., 1996; Kim et al., 2009; Kaushal and Abedi, 2010, Yu et al., 2011; Yaman, 2004) Pyrolysis is a promising method due to its reasonable cost and simple operation and can be classified into two approaches based on the heating rate and gas retention time (Bridgwater, 2003) Conventional pyrolysis involves decomposition at a low heating rate and long retention time to produce charcoal Fast pyrolysis occurs with a very high heating rate over a short retention time, largely for achieving a high yield of biological oils, known as bio-oil Since Address correspondence to S.-S Kim, Department of Chemical Engineering, Kangwon National University, Samcheok, Gangwon-do 363-883, Korea E-mail: sskim2008@kangwon.ac.kr Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/ueso 1186 Downloaded by [New York University] at 16:51 02 June 2015 FAST PYROLYSIS OF COFFEE WASTE AND OAK WOOD CHIPS 1187 bio-oil is appealing as an alternative for depleted fossil-based fuels, fast pyrolysis is receiving increasing attention Many types of reactors coupled with various biomass sources have been employed by researchers for the fast pyrolysis of biomass For instance, Lappas et al (2002) investigated the fast pyrolysis of biomass (Lignocell HBS 150–500) in a fluidized bed reactor Li et al (2004) developed a free fall reactor (a type of reactor used for fast pyrolysis) to conduct an experiment using legume straw and apricot stone to obtain a hydrogen-rich gas fraction Only a few studies, however, have been reported on fast pyrolysis in a small reactor for lab-scale applications Therefore, a micro-tubular reactor, a small apparatus with a length of 50 cm, 75% shorter than that of the free fall reactor reported in Li et al (2004), was designed and applied for fast pyrolysis in this study It should be noted that, while the major cellulosic material is the primary focus of most studies, there have been very few reports referring to the major non-cellulosic material With a diversity of starting structures, the yields as well as the product properties are expected to completely change when a particular biomass is used in fast pyrolysis Spent coffee waste is an abundant leftover non-cellulosic biomass collected from the production of the beverage, with the major carbohydrate consisting of considerable amounts of arabinogalactan and galactomannans (Fischer et al., 2001; Oosterveld et al., 2003), and was chosen for this research Furthermore, oak wood chips, typically a major cellulosic biomass material, were also pyrolyzed under the same conditions to serve as a reference of comparison Using these two biomass feedstocks, all experiments were performed at the temperature of 550–750°C in two different sweep gas flow rates of 20 and 500 mL/min to compare the gas, liquid, and char yields after pyrolysis Subsequently, the gas and liquid product properties at selected conditions were studied From these results, the role of biomass composition and the effect of pyrolysis conditions were clarified EXPERIMENTAL The spent coffee waste and oak wood chips were ground with a knife mill to ca 500 μm and then exposed to air for 24 h The samples were fast pyrolyzed in a vertical tubular reactor (ϕ2.54 cm × 50 cm), which was designed 75% shorter than the free fall reactor by Li et al (2004) For each run, a 1.5-g sample was pre-placed in the feed hopper When the set value of furnace temperature (550, 600, 650, 700, or 750°C) was reached, the on/off valve was subsequently switched on to allow both the biomass sample and sweep gas (at a flow rate of 20 or 500 mL/min) to enter the reactor The liquid product was condensed and separated from the aerosol at the bottom of the condenser (cooled with a eutectic mixture of 76.4 wt% sodium chloride and 23.6 wt% ice water at a temperature of -21.8°C), while the gas product was emitted to and trapped in the water column After being held constant for 10 min, the flow of N2 was deactivated, the oven was turned off, and the pyrolysis was completed In order to compare the characteristic of fast pyrolysis for each type of biomass, the yields of product were calculated as follows: Liquid yield ðwt%Þ ¼ Solid yield ðwt%Þ ¼ weight of liquid  100%; weight of biomas weight of solid  100%; weight of biomas Gas yield wt%ị ẳ 100% Liquid yield Solid yield; Downloaded by [New York University] at 16:51 02 June 2015 1188 T.-A NGO ET AL where the weight of liquid product was determined as the difference in the weight of the condenser before and after pyrolysis, and the weight of solid was obtained from weighted residue after pyrolysis The gaseous product of biomass pyrolysis was quantitatively characterized using gas chromatography (GC) with a flame ionization detector (FID) and thermal conduction detector (TCD) The GC-FID (M600D–Younglin) with an HP-Plot/Al2O3 column (50 m × 0.53 mm × 15 μm) was used to analyze hydrocarbons, while a GC-TCD (ACME 6000GC–Younglin) with a molecular sieve of 5A and a Porapak N column (80/100, ft × 1/8 in., HP) were used to detect CO, H2, and CO2 The liquid product was analyzed using gas chromatography-mass spectrometry (GC-MS) with an HP-1 column (50 m ì 0.32 mm ì 0.52 àm) to identify the composition (Lappas et al., 2002) The oven temperature was programmed to increase from 50 to 300°C at a heating rate of 10°C/min while the injector was maintained at 300°C The water content was analyzed using a method reported in the literature (Orzherovskii, 1969) RESULTS AND DISCUSSION Effect of Pyrolysis Conditions on Product Distribution Figure shows the product yields of fast pyrolysis for the two types of biomass Spent coffee waste was pyrolyzed for the highest liquid yield of 58.50 wt% at 550°C, compared to that of oak wood chips with a liquid yield of 52.47 wt% The gas yields from both biomasses were varied in the range of 19.20–24.86 wt%, while the char yields were not very different in this temperature range, changing from 22.30 and 24.86 wt% By increasing the pyrolysis temperature from 550 to 750°C, the major product changed from liquid to gas At 750°C, the highest yield of a gaseous product (65.74 wt%) was obtained with the pyrolysis of oak wood chips In contrast, the liquid yields were considerably decreased at this condition Generally, it can be found that the gas yields increased with increasing temperature, whereas the liquid and char yields decreased As is commonly known, cracking is an endothermic reaction; therefore, the increase in temperature could facilitate the cracking of heavy molecules to produce smaller ones As a result, the gas yield was enhanced significantly, while both liquid and char yields decreased The liquid yield of the pyrolysis of spent coffee waste only slightly decreased with an increase in temperature, whereas the liquid yield from oak wood chips was more noticeably reduced This indicated that the production of bio-oil from the pyrolysis of spent coffee waste was more thermally stable than was that from pyrolysis of oak wood chips The effect of sweep gas flow rate was investigated based on a comparison of the product yields obtained at the slow (20 mL/min) and fast flow rates (500 mL/min) at various pyrolysis temperatures, which ranged from 550 to 750°C The product yield of fast pyrolysis at these conditions is shown in Figure From Figures and 2, it can be realized that the liquid yield at a fast N2 flow rate (500 mL/min) increased in comparison with that at a N2 slow flow rate (20 mL/min) This might be because all secondary cracking reactions in the pyrolysis process were significantly decreased when the retention of vapor was reduced, thus resulting in an improved bio-oil yield and simultaneous restriction of the gas yield Unexpectedly, all char yields from the pyrolysis of the two types of biomass at a fast flow rate of N2 were also higher than those at the slower N2 flow rate This increase might be explained based on the changes in both the heat transfer and reaction pathway taking place in the pyrolysis process From the perspective of heat transfer, a higher sweep gas flow rate would facilitate greater heat transfer rates from the surface of the biomass particle to the wall of the reactor This could result in insufficient energy at the core of the biomass particle, which could hinder complete FAST PYROLYSIS OF COFFEE WASTE AND OAK WOOD CHIPS 1189 80 char liquid gas Yield, wt% 60 40 550 600 650 700 750 700 750 Temperature, ºC 80 char liq gas 60 Yield, wt% Downloaded by [New York University] at 16:51 02 June 2015 20 40 20 550 600 650 Temperature, ºC FIGURE Product yields of fast pyrolysis of biomass at 20 ml/min of N2 from 550–750°C: (a) spent coffee waste and (b) oak wood chips decomposition; therefore, a small fraction of feedstock might remain after pyrolysis As a result, the solid yield in pyrolysis with a fast flow rate of sweep gas was always higher than that of the slow sweep gas flow rate Due to the effect of reaction pathway, as reported by Liden et al (1988), biomass was pyrolyzed in two ways: one forming the mixture of tar and gas products, and another forming char Based on this reaction mechanism, when the flow rate of sweep gas is increased, the pyrolysis reaction might be altered, preferably toward the formation of char Pyrolysis Product Properties In order to investigate the effect of pyrolysis temperature, sweep gas flow rate, and biomass source on product properties, the gases obtained were analyzed using GC-FID and GC-TCD to determine the hydrocarbons and the abundances of CO, CO2, and H2, respectively The analysis results of the gas products at various conditions are presented in Figure 1190 T.-A NGO ET AL 80 (a) char liquid gas Yield, wt% 60 40 550 600 650 700 750 Temperature, ºC 80 (b) char liq gas 60 Yield, wt% Downloaded by [New York University] at 16:51 02 June 2015 20 40 20 550 600 650 700 750 Temperature, ºC FIGURE Product yields of fast pyrolysis of biomass at 500 ml/min of N2 from 550–750°C: (a) spent coffee waste and (b) oak wood chips As shown, when the temperature increased to 750°C, the yields of hydrocarbons and the mixture of CO, CO2 from both biomass types were considerably enhanced, almost two- or threefold higher than those at 550°C Specifically, for spent coffee waste at pyrolysis conditions of 550° C and 20 mL/min, the contents of hydrocarbons and the mixture of CO, CO2 were 8.45 and 10.75 wt%, respectively, while those of pyrolysis at 750°C were 26.67 and 20.44 wt% The GC-TCD analysis revealed that there was no hydrogen in the gaseous products of the pyrolysis experiments under the selected conditions As reported by Rand and Dell (2008), hydrogen-forming reactions commonly occur at elevated temperature, high pressure, and almost always with the use of catalysts In comparison with these conditions, it is obvious that the pyrolysis temperatures used in this research were not sufficient to facilitate the reactions that produce hydrogen The effect of sweep gas flow rate on fast pyrolysis is demonstrated through the reduction of gas yield, as well as the decrease in the yields of both hydrocarbon-rich gas and the mixture of CO, CO2 when the flow rate was increased Although the gas yield only slightly decreased with an increase in the sweep gas flow rate between and 15 wt% for both biomass at all temperatures, the FAST PYROLYSIS OF COFFEE WASTE AND OAK WOOD CHIPS 70 60 1191 Hydrocarbon gas CO + CO2 Yield, wt% 50 40 30 20 Downloaded by [New York University] at 16:51 02 June 2015 2 10 Spent coffee waste Oak wood chip FIGURE The yields of hydrocarbon and the mixture of CO and CO2 in gaseous products of fast pyrolysis of spent coffee waste and oak wood chips at different conditions: (1) 550°C, 20 mL/min; (2) 550°C, 500 mL/min; (3) 750°C, 20 mL/min; (4) 750°C, 500 mL/min secondary cracking reaction mentioned above was clearly retarded at the faster sweep gas flow rates, thus leading to a lower gas yield but an improved bio-oil yield Finally, the effect of biomass source can be seen in Figure 3, where the gas yields from oak wood chips as well as the yields of hydrocarbons and mixture of CO and CO2 were almost always higher than those from the spent coffee waste at all conditions investigated Additionally, regardless of the dissimilarity in structure of the major non-cellulosic and cellulosic biomasses, the hydrocarbon compositions of both gaseous products obtained from pyrolysis of spent coffee waste and oak wood chips were similar It was observed that the liquid yield, including both water and bio-oil yield, was directly proportional to the sweep gas flow rate, which was explained in the previous section After fast pyrolysis at 550°C, the water contents in the liquid products were ca 28 wt% from spent coffee waste and ca 36 wt% from oak wood chips, respectively Czernik and Bridgwater (2004) reported that the water in the liquid product was produced by the dehydration reaction, which occurred during pyrolysis The water content of oak wood chips was higher than that from spent coffee waste, although the experiments were carried out at the same conditions This difference could be attributed to the usage of a different biomass source for pyrolysis In fact, the oxygen contents of spent coffee waste and oak wood chips were 34.5 and 38.55%, respectively During pyrolysis, these oxygen atoms were eliminated from the biomass to form water Therefore, a higher oxygen content in the biomass resulted in a higher water content in the liquid product In contrast with the water content, the bio-oil content from oak wood chips was lower than that from spent coffee waste It was difficult to explain this difference in bio-oil content due to the fact that there were few factors that affect the formation of bio-oil, such as the molecular structure or relative content of each compound in the biomass (cellulose, cellulose-like, and lignin) Specifically, if these compounds contained a long chain hydrocarbon, a large amount of high molecular weight bio-oil would result In addition, lignin is known as a thermally stable compound and can be decomposed to produce phenol derivatives, a common compound of bio-oil (Wei et al., 2006) Hence, if this compound existed in abundance, it would lead to the creation of more 1192 T.-A NGO ET AL TABLE Major Bio-oil Products of the Fast Pyrolysis of Spent Coffee and Oak Wood Downloaded by [New York University] at 16:51 02 June 2015 Spent Coffee Waste 10 11 12 13 14 15 16 17 18 19 20 Oak Wood Chips Compound Area, % Compound Area,% Acetic acid 2-Propanone, 1-hydroxy1,3-Cyclopentanedione 2-Furanmethanol 3,4-Dihydropyran 2-Cyclopenten-1-one, 3-methylPhenol 2-Cyclopenten-1-one, 2-hydroxy-3-methyl Phenol, 4-methylPhenol, 2,5-dimethyl1,2-Benzenediol 4-Vinylphenol 1,4-Benzenediol Indolizine 2-Methoxy-4-vinylphenol 1,3-Benzenediol, 4-ethylPentadecane Dodecanoic acid Hexadecanoic acid 9,12-Octadecadienoic acid (Z,Z)- 5.1 2.9 5.0 4.3 2.0 1.8 3.9 2.9 3.9 1.6 6.9 1.4 2.0 3.2 2.0 1.9 1.2 3.4 10.9 7.9 Acetic acid 2-Furancarboxaldehyde 2-Furanmethanol 1,2-Cyclopentanedione 2-Furancarboxaldehyde, 5-methylPhenol 2-Cyclopenten-1-one, 2-hydroxy-3-methyl Phenol, 2-methylPhenol, 4-methylPhenol, 2-methoxy1,2-Benzenediol 1,2-Benzenediol, 3-methoxy1,2-Benzenediol, 3-methylPhenol, 4-ethyl-2-methoxy1,2-Benzenediol, 4-methyl2-Methoxy-4-vinylphenol Phenol, 2,6-dimethoxyPhenol, 3,4-dimethoxyPhenol, 2-methoxy-4-(1-propenyl)2,6-Dimethyl-3-(methoxymethyl)-p-benzoquinone 20.7 3.3 2.2 2.1 2.1 2.9 2.5 2.1 3.1 2.7 3.4 2.4 2.4 3.0 3.4 3.2 4.0 2.3 4.2 2.0 phenolic derivatives (bio-oil) Accordingly, additional measurements are needed to confirm the important factors in the bio-oil yields of these two biomass sources Table shows the major products obtained from the pyrolysis of spent coffee waste and oak wood chips As can be seen in the case of the oak wood chip sample, the bio-oil included mainly phenol derivatives As reported by Wei et al (2006), these compounds were assumed to be produced from the decomposition of lignin in the biomass As for the spent coffee waste, these phenol derivatives also existed in the liquid product but in a much smaller amount Additionally, considerable amounts of fatty acids and alkanes were detected There is no research showing that these compounds result from the pyrolysis of ligno-cellulosic biomass Such compounds must be derived from the decomposition of vegetable oil remaining in the biomass This conclusion is consistent with the mechanism for the formation of free fatty acid via pyrolysis of vegetable oil (Jayadas and Prabhakaran, 2007; Schwab et al., 1988) Furthermore, it is commonly known that hydrocarbon compounds with a higher molecular weight have a higher decomposition temperature This means that a high molecular-weight compound would be more thermally stable than a low molecular-weight compound As can be seen in the composition of bio-oil resulting from the pyrolysis of spent coffee waste, fatty acids of high molecular weight, such as dodecanoic or hexadecanoic acid (mainly including C12–C16 hydrocarbons), comprised a considerable fraction of the bio-oil These fatty acids are more thermally stable, and hence, they might remain after pyrolysis As a result, the yield of bio-oil produced from spent coffee waste was always higher than that of oak wood chips at all investigated conditions Noticeably, almost all products were oxygenated compounds The presence of these oxygen atoms in the compounds resulted in a reduced bio-oil quality An upgrading process was therefore recommended for these bio-oils before they can be used as fuel FAST PYROLYSIS OF COFFEE WASTE AND OAK WOOD CHIPS 1193 CONCLUSIONS Spent coffee waste, a major non-cellulosic biomass, and oak wood chips, a major cellulosic biomass, were employed for fast pyrolysis in a micro tubular reactor at various conditions The effects of biomass source, temperature and sweep gas flow rate on the characteristics of fast pyrolysis can be summarized as follows: ● Downloaded by [New York University] at 16:51 02 June 2015 ● ● Fast pyrolysis was preferable for the production of a liquid product at 550°C, whereas a gas product was preferable at 750°C The highest yield of bio-oil from the spent coffee waste was 58.5 wt% when the pyrolysis temperature was 550°C at 20 mL/min In contrast, at this condition, pyrolyzed oak wood chips produced the highest gas yield at 65.74 wt% Also, the char yields varied in the range of 13.73–22.67 wt% When the sweep gas flow rate was increased, the liquid yields increased, the gas yields decreased and the char yield unexpectedly increased compared to those at a slow flow rate The highest gas and liquid yields were 63.4 and 40.7 wt%, corresponding to the pyrolysis of spent coffee waste and oak wood chips, respectively Regardless of biomass composition, the gases produced were qualitatively similar, largely including carbon monoxide, carbon dioxide, methane, ethane, ethylene, propane, and propylene The major compounds of pyrolyzed bio-oils consisted of phenol derivatives, aldehydes, ketones, acids and alcohols Notably, there was a considerable amount of fatty acids in the bio-oil obtained from spent coffee waste, thus imparting greater thermal stability in this bio-oil FUNDING This research was 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Eng J 168:839–847 ... wt%, was obtained after pyrolysis of spent coffee waste at 550°C at a sweep gas rate of 500 mL/ The highest gas yield, 65.74 wt%, was obtained after pyrolysis of the oak wood chips at 750°C at a. .. Samcheok, Gangwon-do, Korea Fast pyrolysis of spent coffee waste, a major non-cellulosic material, and oak wood chips, a cellulosic material, was carried out in a micro tubular reactor over a. .. reported on fast pyrolysis in a small reactor for lab-scale applications Therefore, a micro-tubular reactor, a small apparatus with a length of 50 cm, 75% shorter than that of the free fall reactor