Bioresource Technology 209 (2016) 157-165, Comtonts sts vale at Soni — Bioresource Technology journal homepage: www.elsevier.com/locate/biortech Synergetic and inhibition effects in carbon dioxide gasification of blends of coals and biomass fuels of Indian origin Mews V. Satyam Naidu, P, Aghalayam, S. Jayanti * Department of Cheri Engnerng onl Natonal Cente for Combustion Research and Development (NECRD), MT Maas, Chen 600036, nda + Focus on role of catalytic elements in ash in enhancing COs reactivity of fuels. ‘Tends of chars of coals and biomasses of Indian origin studied experimentally * systematic reactivity studies using isothermal thermogravimetrc analysis. 1 Established synergistic effet through 90% conversion time af coal char. + Inibiton tendency noted at high temperatures fr high ash coal ARTICLE INFO AuSTRACT ‘le Neony Received 1 Janvary 2016 Received in revise form 28 February 2016 ‘Accepted 29 February 2016, ‘usb ontine 4 rch 2016 ‘The present study investigates the enhancement of CO» gasification reactivity of coals due tthe presence ‘of catalytic elements in biomass such as K0, CaO, No.0 and MgO. Co-gasifcaton of three Indian coal ‘chars with «wo biomass chats has been studied using Isothermal thermogravimetric analysis (TCA) in (CO, environment at 900, 1000 and 1100 °C. The conversion profiles have been used to establish syner- etic or inhibitory effect on coal char reactivity by the presence of catalytic elements in biomass char by comparing the 90% conversion time with and without biomass. tis concluded that both biomasses Cn ens evo en Wort th te esc wheat bng ove see Sepsitcatn than empty fat bunch. Some inhibitory effect has been noted forthe high ash coal a the highest tem _ eT oe 6201 sever Li. l ids eseved — a = There has been sustained increase over the last two centuries of atmospheric concentrations of greenhouse gases (GHGs), con- tributing to a significant rise in the global average atmospheric temperature. This is attributed to too much dependence on fossil fuels to satisfy the ever increasing demand for energy. As a recog- nition of the devastating consequences associated with global ‘warming, the recent global meet on climate change held in Paris, (www.cop2 tparis-org) declared its intention to strive toward lim- iting the rise in global temperature to well below 2°C through a concerted worldwide effort to reduce GHG emissions from anthro- pogenic sources. India, the third largest emitter of COs, has ‘declared its commitment (0 reducing CO, emissions per GDP (gross ‘domestic product) so as not to derail its economic growth, While * Goresponing author. aoe sion cin (Sayan). nap dog 10. 1016bortech 201602137 (950-8524) 2016 Elsevier Ud Al gts reserve there is less unanimity on the measures to be adopted to achieve these. Continued reliance on indigenous, coal-based power genes- ation is inevitable for the next couple of decades for many coun- ties such as India, In such a scenario, reductions in GHG emissions are possible only by resorting to more efficient use of hydrocarbon fuels for power generation. The present work is moti- vated by this objective and investigates the possiblity of blending, coal with local biomass to generate syngas, which can then be used to generate power through the more efficient combined cyele route as opposed to using the Rankine cycle ‘Biomass is considered as a carbon-neutral form of energy as the Oz released during its utilization is equal to the COs absorbed {rom the atmosphere during photosynthesis (Tilman et al, 2012; ‘Masnadi et al, 2015), Biomass gasification technologies are not viable economically due to the low energy density of biomass and the lack of assured availability. Adding coal to biomass can increase specific energy content of the product. Since biomass138 Saya Naid ta /Boresource Tecolegy 209 (2016) 157-165 has relatively small amount of ash, blending it with high ash Indian coals mitigates the ash-related problems in direct usage of coal ‘There can be benefits arising from reactivity considerations, too. In view of these factors, we consider the kinetics of co- gasification of two fast growing biomasses, namely, empty fruit bunch (EFB) and casuarina equisetfolia, with Indian high ash coals. ‘The conventional route to syngas generation from solid fuels is through steam gasification, OFlate, there has been geawing interest in CO, as the gasifying agent (Saravanan etal, 2011; Lahijani etal, 201 a,b; Naidu et al, 2016). This i partly driven by the prospect, ‘of having highly concentrated COs stream teatily available on-site ina futuristic scenario in which carbon capture and sequestration (CCS) is employed to minimize CO; emissions into the atmosphere Given India's abundance reserves of coal and seasonal availability ‘of agricultural waste in large quantities, syngas generation through co-gasifcation appears to be the most appropriate route to efficient utilization of indigenous resources. In view of this, the ‘co-gasifcation possibilities of three high ash Indian coals and two fast-growing biomasses, namely, empty fruit bunch (EFB) of, palm trees and the twigs of casuarina tree (casuarina equisetifol referred to henceforth as CE), are of interest in for the present study. Of the five solid fuels selected for the present study, EFB has been studied widely and is known to have much higher reac- tivity than coals, which is attributed to the presence of catalytic elements in ash (Mohammed et al, 2011; Lahijani et al, 2013a; Naidu et al, 2016). The other biomass considered in the present study is the fast growing tree, casuarina, found on the sea shore along the coastline of India. The needle-like twigs which are con- tinuously shed are currently used for low grade heat generation. ‘The reactivity studies of casuarina are of recent origin (Sharma fet al, 2015; Naidu et al, 2016); these indicate that its reactivity is comparable to that of EFB Co-utilization of biomass with coal can be achieved by direct co-combustion and co-gasification. ‘The reactivity of co- gasification of the blended coal and biomass can be enhanced ‘due (0 the catalytic effect of the nigh content of metal elements in the biomass ash (Lahijani et al, 2012a,b), Biomass is already being used as a supplemental fuel to substitute up to 10% of the base fuel in commercial operations to reduce formation of NO, and SO, emissions (Agbor et al. 2014). In the case of direct co- firing, the presence of 80% of volatile matter on dry basis in the bio- ‘mass has the potential to be very effective reburn fuel so as to reduce the NO, produced when coal is used as the primary fuel (Sami et al, 2001). Biomass can also be used in indirect gasification ‘mode; this would require additional biomass gasifier which needs to be dynamically coupled and thermally integrated with the rest ‘of the plant. Unless this becomes mandatory, for example, due to severe fouling and slagging problems that may result from incom patible ash characteristics, co-firing is advantageous. ‘Although adding synthetic catalysts can be very effective in ‘enhancing gasification, cost and recovery ofthe catalysts are major issues. One possibility to address this isto co-gasify biomass with the coal, in which ash minerals ofthe biomass, constituting alkali ‘components (eg. K’, Na" and Ca?*), act as inexpensive natural cat- alysts to enhance co-gasification (Lahijani et al, 2013b; Masnadi ‘eC al, 2015}. Studies reported in the literature (Gilet al, 1997; McLendon et al, 2004; Lapuerta etal. 2008) show that the effect ‘and extent of synergy or inhibition depend on the gasification ‘operating and fuel conditions, such as feedstock type, particle con- tact, temperature and pressure, and reactor type. Char gasification ‘can be considered as the rate controlling step in the thermochem- ical conversion of carbonaceous materials. The presence of alkaline (Kand Na) alkaline earth (Ca and Mg) metals promotes the carbon. reaction rate (Dupont etal, 2011; Lahijani et al,.2013a,b). The ash Forming elements in biofuels are salts such as chlorides (KCI), and sulfates (K;$0,) (Arvelakis et al, 2003; Fryda et al, 2008; Mettanant et al, 2009; Serrano et al, 2015), Therefore, for high potassium containing biomass fuels such as empty fruit bunch, ‘gasification or combustion is recommended to be restricted co 800 °C or lower in order to ensure that there is no formation of ‘agglomeration (Lahijani and Zainal, 2011), Recent experimental studies using high ash Indian coals (Datta et al. 2015) showed agglomeration tendency under steam gasification conditions Which could be avoided by maintaining proper steam to fuel ratio fora fixed flow rate of air to fuel ratio. The Boudouard reaction is also strongly influenced by the surface morphology. The gasifica- tion reaction initiates with the more disorganized carbon where the active sites are activated by the adsorption of the gasifying agent. Therefore, afer an initial rise in reactivity to a maximum, limit, the reactivity decreases and tends to flatten as time pro- _gresses as the available surface area diminishes due to reduction in the number of potential gasification sites (Diez and Borrego, 2013), In the light of the considerable literature that exists on the ‘effect of biomass on the reactivity of coals, the present study is ‘motivated by the need to study the reactivity enhancement possi- bilities with two biomasses, namely, empty fruit bunch (EFB) and ‘casuarina equiseifolia (CE) in the context of co-gasification with, Indian coals using CO, as the gasifying agent. To this end, system- atic isothermal TGA studies have been conducted ever a range of emperatures and for different proportions of biomass and coal ‘chars. The results show that improvement in reactivity occurs under most conditions for the blended samples; however, inhibi- tion of reactivity too has been found under certain conditions. Details of the experiments and the results obtained are discussed below. 2. Methods One high ash coal (nearly 48% of ash) obtained from Bilaspur (in the state of Chhattisgarh), denoted as BS, two medium ash coals ‘obtained from Godavari Khani and Bellampali (in the state of ‘Andhra Pradesh) denoted as GK and BM, respectively, and two bio- ‘mass fuels, namely, empty fruit bunch and casuarina equisetifolla (of nearly 70% of volatile matter), denoted as EFB and CE, respec~ tively, obtained from locally available agro fields, have been used in the present study t0 investigate the reactivity of blended fuels. “The coal was crushed and ground toa size of ~106/+90 um to min- mize diffusional effects during the gasification reaction. The bio- mass fuels were cut to the size tange of 1-2mm in order to prepare chars, These raw fuels were characterized through proxi- mate and ultimate analyses as per ASTM standards. The calorific ‘value was measured using a bomb calorimeter. The detailed anal- ysis of the fuels is given in Table 1, Ash analysis ofthe fuels is of particular importance to the present study and it was performed based on ASTM standard for coal and both ASTM and EN standards for the biomass fuels. The high percentage of alkali and alkaline ‘compounds in the biomass mineral matter would not be reflected in the ASTM standard carried out at 900°C and therefore the ash analysis of biomass fuels was carried out atthe lower temperature ‘of 550°C as per EN standard. The detailed ash analysis of the raw fuels is given in Table 2. The results for high ash coal and FB com- pare well with those reported in the literature (Datta etal, 2015; Madhiiyanon et aly 2012), respectively. About 80-85% of the ash 's composed of silica and alumina in the three coals with silica alone contributing about 60-70%. Inthe case of EFB, KO isthe lar~ ‘gest contributor to ash but it also has a significant amount of silica. ‘The other biomass (CE) has a large amount of CaO and very little silica and alumina and thus presents a contrasting feature. Al chars were prepared in a muffle furnace at 900 °C for seven ‘minutes as per ASTM standards. In the process, a significantsupra) 15-15 * Tent an ea np Tine ont aa Tine aa cave eae (neta 2 eS m0 es se aaa Tide Anse i ee ee Ce ee Sonos Asea Sf Ss ge at ios fw ig te aes tne Suro ca ee ee ee ee) Somes Cee ait vatiez ts fs Mie 89, AiG) GGG iets sojeten Osea ONE IA Co A dat Bina ST dort) ns ons am was goes nk am Sino (sna) aoe oe ae oe oes oo —. fuel char blend sample of 810mg was taken for both non- Penne ss et has. fsothermal and. ister srvimetic analyses. In the mon Sa ey stheral gasification studs, Nz was vsed 25 9 sweeping gas < - and CO» was used as the reactant gas. These reactants were intro- x “0 287 3672 ‘3582 3364 duced at room temperature and maintained at a flow rate of a SL 2m maori! and 30a mar respectively, lothermal expe a ee el eee emer ners ee = tia deme f1T__ S038 1782___nom-sothermal experiments, but the gsivng reactant nas into amount of volatile matter (~60% to 70%) was removed along with all the moisture. However, the latter was picked by the char during storage. The proximate analysis of the chars prior to gasification experiments was cartied out using TGA under Ny and air environ- :ments as per ASTM standard procedure, and the results are shown in Table 3. Itcan be seen that a significant amount of volatile mat- ter in the chat, especially in the two biomasses. However, most of this gets removed duting the pre-heating stage in inert Nz environ- ‘ment during isothermal TG analysis (Naidu etal, 2016). Typically, an appreciable amount of mass loss (both moisture and volatile matter) occurs prior to the introduction of CO. When this is included, more than 90% of the volatile matter in the fuel is esti ‘ated to have been removed prior to the initiation of the Bou- ddouard reaction. The coals (BS, GK and BM) and biomasses (EFB and CE) chars obtained from the furnace were blended in propor- tions of coal char to biomass char ratios of 70:30 and 50:50 by mix- ing individually weighed samples thoroughly for 10 min. These samples were then directly used for proximate and TGA analysis. ‘The mass percentage of ash to the fixed carbon listed in the last column of Table 3 shows that the ash constitutes ~75% of the total ‘mass in the case of BS while its only ~18% in the case of CE. "Non isothermal and isothermal TG ofthe char blends were per- formed using TA Instruments SDT Q600. The non-isothermal experiments were performed in the range from 25 to 1200 °C with a heating rate of 20°C min ' and isothermal experiments were pperformed at 900, 1000, 1100°C with a heating rate of 100°- Cmin * in the preheating stage. The relatively high temperatures {or isothermal TGA were due to the high temperatures at which Boudouard reactions sets in for these coals (Naidu et al, 2016). A ‘duced after the sample reached the set target temperature. The supply of the reactant gas was maintained for 1h. All experiments ‘were performed at atmospheric pressure. 3. Results and discussion 3.1, Non-isothermal gasification studies ‘The TG and DTG curves for the 70:30 and 50:50 wt% blend of coal and biomass chars along with those for the pure fuels are given in Figs. 1 and 2, respectively for different solid fuels. As ‘expected, the remaining mass after gasification reaction decreases ‘with addition of biomass to the blend. As gasification reaction is initiated only at high temperatures and since theve is significant amount of moisture and remnant volatiles in the char, we see a two- or three-peak variation in the DTG curves, the peaks corre- sponding to moisture removal, devolatlization and the Boudouard reaction of CO gasification of char, which occurred only after 700°C or even later. The peak rates and the corresponding temper- atures corresponding to the Boudouard reaction, which are of interest in the present study, have been deduced from the DTG curves. These characteristic parameters are listed in Table 4 for the non-isothermal studies of diferent blends. The values of the peaks are not quantitatively comparable as the amount of moisture And volatiles are different for each chat. The temperature range for the gasification reaction is in the range of 800-1100 °C and decreases from the pure coal value as the biomass content increases. Although the addition of biomass reduces the peaking temperature, it is not possible to attribute this to synergistic effects, For this, it is necessary to conduct isothermal TCA studies. -ased on the teactivity tange obtained for the Boudouatd reaction\Suyam Naid ta /Boresoure Tecolegy 209 (2016) 157-165 1 » ° “ » 8 co | Ba 20. : 8 « —s : =e ‘ See aoe ‘Temperature (°C) Fig. 1. 1G curves for coal and biomass len chars ‘obtained from the non-isothermal TGA, isothermal TGA has been performed for the char blends at 900, 1000, 1100 °C and the results are discussed below. 3.2. Isothermal gasification of char blends In these studies, a small sample of the pure char or the char bend was preheated in inert (N,) atmosphere to the target tem- perature at a heating rate of 100°C/min and then CO. was intro- ‘duced along with the sweep gas (Nz). The mass at the time of introduction of CO: was taken as the initial mass and conversion ‘of the fuel was evaluated based on further mass loss (Naidu ‘al, 2016). Fig. 2 shows the conversion of BS char blended with, EB and CE biomasses at 900, 1000 and 1100°C. Typically, the con- ‘version plots for blends show faster conversion than for pure coal char. However, ths is not always the case: in Fig. 3c, some results for the blends show slower conversion, Such behavior is not unique ‘and has been found for other coal chars (see Figs. 4 and 5) and has also been reported in the literature. This indicates an inhibition effect in some cases, especially at low conversions. Since under practical gasification conditions, high conversions, typically in ‘excess of 90% ate sought, we Focus inthe present study on the time for 95% of the fuel char. However, such conversions have not been achieved at all temperatures. For example, carbon conversion of ‘only 73% was achieved at 900°C in 34075 for the pure BS char and complete conversion was observed for 1000 and 1100 °C with ‘95% conversion times of 1965 and 637s, respectively. The 95% con- version times for EFB at 900, 1000 and 1100°C are 283, 130 and 1195, respectively. The corresponding values for pure CE chars are 233, 147 and 130s, Thus, the conversion times of the BS coal ‘and the two biomasses are significantly different. The adeltion of biomass to coal shows improved reactivity in the form of decreased time of conversion. For example, from the data shown in Fig. 3, one can obtain the 95% conversion times for 70:30 w.% blend of BS and EFB to be 2460, 1360 and 1090 sat temperatures ‘of 900, 1000 and 100°C, respectively. For a 50:50 wt blend of the two chars, the corresponding times are further reduced to 1850, 670 and 3305, The blending of BS with CE biomass char {oo results in significant reductions in the 95% conversion time. For example, for a 50:50 wl mixture of BS and CE, the 95% con- ‘version times are further reduced to 1145, 455 and 255 s at 900, 1000, 1100°C, respectively. ‘Similar results have been obtained for the blends of other coal chats with EFB and CE, although there is some variation within the overall reduction, The isothermal TGA mass loss curves are for GK and BM coal chars and their blends are shown in Figs. 4 ‘and 5, respectively, in each case, at 900, 1000 and 1100°C and for coal char to biomass char blend ratios of 70:30 and 50:50 by ‘mass. The consolidated data of 95% conversion times for all chars at the three temperatures are presented in Table 5. One can see that despite its lower amount of ash, GK is less reactive than BS ‘at 900 and 1000 °C while BM is more reactive presumably due to the CaO content in its ash (see Table 2). There is significant improvement in the reactivity in both cases by blending with either EFB or CE leading to conservable reduction in the 95% con- ‘version times. The amount of ash and the components of ash can also play a part in the enhancement or otherwise ofthe reactivity. ‘The enhanced rate of reaction for BSCE blend may be due to lower percentage of ash present in the CE char and also the lower percentage of silica and aluminum oxides in the ash. The presence ‘of large amounts of potassium typically found in biomass ash (e.g, EFB, see Table 2). together with large amounts of silica and alumina in the coal chars may lead to the formation of potassium alumi- nosilicates such as KAISi,Os and KAISIO, under co-gasificationSayan Nid ea /Siresource Technology 209 (2016) 157-165 6 ge Se] Cations = 7020 . 7 oxen Bas men jen 02 ty met aN te 4 oo] 8 oa] coattiomass = 50450 2407 s (this much conversion could not be achieved during the TGA) ata temperature of 900°C which itis 2460 s when blended with 30% EFB showing a signifi cant decrease and thus synergetic effect, At a temperature of 11000, the same conversion of 90.12% takes 1430's when gasified alone and 1360 s when blended with 20% biomass. In this case, the two conversion times are not significantly different and lie within 10% of each other. Iti reckoned that in this case, there is neither synergetic effect nor inhibition. For the same blend, one notes that at 110°C, the time of conversion is 1090 whereas in pure coal char itis 458 , thus indicating a clear inhibition effect. Similar results have been compiled in Table 6 forall the 12 com- binations that have been studied in the present investigation. One can see that in all cases, the conversion % of coal is fairly high (81% and typically 90%). The following trends can be abserved: + In almost all cases, increasing the proportion of biomass led toa stronger synergetic effect. This was found to be true for both the biomasses and for all the three coals. The coal char conversion, ‘ime was reduced when the percentage of biomass was increased from 30% to 50%, + Incteasing the temperature at which gasification occurred decreased the 90% conversion time for temperatures up to 1100°C. This indicates the prevalence of chemical kinetic con- ‘sol on the gasification reaction even at this high temperature. ‘Clear case of inhibition has been found to occur only for the blends of the high ash coal, BS, with the biomasses (Cases 1, 2 and 3 of Table 6). Even for these fuel combinations, inhibition ‘of reactivity by more than 10% occurred only at the gasification, temperature of 1100°C in all the three eases. The increase ofet Saya Naid ta /Boresource Tecolegy 209 (2016) 157-165 ‘Shae or inhibition eet on CO ssifstion eatviy dt lending. ae No Gharbiewd —_—_‘ECoalcharcomversion —__Temperatre("©) Times) for eonvesion or biomass Synerylahibiton mane of o » 0 7 wre 2 00 ST 20 Syneray 100 10. 1360 Nether tieo 258 080 tation a es +eF8 ne 900 S07 1850 Synergy 1000 1030 670 Sinesay 00 386 30 either 3 Bs ce sont 900 S407 2495, Synergy 10 1st mass Neither 00 25 ns Initio 4 as +ce 8126 900 S07 1s Syne co on ass Seen veo 3 255, sey 5 oxo ous 900 35235 ms smerny 10 1919 750 Synergy 6 cxsern 078 00 Sas ous Syeecy 100 ie 350 synergy 0 09 195 Synergy 7 cxvce oe soo. 3a sus Swen 100 1s 700 Syne eo 295 Bs synergy ‘ oxsce wo91 00 Seas 100 Sines 10 154 510 sinerty 00 19, 285, synergy 9 ate nar 00 16 1970 Nether co 8 45 Synergy to 25 as syneray 10 eM em ous 900 i810 1085, Neither 100 ane 19 synergy io a8 as synergy " wuece soa 300 1964 1815, Nether 1000 00 es Syneray 00 365 20 Synergy 2 auece nat 00, 151 915 Syeeey 1000 02 5 sinesay 00 386 240 synergy biomass content to 50% by mass mitigated this effect somewhat (€f Case 1 and Case 2) in the case of BS blend with EFB. In the ‘ase of BS with blend with CE, increasing the biomass content +0 50% actually reversed the inhibitory effect (cf. Case 3 and Case 4). Taken together, these data point to 2 combination of factors leading to inhibition. Firstly, the higher temperatures ‘may have reduced the kinetic dependence of the reaction lead- ing to a more muted role of catalytic activity. Secondly, the presence of large amount ash in the BS char, most of which ‘would have remained in the crucible during the experiment, could have accentuated the diffusional effects on the overall reactivity by presenting a physical barrier for the gasifying to have to diffuse through, Thirdly, the increased amount of silicates in the ash, coupled with the higher temperature of ‘operation, could have led to the formation of potassium alumi- nosilicates in the case of BS + EFB and calcium aluminosilicates, in the case of BS + CE. It may be noted that the relatively stron- ger synergetic effect of CE compared to EFB is supported by the last two arguments as both the ash content and the silica con- tent in the ash are lower for CE. 4. Conclusions Blends of three coals chars and two biomass chars of indian ori gin have been assessed through isothermal TGA for synergistic effects during CO, gasification. The conversion times for coal char have been deduced indirectly by assuming that for high conver- sions all the biomass char would have converted leaving only some amount of coal char unconverted. Compating the time requited for «coal char conversion with and without blending with biomass for 12 different cases of blending. it is concluded that both EFB and CE have synergetic effect with CE being the more reactive of the two. 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