A comparative analysis of the response of agave bagasse (AGB) to pretreatment by ammonia fiber expansion (AFEX™), autohydrolysis (AH) and ionic liquid (IL) was performed using 2D nuclear magnetic resonance (NMR) spectroscopy, wet chemistry, enzymatic saccharification and mass balances. It has been found that AFEX pretreatment preserved all carbohydrates in the biomass, whereas AH removed 62.4% of xylan and IL extracted 25% of lignin into wash streams. Syringyl and guaiacyl lignin ratio of untreated AGB was 4.3, whereas for the pretreated biomass the ratios were 4.2, 5.0 and 4.7 for AFEX, AH and IL, respectively. Using NMR spectra, the intensity of β-aryl ether units in aliphatic, anomeric, and aromatic regions decreased in all three pretreated samples when compared to untreated biomass. Yields of glucose plus xylose in the major hydrolysate stream were 42.5, 39.7 and 26.9kg per 100kg of untreated AGB for AFEX, IL and AH, respectively.
Agave bagasse (AGB) has gained recognition as a drought-tolerant biofuel feedstock with high productivity in semiarid regions. A comparative analysis of ionic liquid (IL) and organosolv (OV) pretreatment technologies in AGB was performed using a sequential enzymatic saccharification and fermentation (SESF) strategy with cellulolytic enzymes and the ethanologenic Escherichia coli strain MS04. After pretreatment, 86% of xylan and 45% of lignin were removed from OV-AGB, whereas IL-AGB reduced lignin content by 28% and xylan by 50% when compared to the untreated biomass. High glucan (>90%) and xylan (>83%) conversion was obtained with both pretreated samples. During the fermentation stage (48h), 12.1 and 12.7kg of ethanol were produced per 100kg of untreated AGB for IL and OV, respectively. These comparative analyses showed the advantages of SESF using IL and OV in a biorefinery configuration where a better understanding of AGB recalcitrance is key for future applications.
Available onlineKeywords: Agave bagasse Ionic liquid pretreatment Lignocellulosic biofuels Calcium oxalate Characterization a b s t r a c t Previous studies of agave bagasse (AGB-byproduct of tequila industry) presented unidentified crystalline peaks that are not typical from common biofuel feedstocks (e.g. sugarcane bagasse, switchgrass or corn stover) making it an important issue to be addressed for future biorefinery applications. Ionic liquid (IL) pretreatment of AGB was performed using 1-ethyl-3-methylimidazolium acetate ([C 2 mim][OAc]) at 120, 140 and 160 C for 3 h and a mass fraction of 3% in order to identify these peaks. Pretreated samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electronic microscopy (FE-SEM), thermal analysis (TGA-DSC) and wet chemistry methods. Previous unidentified XRD peaks on AGB at 2q ¼ 15 , 24.5 and 30.5 , were found to correspond to calcium oxalate (CaC 2 O 4 ) in a monohydrated form. IL pretreatment with [C 2 mim][OAc] was observed to remove CaC 2 O 4 and decrease cellulose crystallinity. At 140 C, IL pretreatment significantly enhances enzymatic kinetics and leads to~8 times increase in sugar yield (6.66 kg m À3 ) when compared to the untreated samples (960 g m À3 ). These results indicate that IL pretreatment can effectively process lignocellulosic biomass with high levels of CaC 2 O 4 .
Utilization of lignocellulosic materials for the production of value-added chemicals or biofuels generally requires a pretreatment process to overcome the recalcitrance of the plant biomass for further enzymatic hydrolysis and fermentation stages. Two of the most employed pretreatment processes are the ones that used dilute acid (DA) and alkaline (AL) catalyst providing specific effects on the physicochemical structure of the biomass, such as high xylan and lignin removal for DA and AL, respectively. Another important effect that need to be studied is the use of a high solids pretreatment (≥15%) since offers many advantaged over lower solids loadings, including increased sugar and ethanol concentrations (in combination with a high solids saccharification), which will be reflected in lower capital costs; however, this data is currently limited. In this study, several variables, such as catalyst loading, retention time, and solids loading, were studied using response surface methodology (RSM) based on a factorial central composite design of DA and AL pretreatment on agave bagasse using a range of solids from 3 to 30% (w/w) to obtain optimal process conditions for each pretreatment. Subsequently enzymatic hydrolysis was performed using Novozymes Cellic CTec2 and HTec2 presented as total reducing sugar (TRS) yield. Pretreated biomass was characterized by wet-chemistry techniques and selected samples were analyzed by calorimetric techniques, and scanning electron/confocal fluorescent microscopy. RSM was also used to optimize the pretreatment conditions for maximum TRS yield. The optimum conditions were determined for AL pretreatment: 1.87% NaOH concentration, 50.3 min and 13.1% solids loading, whereas DA pretreatment: 2.1% acid concentration, 33.8 min and 8.5% solids loading.
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