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This work studied the optimization of enzymatic saccharification of Agave tequilana bagasse (ATB) pretreated with the low-cost protic ionic liquid (PIL) ethanolamine acetate ([EOA][OAc]) using the highly available and cost-effective mixture of the enzymatic cocktails Celluclast 1.5L-Viscozyme L. Response surface methodology (RSM) was employed to maximize the sugars concentration and yield. The RSM optimization conditions of the enzymatic saccharification of pretreated ATB that achieved the maximum reducing sugars (RS) concentration were: 11.50 % w/v solids loading, 4.26 pH with 0.76 and 1.86 mg protein/mL buffer of Viscozyme L and Celluclast 1.5L, respectively. Similarly, the conditions that maximize the sugar yield (SY) were solids loading of 5.62 % w/v, and 4.51 pH as well as 1.07 and 2.03 mg protein/mL buffer of Viscozyme L and Celluclast 1.5L, respectively. Saccharification performance of the first-generation and low-cost enzyme mixture Celluclast 1.5L-Viscozyme L was compared with that reached by a second-generation and higher-cost CTec2, where Celluclast 1.5L-Viscozyme L achieved 60.86 ± 2.66 % y 79.25 ± 3.34 % of the sugars released by CTec2 at the same hydrolysis time (12 h) for the sugar concentration and yield models, respectively. These results are encouraging since they positively contribute to cost reduction and availability issues, which are key parameters to consider when thinking about scaling-up the process.

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We present an implementation of the interacting quantum atom (IQA) energy decomposition scheme using the complete active space second-order perturbation theory (CASPT2). This combination yields a real-space interpretation tool with a proper account of the static and dynamic correlation that is particularly relevant for the description of processes in electronic excited states. The IQA/CASPT2 approach allows determination of the energy redistribution that takes place along a photophysical/photochemical deactivation path in terms of self- and interatomic contributions. The applicability of the method is illustrated by the description of representative processes spanning different bonding regimes: noble gas excimer and exciplex formation, the reaction of ozone with a chlorine atom, and the photodissociations of formaldehyde and cyclobutane. These examples show the versatility of using CASPT2 with the significant information provided by the IQA partition to describe chemical processes with a large multiconfigurational character.

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Sequential 2k factorial and central composite designs were used to optimize Agave tequilana bagasse (ATB) pretreatment by using 1-ethyl-3-methylimidazolium acetate ([Emim][OAc]). Reaction time, temperature and solids loading were the studied factors while sugar yield was the response variable. Results indicated that optimal conditions (119 °C, 142 min) using high solids loading (30%) were achieved at lower temperatures and reaction times than those previously reported in the literature. It was also revealed that solid recovery after pretreatment with [Emim][OAc] is a key factor. The increase in enzymatic digestibility of pretreated ATB was correlated to a decrease in crystallinity and lower lignin content as observed using microscopy techniques and weaken chemical bonds by Fourier transform infrared spectroscopy. Yields of glucose and xylose in the hydrolysate were 41.3, and 13.0 kg per 100 kg of untreated ATB, which are equivalent to glucan and xylan conversions of 75.9% and 82.9%, respectively.

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BACKGROUND: Pretreatment is necessary to reduce biomass recalcitrance and enhance the efficiency of enzymatic saccharification for biofuel production. Ionic liquid (IL) pretreatment has gained a significant interest as a pretreatment process that can reduce cellulose crystallinity and remove lignin, key factors that govern enzyme accessibility. There are several challenges that need to be addressed for IL pretreatment to become viable for commercialization, including IL cost and recyclability. In addition, it is unclear whether ILs can maintain process performance when utilizing low-cost, low-quality biomass feedstocks such as the paper fraction of municipal solid waste (MSW), which are readily available in high quantities. One approach to potentially reduce IL cost is to use a blend of ILs at different concentrations in aqueous mixtures. Herein, we describe 14 IL-water systems with mixtures of 1-ethyl-3-ethylimidazolium acetate ([C2C1Im][OAc]), 1-butyl-3-ethylimidazolium acetate ([C4C1Im][OAc]), and water that were used to pretreat MSW blended with agave bagasse (AGB). The detailed analysis of IL recycling in terms of sugar yields of pretreated biomass and IL stability was examined. RESULTS: Both biomass types (AGB and MSW) were efficiently disrupted by IL pretreatment. The pretreatment efficiency of [C2C1Im][OAc] and [C4C1Im][OAc] decreased when mixed with water above 40%. The AGB/MSW (1:1) blend demonstrated a glucan conversion of 94.1 and 83.0% using IL systems with ~10 and ~40% water content, respectively. Chemical structures of fresh ILs and recycle ILs presented strong similarities observed by FTIR and 1H-NMR spectroscopy. The glucan and xylan hydrolysis yields obtained from recycled IL exhibited a slight decrease in pretreatment efficiency (less than 10% in terms of hydrolysis yields compared to that of fresh IL), and a decrease in cellulose crystallinity was observed. CONCLUSIONS: Our results demonstrated that mixing ILs such as [C2C1Im][OAc] and [C4C1Im][OAc] and blending the paper fraction of MSW with agricultural residues, such as AGB, may contribute to lower the production costs while maintaining high sugar yields. Recycled IL-water mixtures provided comparable results to that of fresh ILs. Both of these results offer the potential of reducing the production costs of sugars and biofuels at biorefineries as compared to more conventional IL conversion technologies.Graphical abstractSchematic of ionic liquid (IL) pretreatment of agave bagasse (AB) and paper-rich fraction of municipal solid waste (MSW).

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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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Lignocellulose represents a sustainable source of carbon for transformation into biofuels. Effective biomass to sugar conversion strategies are needed to lower processing cost without degradation of polysaccharides. Since ionic liquids (ILs) are excellent solvents for pretreatment/dissolution of biomass, IL pretreatment was carried out on agave bagasse (AGB-byproduct of tequila industry) and digestibility and sugar yield was compared with that obtained with switchgrass (SWG). The IL pretreatment was conducted using ([C2mim][OAc]) at 120 and 160 °C for 3h and 15% biomass loading. While pretreatment using [C2mim][OAc] was very effective in improving the digestibility of both feedstocks, IL pretreatment at 160 °C resulted in higher delignification for AGB (45.5%) than for SWG (38.4%) when compared to 120 °C (AGB-16.6%, SWG-8.2%), formation of a highly amorphous cellulose structure and a significant enhancement of enzyme kinetics. These results highlight the potential of AGB as a biofuel feedstock that can produce high sugar yields with IL pretreatment.

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