Inmaculada Romero

Hydrothermal pre-treatment of rapeseed straw

As a first step for ethanol production from alternative raw materials, rapeseed straw was studied for fermentable sugar production. Liquid hot water was used as a pre-treatment method and the influence of the main pre-treatment variables was assessed. Experimental design and response surface methodology were applied using pre-treatment temperature and process time as factors. The pretreated solids were further submitted to enzymatic hydrolysis and the corresponding yields were used as pre-treatment performance evaluation. Liquid fractions obtained from pre-treatment were also characterized in terms of sugars and no-sugar composition. A mathematical model describing pre-treatment effects is proposed. Results show that enzymatic hydrolysis yields near to 100% based on pretreated materials can be achieved at 210-220 degrees C for 30-50 min, equivalent to near 70% of glucose present in the raw material. According to the mathematical model, a softer pre-treatment at 193 degrees C for 27 min results in 65% of glucose and 39% of xylose available for fermentation.

Liquid Hot Water Pretreatment of Olive Tree Pruning Residues

Olive tree pruning generates an abundant, renewable lignocellulose residue, which is usually burnt on fields to prevent propagation of vegetal diseases, causing economic costs and environmental concerns. As a first step in an alternative use to produce fuel ethanol, this work is aimed to study the pretreatment of olive tree pruning residues by liquid hot water. Pretreatment was carried out at seven temperature levels in the range 170–230°C for 10 or 60 min. Sugar recoveries in both solid and liquid fractions resulting from pretreatment as well as enzymatic hydrolysis yield of the solid were used to evaluate pretreatment performance. Results show that the enzyme accessibility of cellulose in the pretreated solid fraction increased with pretreatment time and temperature, although sugar degradation in the liquid fraction was concomitantly higher.

Dilute acid pretreatment of rapeseed straw for fermentable sugar generation

The influence of the main pretreatment variables on fermentable sugar generation from rapeseed straw is studied using an experimental design approach. Low and high levels for pretreatment temperature (140-200 °C), process time (0-20 min) and concentration of sulfuric acid (0.5-2% w/v) were selected according to previous results. Glucose and xylose composition, as well as sugar degradation, were monitored and adjusted to a quadratic model. Non-sugar components of the hydrolysates were also determined. Enzymatic hydrolysis yields were used for assessing pretreatment performance. Optimization based on the mathematical model show that total conversion of cellulose from pretreated solids can be achieved at pretreatment conditions of 200 °C for 27 min and 0.40% free acid concentration. If optimization criteria were based on maximization of hemicellulosic sugars recovery in the hydrolysate along with cellulose preservation in the pretreated solids, milder pretreatment conditions of 144 °C, 6 min and 2% free acid concentration should be used.

Optimization of uncatalyzed steam explosion pretreatment of rapeseed straw for biofuel production.

Rapeseed straw constitutes an agricultural residue with great potential as feedstock for ethanol production. In this work, uncatalyzed steam explosion was carried out as a pretreatment to increase the enzymatic digestibility of rapeseed straw. Experimental statistical design and response surface methodology were used to evaluate the influence of the temperature (185-215°C) and the process time (2.5-7.5min). According to the rotatable central composite design applied, 215°C and 7.5min were confirmed to be the optimal conditions, considering the maximization of enzymatic hydrolysis yield as optimization criterion. These conditions led to a maximum yield of 72.3%, equivalent to 81% of potential glucose in pretreated solid. Different configurations for bioethanol production from steam exploded rapeseed straw were investigated using the pretreated solid obtained under optimal conditions as a substrate. As a relevant result, concentrations of ethanol as high as 43.6g/L (5.5% by volume) were obtained as a consequence of using 20% (w/v) solid loading, equivalent to 12.4g ethanol/100g biomass.

Pretreatment of olive tree biomass with FeCl3 prior enzymatic hydrolysis.

Olive tree biomass (OTB) is an agricultural residue which can be used as raw material for bioethanol production. OTB was pretreated with 0.05-0.275 M FeCl(3) solutions at 120-180 °C for 0-30 min. Enzymatic hydrolysis yields were used for assessing pretreatment performance. Optimum FeCl(3) pretreatment conditions were found to be 152.6 °C, 0.26 M FeCl(3) for 30 min. Under such conditions, 100% of hemicellulose was removed, and enzymatic hydrolysis of pretreated solids resulted in a yield of 36.6g glucose/100g of glucose in the raw material. Hemicellulosic sugar recovery in the prehydrolysate was 63.2%. Results compare well with those obtained by other pretreatment strategies on the same raw material, confirming FeCl(3) solutions as a new, feasible approach for bioethanol production.

Ethanol production from glucose and xylose obtained from steam exploded water-extracted olive tree pruning using phosphoric acid as catalyst

In this work, the effect of phosphoric acid (1% w/w) in steam explosion pretreatment of water extracted olive tree pruning at 175°C and 195°C was evaluated. The objective is to produce ethanol from all sugars (mainly glucose and xylose) contained in the pretreated material. The water insoluble fraction obtained after pretreatment was used as substrate in a simultaneous saccharification and fermentation (SSF) process by a commercial strain of Saccharomyces cerevisiae. The liquid fraction, containing mainly xylose, was detoxified by alkali and ion-exchange resin and then fermented by the xylose fermenting yeast Scheffersomyces stipitis. Ethanol yields reached in a SSF process were close to 80% when using 15% (w/w) substrate consistency and about 70% of theoretical when using prehydrolysates detoxified by ion-exchange resins. Considering sugars recovery and ethanol yields about 160g of ethanol from kg of water extracted olive tree pruning could be obtained.

Dilute sulfuric acid pretreatment of sunflower stalks for sugar production.

In this work the pretreatment of sunflower stalks by dilute sulfuric acid is studied. Pretreatment temperature and the concentration of acid solution were selected as operation variables and modified according to a central rotatable composite experimental design. Based on previous studies pretreatment time was kept constant (5 min) while the variation range for temperature and acid concentration was centered at 175°C and 1.25% (w/v) respectively. Following pretreatment the insoluble solids were separated by filtration and further submitted to enzymatic hydrolysis, while liquid fractions were analyzed for sugars and inhibitors. Response surface methodology was applied to analyze results based on the combined severity of pretreatment experiments. Optimized results show that up to 33 g of glucose and xylose per 100g raw material (65% of the glucose and xylose present in the raw material) may be available for fermentation after pretreatment at 167°C and 1.3% sulfuric acid concentration.

Combined acid/alkaline-peroxide pretreatment of olive tree biomass for bioethanol production

Olive tree biomass (OTB) can be used for producing second generation bioethanol. In this work, extracted OTB was subjected to fractionation using a sequential acid/alkaline oxidative pretreatment. In the first acid stage, the effects of sulfuric acid concentration and reaction times at 130°C were investigated. Up to 71% solubilization of hemicellulosic sugars was achieved under optimized conditions (2.4% H2SO4, 84min). In the second stage, the influence of hydrogen peroxide concentration and process time were evaluated at 80°C. Approximately 80% delignification was achieved under the best operational conditions (7% H2O2, 90min) within the experimental range studied. This pretreatment produced a substrate with 72% cellulose that was highly accessible to enzymatic attack, yielding 82g glucose/100g glucose in delignified OTB. Ethanol production from both hemicellulosic sugars solubilized in the acid pretreatment and glucose from enzymatic hydrolysis of delignified OTB yielded 15g ethanol/100g OTB.

Xylitol production by Debaryomyces hansenii and Candida guilliermondii from rapeseed straw hemicellulosic hydrolysate.

This study evaluated the possibility of using rapeseed straw hemicellulosic hydrolysate as a fermentation medium for xylitol production. Two yeast strains, namely Debaryomyces hansenii and Candida guilliermondii, were used for this bioconversion process and their performance to convert xylose into xylitol was compared. Additionally, different strategies were evaluated for the hydrolysate detoxification before its use as a fermentation medium. Assays in semi-defined media were also performed to verify the influence of hexose sugars on xylose metabolism by the yeasts. C. guilliermondii exhibited higher tolerance to toxic compounds than D. hansenii. Not only the toxic compounds present in the hydrolysate affected the yeasts performance, but glucose also had a negative impact on their performance. It was not necessary to completely eliminate the toxic compounds to obtain an efficient conversion of xylose into xylitol, mainly by C. guilliermondii (YP/S=0.55g/g and 0.45g/g for C. guilliermondii and D. hansenii, respectively).

Pretreatment With Metal Salts

Abstract Metal salts have been proved to play a key role in the pretreatment of biomass. The development of the biorefinery concept, based on the fractionation of biomass into its constituents and further transformation, can benefit from either milder operational conditions or increased product yields by means of metal salts, generally in combination with other procedures. While biofuel production has been one of the traditional main targets, where metal salts have found an interesting application on the pretreatment stage, metal salts have also been applied to the production of other added-value chemicals. The wide range of raw materials, catalysts, methods, results, and future possibilities make these type of compounds, metal salts, a versatile and promising objective of research on lignocellulosic biomass. The main features of this research topic are briefly presented in this chapter.