Pretreatment of corn fiber by pressure cooking in water

The pretreatment of corn fiber using liquid water at temperatures between 220 and 260°C enhances enzymatic hydrolysis. This paper describes the laboratory reactor system currently in use for cooking of corn fiber at temperatures ranging from 200 to 260°C. The corn fiber at approx 4.4% solid/liquid slurry was treated in a 2-L, 304 SS, Parr reactor with three turbine propeller agitators and a Proportional-Integral-Derivative (PID), controller that controlled temperature within ±1°C. Heat-up times to the final temperatures of 220, 240, or 260°C were achieved in 50 to 60 min. Hold time at the final temperature was less than 10 s. A serpentine cooling coil, through which tap water was circulated at the completion of the run, cooled the reactor’s contents to 180°C within 2 min after the maximum temperature was attained. Ports in the reactor’s head plate facilitated sampling of the slurry and monitoring the pH. A continuous pH monitoring system was developed to help observe trends in pH during pretreatment and to assist in the development of a base (2.0M KOH) addition profile to help keep the pH within the range of 5.0 to 7.0. Enzymatic hydrolysis gave 33 to 84% conversion of cellulose in the pretreated fiber to glucose compared to 17% for untreated fiber.     

Comparison of microbial inhibition and enzymatic hydrolysis rates of liquid and solid fractions produced from pretreatment of biomass with carbonic acid and liquid hot water

This research quantified the enzymatic digestibility of the solid component and the microbial inhibition of the liquid component of pretreated aspen wood and cornstover hydrolysates. Products of liquid hot water and carbonic acid pretreatment were compared. Pretreatment temperatures tested ranged from 180 to 220°C, and reaction times were varied between 4 and 64 min. Both microbial inhibition rates and enzymatic hydrolysis rates showed no difference between pretreatments containing carbonic acid and those not containing no carbonic acid. Microbial inhibition increased as the reaction severity increased, but only above a midpoint severity parameter of 200°C for 16 min. Both the rates and yields of enzymatic hydrolysis displayed an increase from the lowest tested reaction severity to the highest tested reaction severity.     

Combined steam pretreatment and enzymatic hydrolysis of starch-free wheat fibers

Steam treatment of an industrial process stream, denoted starch-free wheat fiber, was investigated to improve the formation of monomeric sugars in subsequent enzymatic hydrolysis for further bioconversion into ethanol. The solid fraction in the process stream, derived from a combined starch and ethanol factory, was rich in arabinose (21.1%), xylose (30.1%), and glucose (18.6%), in the form of polysaccharides. Various conditions of steam pretreatment (170–220°C for 5–30 min) were evaluated, and their effect was assessed by enzymatic hydrolysis with 2 g of Celluclast + Ultraflo mixture/ 100 g of starch-free fiber (SFF) slurry at 5% dry matter (DM). The highest overall sugar yield for the combined steam pretreatment and enzymatic hydrolysis, 52g/100 g of DM of SFF, corresponding to 74% of the theoretical, was achieved with pretreatment at 190°C for 10 min followed by enzymatic hydrolysis.     

Ethanol production from olive oil extraction residue pretreated with hot water

The olive pulp fraction contained in the residue generated in olive oil extraction by a two-step centrifugation process can be upgraded by using the cellulose fraction to produce ethanol and recovering high value phenols (tyrosol and hydroxytyrosol). Olive pulp was pretreated in a laboratory scale stirred autoclave at different temperatures (150–250°C). Pretreatment was evaluated regarding cellulose recovery, enzymatic hydrolysis effectiveness ethanol production by a simultaneous saccharification and fermentation process (SSF), and phenols recovery in the filtrate. The pretreatment of olive pulp using water at temperatures between 200°C and 250°C enhanced enzymatic hydrolysis. Maximum ethanol production (11.9 g/L) was obtained after pretreating pulp at 210°C in a SSF fed-batch procedure. Maximum hydroxytyrosol recovery was obtained in the liquid fraction when pretreated at 230°C.     

Comparison of yellow poplar pretreatment between NREL digester and sunds hydrolyzer

Single-stage cocurrent dilute acid pretreatments were carried out on yellow poplar (Liriodendron tulipifera) sawdust using an as-installed and short residence time modified pilot-scale Sunds hydrolyzer and a 4-L bench-scale NREL digester (steam explosion reactor). Pretreatment conditions for the Sunds hydrolyzer, installed in the NREL process development unit (PDU), which operates at 1 t/d (bone-dry t) feed rate, spanned the temperature range of 160 – 210°C, 0.1 – 1.0% (w/w) sulfuric acid, and 4-10-min residence times. The batch pretreatments of yellow poplar sawdust in the bench-scale digester were carried out at 210 and 230°C, 0.26% (w/w) sulfuric acid, and 1-, 3-, and 4-min residence times. The dilute acid prehydrolysis solubilized more than 90% of the hemicellulose, and increased the enzymatic digestibility of the cellulose that remained in the solids. Compositional analysis of the pretreated solids and liquors and mass balance data show that the two pretreatment devices had similar pretreatment performance.     

High pressure solids feeding using a lockhopper system: Design and operating experience

The feeding of solids into a high pressure reactor has always been difficult because of both high equipment costs and poor material characteristics. As part of the Solar Energy Research Institute’s investigation into the acid hydrolysis process, a lockhopper system was developed to feed wood into a vessel operating at 160°C (320°F) and 1.12 MPa (150 psig). Preliminary results show that the lockhopper operates successfully at temperature and pressure for a limited amount of time on wood sawdust. However, a problem that must be watched during operation is plugging of pneumatic lines by wood dust.     

Cellulose hydrolysis under extremely low sulfuric acid and high-temperature conditions

The kinetics of cellulose hydrolysis under extremely low acid (ELA) conditions (0.07 wt%) and at temperatures >200°C was investigated using batch reactors and bed-shrinking flow-through (BSFT) reactors. The maximum yield of glucose obtained from batch reactor experiments was about 60% for α-cellulose, which occurred at 205 and 220°C. The maximum glucose yields from yellow poplar feedstockswere substantially lower, falling in the range of 26–50%. With yellow poplar feedstocks, a large amount of glucose was unaccounted for at the latter phase of the batch reactions. It appears that a substantial amount of released glucose condenses with nonglucosidic substances. in liquid. The rate of glucan hydrolysis under ELA was relatively insensitive to temperature in batch experiments for all three substrates. This contradicts the traditional concept of cellulose hydrolysis and implies that additional factors influence the hydrolysis of glucan under ELA. Inexperiments using BSFT reactors, the glucose yields of 87.5, 90,3, and 90.8% were obtained for yellow poplar feedstocks at 205, 220, and 235°C, respectively. The hydrolysis rate for glucan was about three times higher with the BSFT than with the batch reactors. The difference of observed kinetics and performance data between the BSFT and the batch reactors was far above that predicted by the reactor theory.     

Ethanol production from pretreated olive tree wood and sunflower stalks by an SSF process

Olive tree wood and sunflower stalks are agricultural residues largely available at low cost in Mediterranean countries. As renewable lignocellulosic materials, their bioconversion may allow both obtaining a value-added product, for fuel ethanol, and facilitating their elimination. In this work, the ethanol production from olive tree wood and sunflower stalks by a simultaneous saccharification and fermentation (SSF) process is studied. As a pretreatment, steam explosion at different temperatures was applied. The water insoluble fractions of steam-pretreated sunflower stalks and steamed, delignified olive tree wood were used as substrates at 10% w/v concentration for an SSF process by a cellulolytic commercial complex and Saccharomyces cerevisiae. After 72-h fermentation, ethanol concentrations up to 30 g/L were obtained in delignified steam-pretreated olive tree wood at 230°C and 5 min. Sunflower stalks pretretated at 220°C and 5 min gave maximum ethanol concentrations of 21 g/L in SSF experiments.     

Optimization of SO2-catalyzed steam pretreatment of corn fiber for ethanol production

A batch reactor was employed to steam explode corn fiber at various degrees of severity to evaluate the potential of using this feedstock as part of an enzymatically mediated cellulose-to-ethanol process. Severity was controlled by altering temperature (150–230°C), residence time (1–9 min), and SO₂ concentration (0–6% [w/w] dry matter). The effects of varying the different parameters were assessed by response surface modeling. The results indicated that maximum sugar yields (hemicellulose-derived water soluble, and cellulose-derived following enzymatic hydrolysis) were recovered from corn fiber pretreated at 190°C for 5 minutes after exposure to 3% SO₂. Sequential SO₂-catalyzed steam explosion and enzymatic hydrolysis resulted in a conversion efficiency of 81% of the combined original hemicellulose and cellulose in the corn fiber to monomeric sugars. An additional posthydrolysis step performed on water soluble hemicellulose stream increased the concentration of sugars available for fermentation by 10%, resulting in the high conversion efficiency of 91%. Saccharomyces cerevisiae was able to ferment the resultant corn fiber hydrolysates, perhydrolysate, and liquid fraction from the posthydrolysis steps to 89, 94, and 85% of theoretical ethanol conversion, respectively. It was apparent that all of the parameters investigated during the steam explosion pretreatment had a significant effect on sugar recovery, inhibitory formation, enzymatic conversion efficiency, and fermentation capacity of the yeast.     

Conversion of lignocellulosics pretreated with liquid hot water to ethanol

Lignocellulosic materials pretreated using liquid hot water (LHW) (220°C, 5 MPa, 120 s) were fermented to ethanol by batch simultaneous saccharification and fermentation (SSF) usingSaccharomyces cerevisiae in the presence ofTrichoderma reesei cellulase. SSF of sugarcane bagasse (as received), aspen chips (smallest dimension 3 mm), and mixed hardwood flour (−60 +70 mesh) resulted in 90% conversion to ethanol in 2–5 d at enzyme loadings of 15–30 FPU/g. In most cases, 90% of the final conversion was achieved within 75 h of inoculation. Comminution of the pretreated substrates did not affect the conversion to ethanol. The hydrolysate produced from the LHW pretreatment showed slight inhibition of batch growth ofS. cerevisiae. Solids pretreated at a concentration of 100 g/L were as reactive as those pretreated at a lower concentration, provided that the temperature was maintained at 220°C.     

Pretreatment of Rice Straw by a Hot-Compressed Water Process for Enzymatic Hydrolysis

Hot-compressed water (HCW) is among several cost-effective pretreatment processes of lignocellulosic biomass for enzymatic hydrolysis. The present work investigated the characteristics of HCW pretreatment of rice straw including sugar production and inhibitor formation in the liquid fraction and enzymatic hydrolysis of pretreated material. Pretreatment was carried out at a temperature ranging from 140 to 240 °C for 10 or 30 min. Soluble oligosaccharides were found to constitute almost all the components of total sugars in the liquid fraction. The maximal production of total glucose at 180 °C and below accounted for 4.4–4.9% of glucan in raw material. Total xylose production peaked at 180 °C, accounting for 43.3% of xylan in raw material for 10-min pretreatment and 29.8% for 30-min pretreatment. The production of acetic acid increased at higher temperatures and longer treatment time, indicating more significant disruption of lignocellulosic structure, and furfural production achieved the maximum (2.8 mg/ml) at 200 °C for both 10-min and 30-min processes. The glucose yield by enzymatic hydrolysis of pretreated rice straw was no less than 85% at 180 °C and above for 30-min pretreatment and at 200 °C and above for 10-min pretreatment. Considering sugar recovery, inhibitor formation, and process severity, it is recommended that a temperature of 180 °C for a time of 30 min can be the most efficient process for HCW pretreatment of rice straw.     

SO2-catalyzed steam explosion of corn fiber for ethanol production

Corn fiber, a by-product of the corn wet-milling industry, represents a renewable resource that is readily available in significant quantities and could potentially serve as a low-cost feedstock for the production of fuel-grade alcohol. In this study, we used a batch reactor to steam explode corn fiber at various degrees of severity to evaluate the potential of using this feedstock in the bioconversion process. The results indicated that maximum sugar yields (soluble and following enzymatic hydrolysis) were recovered from corn fiber that was pretreated at 190°C for 5 min with 6% SO₂. Sequential SO₂-catalyzed steam explosion and enzymatic hydrolysis resulted in very high conversion (81%) of all polysaccharides in the corn fiber to monomeric sugars. Subsequently, Saccharomyces cerevisiae was able to convert the resultant corn fiber hydrolysates to ethanol very efficiently, yielding 90–96% of theoretical conversion during the fermentation process.     

Influence of particle size and pyrolysis conditions on yield,density and some textural parameters of chars prepared from holm-oak wood

Chars were prepared from holm-oak wood (Quercus ilex) using sawdust, cubes (20 × 20 × 20 mm) and octagonal prisms (20 × 20 × 80 mm) by heating in nitrogen under dynamic (sawdust and cubes) and isothermal (sawdust and prisms) conditions to different final temperatures. The yield of char production depends on the wood particle size, heating rate and final temperature. The density of the chars as measured by helium displacement, ϱ_He (g/cm³), is influenced by the wood particle size and heating conditions. Chars prepared from holm-oak wood are essentially microporous solids. The apparent surface area and the micropore volume increase only slightly up to the treatment temperature of 500°C, increase greatly up to 800°C and decrease at higher temperatures.     

Kinetics of Lime Pretreatment of Sugarcane Bagasse to Enhance Enzymatic Hydrolysis

The objective of this work was to determine the optimum conditions of sugarcane bagasse pretreatment with lime to increase the enzymatic hydrolysis of the polysaccharide component and to study the delignification kinetics. The first stage was an evaluation of the influence of temperature, reaction time, and lime concentration in the pretreatment performance measured as glucose release after hydrolysis using a 2³ central composite design and response surface methodology. The maximum glucose yield was 228.45 mg/g raw biomass, corresponding to 409.9 mg/g raw biomass of total reducing sugars, with the pretreatment performed at 90°C, for 90 h, and with a lime loading of 0.4 g/g dry biomass. The enzymes loading was 5.0 FPU/dry pretreated biomass of cellulase and 1.0 CBU/dry pretreated biomass of β-glucosidase. Kinetic data of the pretreatment were evaluated at different temperatures (60°C, 70°C, 80°C, and 90°C), and a kinetic model for bagasse delignification with lime as a function of temperature was determined. Bagasse composition (cellulose, hemicellulose, and lignin) was measured, and the study has shown that 50% of the original material was solubilized, lignin and hemicellulose were selectively removed, but cellulose was not affected by lime pretreatment in mild temperatures (60–90°C). The delignification was highly dependent on temperature and duration of pretreatment.     

Dilute-sulfuric acid pretreatment of corn stover in pilot-scale reactor

Corn stover is a domestic feedstock that has potential to produce significant quantities of fuel ethanol and other bioenergy and biobased products. However, comprehensive yield and carbon mass balance information and validated kinetic models for dilute-sulfuric acid (H₂SO₄) pretreatment of corn stover have not been available. This has hindered the estimation of process economics and also limited the ability to perform technoeconomic modeling to guide research. To better characterize pretreatment and assess its kinetics, we pretreated corn stover in a continuous 1 t/d reactor. Corn stover was pretreated at 20% (w/w) solids concentration over a range of conditions encompassing residence times of 3–12 min, temperatures of 165–195°C, and H₂SO₄ concentrations of 0.5–1.4% (w/w). Xylan conversion yield and carbon mass balance data were collected at each run condition. Performance results were used to estimate kinetic model parameters assuming biphasic hemicellulose hydrolysis and a hydrolysis mechanism incorporating formation of intermediate xylo-oligomers. In addition, some of the pretreated solids were tested in a simultaneous saccharification and fermentation (SSF) process to measure the reactivity of their cellulose component to enzymatic digestion by cellulase enzymes. Monomeric xylose yields of 69–71% and total xylose yields (monomers and oligomers) of 70–77% were achieved with performance level depending on pretreatment severity. Cellulose conversion yields in SSF of 80–87% were obtained for some of the most digestible pretreated solids.     

Ethanol production from steam-explosion pretreated wheat straw

Bioconversion of cereal straw to bioethanol is becoming an attractive alternative to conventional fuel ethanol production from grains. In this work, the best operational conditions for steam-explosion pretreatment of wheat straw for ethanol production by a simultaneous saccharification and fermentation process were studied, using diluted acid [H₂SO₄ 0.9% (w/w)] and water as preimpregnation agents. Acid-or water-impregnated biomass was steam-exploded at different temperatures (160–200°C) and residence times (5, 10, and 20 min). Composition of solid and filtrate obtained after pretreatment, enzymatic digestibility and ethanol production of pretreated wheat straw at different experimental conditions was analyzed. The best pretreatment conditions to obtain high conversion yield to ethanol (approx 80% of theoretical) of cellulose-rich residue after steam-explosion were 190°C and 10 min or 200°C and 5 min, in acid-impregnated straw. However, 180°C for 10 min in acid-impregnated biomass provided the highest ethanol yield referred to raw material (140 L/t wheat straw), and sugars recovery yield in the filtrate (300 g/kg wheat straw).     

Optimization of steam pretreatment of SO2-impregnated corn stover for fuel ethanol production

In this study, corn stover with a dry matter content of 20% was impregnated with SO₂ and then steam pretreated for various times at various temperatures. The pretreatment was evaluated by enzymatic hydrolysis of the solid material and analysis of the sugar content in the liquid. The maximum overall yield of glucose, 89% of the theoretical based on the glucan in the raw material, was achieved when the corn stover was pretreated at 200°C for 10 min. The maximum overall yield of xylose, 78%, was obtained with pretreatment at 190°C for 5 min.     

Hydrolysis of Ammonia-pretreated Sugar Cane Bagasse with Cellulase, β-Glucosidase, and Hemicellulase Preparations

Sugar cane bagasse consists of hemicellulose (24%) and cellulose (38%), and bioconversion of both fractions to ethanol should be considered for a viable process. We have evaluated the hydrolysis of pretreated bagasse with combinations of cellulase, β-glucosidase, and hemicellulase. Ground bagasse was pretreated either by the AFEX process (2NH₃: 1 biomass, 100 °C, 30 min) or with NH₄OH (0.5 g NH₄OH of a 28% [v/v] per gram dry biomass; 160 °C, 60 min), and composition analysis showed that the glucan and xylan fractions remained largely intact. The enzyme activities of four commercial xylanase preparations and supernatants of four laboratory-grown fungi were determined and evaluated for their ability to boost xylan hydrolysis when added to cellulase and β-glucosidase (10 filter paper units [FPU]: 20 cellobiase units [CBU]/g glucan). At 1% glucan loading, the commercial enzyme preparations (added at 10% or 50% levels of total protein in the enzyme preparations) boosted xylan and glucan hydrolysis in both pretreated bagasse samples. Xylanase addition at 10% protein level also improved hydrolysis of xylan and glucan fractions up to 10% glucan loading (28% solids loading). Significant xylanase activity in enzyme cocktails appears to be required for improving hydrolysis of both glucan and xylan fractions of ammonia pretreated sugar cane bagasse.     

Biochemical properties of genetic recombinant xylanase II

An ultraviolet (UV) coil reactor was designed and used for the online sterilization of cheese whey. Its microbial destruction efficiency was compared to that of the conventionally used UV reactor. Both reactors have the same geometry (840 ml volume and 17 mm gap size) and were tested at 11 flow rates of 5, 10, 15, 20, 25, 30, 35, 40, 50, 60, and 70 ml/min. The results obtained from this study showed that despite of its high turbidity, cheese whey could be sterilized using UV radiation if the proper reactor design and flow rate are used. The performances of the UV reactors were governed by the flow rate and the hydraulics of flow inside the reactor. The flow was laminar in both the reactors, as the Reynolds number was in the range of 1.39–20.10. The phenomenon of Dean Flow was observed in the coil reactor and the Dean number was in the range of 1.09–15.41. Dean vortices resulted in higher microbial destruction efficiency in the coil reactor in a shorter retention time. The rate of microbial destruction was found to be exponential in the conventional reactor and polynomial in the coil reactor. Increasing the flow rate from 5 ml/min to 70 ml/min decreased the microbial destruction efficiency of the conventional reactor from 99.40 to 31.58%, while the microbial destruction efficiency in the coil reactor increased from 60.77% at the flow rate of 5 ml/min to 99.98% at the flow rate of 30 ml/min and then decreased with further increases in flow rate reaching 46.2% at the flow rate of 70 ml/min. The maximum effluent temperatures in the conventional and coil reactors were 45.8 and 46.1°C, respectively. Fouling in the coil reactor was significantly less compared to the conventional reactor. The extent of fouling was influenced by flow rate and reactor’s hydraulics.     

Production of phenol compounds by alkaline treatment of technical hydrolysis lignin and wood biomass

Aqueous alkaline depolymerization of technical hydrolysis lignin (THL) was carried out with a 5% NaOH solution at a temperature of 180°C for 6 hours, the ratio between the biomass and depolymerizing agent being 1:8. The poplar wood sawdust was treated under the same conditions for 2 hours, where anthraquinone was added as a catalyst (0.5 wt %). The poplar wood bark was treated for 4 hours, without anthraquinone. Compounds contained in the aqueous phase were extracted three times by means of toluene for a ratio between the organic and aqueous phases equal to 1:5, 1:5 and 1:5. The compounds 2-methoxyphenol, 2,6-dimethoxyphenol, 4-hydroxy-3-methoxybenzaldehyde, 1-(4-hydroxy-3-methoxyphenyl)ethanone, 4-hydroxy-3,5-dimethoxybenzaldehyde, etc., were identified through GC-MS analysis in obtained extracts. Published in Khimiya Prirodnykh Soedinenii, No. 2, pp. 144–146, March–April, 2008.