Optimizing monosaccharide production from liquid hot water pretreatment and enzymatic hydrolysis of grass-clover press cake.

In the present study, clover-grass press cake was treated by liquid hot water at temperatures of 180-200 °C for a reaction time of 5-10 min. Evaluation of pretreatments was based on the monosaccharide yield after enzymatic hydrolysis of the pretreated slurry and solid fraction, respectively. Extraction of up to 48% hemicellulose and 4% cellulose was observed during pretreatment. The optimal pretreatment conditions were identified as 190 °C and 10 min resulting in monosaccharide yields of 90% and 73% of the theoretical maximum by slurry and solid conversion, respectively. At optimal conditions, the C6 monosaccharide yield (83-90%) was fairly equal compared to the C5 monosaccharide yield (56-89%), which increased by slurry conversion due to near-complete monomerization of soluble xylo-oligosaccharides. In this study, we showed that clover-grass press cake possesses considerable potential as feedstock for production of fermentable sugars in a biorefinery context.

Liquid hot water pretreatment combined with high-solids enzymatic hydrolysis and fed-batch fermentation for succinic acid sustainable processed from sugarcane bagasse.

In order to sustainable process of bio-succinic acid (SA), response surface methodology (RSM) was applied to optimize liquid hot water pretreatment pretreatment of sugarcane bagasse (SCB), followed by high-solids enzymatic hydrolysis of pretreated residual that without washing, then the hydrolysates and partial pretreatment liquid were used as carbon sources for SA fermentation. Results showed that the highest sugars yield could be achieved at pretreatment conditions of temperature 186 °C, time 25 min and solid-to-liquid ratio 0.08; enzymatic digestion the pretreated residuals at 20 % (w/v) solid content via enzymes reconstruction and fed-batch strategy, the obtained sugars reached to 121 g/L; by controlling the nutrition and conditions of the fermentation process, most of the C5 and C6 sugars in the hydrolysate and pretreatment liquid were converted into SA with a conversion rate high to 280 mg/g SCB. This study can provide a novel clue for clean and efficient biorefining of chemicals.

Evaluation of the Hydrolysis Efficiency of Bacterial Cellulose Gel Film after the Liquid Hot Water and Steam Explosion Pretreatments.

The influence of bacterial cellulose gel film pretreatment methods on the efficiency of enzymatic hydrolysis was investigated. An increase in the efficiency of enzymatic hydrolysis due to liquid hot water pretreatment or steam explosion was shown. The glucose yield of 88% was obtained from raw, non-purified, bacterial cellulose treated at 130 °C. The results confirm the potential of bacterial cellulose gel film as a source for liquid biofuel production.

From liquid hot water pretreatment solution to lignin-based hydrophobic deep eutectic solvent for highly efficient extraction of Cr (VI).

Liquid hot water (LHW) pretreatment has been widely investigated attributed to its advantages, such as environmental friendliness, the potential application of dissolved hemicellulose, and no chemical addition. Expanding the portfolio of products that can be made from LHW pretreatment solutions will be critical to enabling a viable LHW-based economy. We provide a one-step method to separate and functionalize lignin from the LHW pretreatment solution. A hydrophobic deep eutectic solvent (hDES) was prepared by using methyltrioctylammonium chloride (MTAC) and the LHW pretreatment solution and directly applied to the extraction of Cr (VI) in an aqueous solution. In the process of forming hDES, the removal rate of liquid hot water lignin (LHWL) was reached 99%. The new LHW-hDES exhibited excellent extraction performance for Cr (VI), the extraction capacity was as high as 198.402 mg g-1, optimum extraction conditions at the mass of hDES 0.10 g, vortex time 90 s, room temperature, and natural pH. Notably, we have shown that the method of combining the separation and functionalization of lignin in the LHW pretreatment solution, which can provide a way of thinking for the application of the LHW pretreatment solution.

Hydrothermal pretreatment for the production of oligosaccharides: A review.

Oligosaccharides are low-molecular-weight carbohydrates with crucial physical, chemical, and physiological properties, which are increasingly important in the fields of food, pharmaceuticals, cosmetics, and biomedicine. Pretreating biomass in a cost-effective way is a significant challenge for oligosaccharides research. Hydrothermal pretreatment is a potentially eco-friendly technology to obtain oligosaccharides by deconstructing biomass. In this work, we compared the differences between hydrothermal pretreatment and the traditional pretreatment method. The fundamentals and classification of hydrothermal pretreatment, as well as the latest studies on hydrothermal preparation of oligosaccharides, were further reviewed and evaluated to provide a theoretical basis for the production and application of oligosaccharides. Some challenges and future trends to develop green and large-scale hydrothermal pretreatment were proposed for the production of oligosaccharides.

Hydrothermal systems to obtain high value-added compounds from macroalgae for bioeconomy and biorefineries.

The search of sustainable and environmentally friendly alternatives to obtain compounds for different industrial sectors has grown exponentially. Following the principles of biorefinery and circular bioeconomy, processes in which the use of natural resources such as macroalgae biomass is prioritized are required. This review focuses on a description of the relevance, application and engineering platforms of hydrothermal systems and the operational conditions depending on the target as an innovative technology and bio-based solution for macroalgae fractionation in order to recover profitable products for industries and investors. In this sense, hydrothermal treatments represent a promising alternative for obtaining different high value-added compounds from this biomass; since, the different variations in terms of operating conditions, gives great versatility to this technology compared to other types of processing, allowing it to be adapted depending on the objective, whether it is working under sub/super critical conditions, thus expanding its field of application.

Liquid hot water as sustainable biomass pretreatment technique for bioenergy production: A review.

In recent years, lignocellulosic biomass has emerged as one of the most versatile energy sources among the research community for the production of biofuels and value-added chemicals. However, biomass pretreatment plays an important role in reducing the recalcitrant properties of lignocellulose, leading to superior quality of target products in bioenergy production. Among existing pretreatment techniques, liquid hot water (LHW) pretreatment has several outstanding advantages compared to others including minimum formation of monomeric sugars, significant removal of hemicellulose, and positive environmental impacts; however, several constraints of LHW pretreatment should be clarified. This contribution aims to provide a comprehensive analysis of reaction mechanism, reactor characteristics, influencing factors, techno-economic aspects, challenges, and prospects for LHW-based biomass pretreatment. Generally, LHW pretreatment could be widely employed in bioenergy processing from biomass, but circular economy-based advanced pretreatment techniques should be further studied in the future to achieve maximum efficiency, and minimum cost and drawbacks.

Hydrothermal pretreatment of lignocellulosic biomass for hemicellulose recovery.

The hemicellulosic fraction recovery is of interest for integrated processes in biorefineries, considering the possibility of high economic value products produced from their structural compounds of this polysaccharide. However, to perform an efficient recovery, it is necessary to use biomass fractionation techniques, and hydrothermal pretreatment is highlighted as a valuable technique in the hemicellulose recovery by applying high temperatures and pressure, causing dissolution of the structure. Considering the possibility of this pretreatment technique for current approaches to hemicellulose recovery, this article aimed to explore the relevance of hydrothermal pretreatment techniques (sub and supercritical water) as a strategy for recovering the hemicellulosic fraction from lignocellulosic biomass. Discussions about potential products to be generated, current market profile, and perspectives and challenges of applying the technique are also addressed.

Efficient short-time hydrothermal depolymerization of sugarcane bagasse in one-pot for cellulosic ethanol production without solid-liquid separation, water washing, and detoxification.

In these studies, a low-cost and energy efficiency production of cellulosic ethanol from sugarcane bagasse (SCB) using one-pot without solid-liquid separation, water washing, and detoxification was performed. Firstly, SCB was pretreated using liquid hot water as the only reagent at 210 °C for a short time (0 min), and the solid liquid ratio (SLR) was 1:20 (w/v). Then, the whole slurry of pretreated SCB was enzymatically hydrolyzed and fermented for cellulosic ethanol in one-pot. The results indicated that the one-pot preparation for ethanol achieved a high total fermentable sugar conversion of 84.52 ± 1.24%, containing 88.61 ± 1.57% of glucose and 78.01 ± 1.63% of xylose. Moreover, the ethanol yield reached 257 ± 5.51 mg/g SCB, which was 77.56 ± 1.64% of the theoretical ethanol conversion from SCB. Importantly, there was no wastewater discharge in the whole process. Overall, the present work provides an economically feasible method for ethanol production.

Evaluation of Xylooligosaccharides Production for a Specific Degree of Polymerization by Liquid Hot Water Treatment of Tropical Hardwood.

Eucalyptus pellita is known as attractive biomass, and it has been utilized for eucalyptus oil, furniture, and pulp and paper production that causes a significant amount of byproducts. Liquid hot water treatment depending on combined severity factor (CSF) was subjected to isolate hemicellulose fraction from E. pellita and to produce xylooligosaccharides (XOS). The xylan extraction ratio based on the initial xylan content of the feedstock was maximized up to 77.6% at 170 °C for 50 min condition (CSF: 1.0), which had accounted for XOS purity of 76.5% based on the total sugar content of the liquid hydrolysate. In this condition, the sum of xylobiose, xylotriose, and xylotetraose which has a low degree of polymerization (DP) of 2 to 4 was determined as 80.6% of the total XOS. The highest XOS production score established using parameters including the xylan extraction ratio, XOS purity, and low DP XOS ratio was 5.7 at CSF 1.0 condition. XOS production score evaluated using the CSF is expected to be used as a productivity indicator of XOS in the industry (R-squared value: 0.92).

Effects of Microwave-Assisted Liquid Hot Water Pretreatment on Chemical Composition and Structure of Moso Bamboo.

The effects of microwave assisted liquid hot water (MA-LHW) pretreatment on the chemical composition of Moso bamboo were investigated, and the fiber structure of pretreated residues were studied. The results showed that MA-LHW pretreatment had high selectivity for the degradation of hemicellulose in Moso bamboo, and the extracted hemicellulose could be used to prepare xylooligosaccharide through enzyme depolymerization. The degradation rates of cellulose and lignin after MA-LHW pretreatment were only 14.73% and 7.18%, which were significantly lower than those of LHW pretreatment; 155.0 mg/g xylobiose and 61.0 mg/g xylotrisoe can be obtained after enzymatic hydrolysis, and the yield of xylo-oligosaccharide reached 80.59% of the theoretical conversion rate. MA-LHW pretreatment increased the removal of hemicellulose, lignin, and other non-crystalline parts in bamboo materials, and more cellulose with crystalline structure was retained, which increased the CrI value of Moso bamboo by 14.84%. FTIR spectra showed that the characteristic peak intensity of hemicellulose was significantly reduced after MA-LHW pretreatment, which confirmed the selective degradation of hemicellulose by MA-LAW pretreatment. Moreover, MA-LHW pretreatment also destroyed O-H, C-H, C-O-C, and ß-glucoside bonds in Moso bamboo fiber, caused by the recombination and synthesis of some groups (-CH2 and C=O) of cellulose, hemicellulose, and lignin destroyed under pretreatment conditions.

Effect of sequential pretreatment combinations on the composition and enzymatic hydrolysis of hazelnut shells.

Hazelnut shells, a high lignin containing biomass, were subjected to individual and sequential liquid hot water (LHW), alkaline (AP) and dilute acid pretreatments (DAP). Among the single pretreatments, LHW demonstrated the highest cellulose recovery of 98.1%, DAP resulted in the highest hemicellulose solubilization of 56.0%, and AP of the highest lignin removal of 49.6%. Employing two-step pretreatment on hazelnut shells, in general, demonstrated an enhanced action of the second pretreatment; therefore, the sequence of the pretreatment methods had a significant impact on both substrate characteristics and enzymatic hydrolysis efficiency of biomass. In terms of delignification, AP-LHW achieved 60.7% lignin removal, while LHW-DAP showed the highest hemicellulose removal of 93.8% and DAP-LHW resulted in the highest cellulose recovery of 94.0%. Structural properties of raw and pretreated hazelnut shells were observed by FTIR. The maximum glucose recovery of 54.9% was observed in DAP-LHW pretreated samples. For this pretreatment combination, almost 1.8 MJ total energy was required to recover 10.2 g glucose. The findings indicated that complete removal of the physical barrier of lignin and hemicellulose might not be essential; partial relocation of lignin and alteration of cellulose structure may also be efficient in increasing the sugar recovery from the lignocellulosic biomass.

Liquid Hot Water Pretreatment and Enzymatic Hydrolysis as a Valorization Route of Italian Green Pepper Waste to Delivery Free Sugars.

In this work, liquid hot water pretreatment (autohydrolysis) was used to improve enzymatic hydrolysis of a commonly consumed vegetable waste in Spain, Italian green pepper, to finally produce fermentable sugars. Firstly, the effect of temperature and contact time on sugar recovery during pretreatment (in insoluble solid and liquid fraction) was studied in detail. Then, enzymatic hydrolysis using commercial cellulase was performed with the insoluble solid resulting from pretreatment. The objective was to compare results with and without pretreatment. The results showed that the pretreatment step was effective to facilitate the sugars release in enzymatic hydrolysis, increasing the global sugar yield. This was especially notable when pretreatment was carried out at 180 °C for 40 min for glucose yields. In these conditions a global glucose yield of 61.02% was obtained. In addition, very low concentrations of phenolic compounds (ranging from 69.12 to 82.24 mg/L) were found in the liquid fraction from enzymatic hydrolysis, decreasing the possibility of fermentation inhibition produced by these components. Results showed that Italian green pepper is an interesting feedstock to obtain free sugars and prevent the enormous quantity of this food waste discarded annually.

Liquid hot water treatment of rice straw enhances anaerobic degradation and inhibits methane production during in vitro ruminal fermentation.

Liquid hot water (LHW) treatment can be used to disrupt the fiber structure of rice straw. This in vitro ruminal batch culture study investigated the effect of LHW treatment on feed degradation, methane (CH4) production, and microbial populations. Rice straw was treated by LHW, and in vitro ruminal fermentation was performed using an automatic system with 72 h of incubation. Scanning electron microscopy showed that LHW treatment disrupted the physical structure of rice straw. Liquid hot water treatment decreased neutral detergent fiber and hemicellulose contents of the rice straw and increased neutral detergent solubles, water-soluble carbohydrates, and arabinose contents. Liquid hot water treatment increased dry matter degradation and volatile fatty acid concentration and decreased the acetate:propionate ratio, CH4 production, hydrogen accumulation, neutral detergent fiber degradation, and populations of protozoa, fungi, and cellulolytic bacteria. In summary, LHW treatment disrupted the cellulose-hemicellulose-lignin structure matrix of rice straw, leading to increased substrate degradability and decreased CH4 production. Therefore, the LHW treatment is a potential strategy to improve the nutritive value of forage such as rice straw and decrease the CH4 emissions in ruminants.

Engineering aspects of hydrothermal pretreatment: From batch to continuous operation, scale-up and pilot reactor under biorefinery concept.

Different pretreatments strategies have been developed over the years mainly to enhance enzymatic cellulose degradation. In the new biorefinery era, a more holistic view on pretreatment is required to secure optimal use of the whole biomass. Hydrothermal pretreatment technology is regarded as very promising for lignocellulose biomass fractionation biorefinery and to be implemented at the industrial scale for biorefineries of second generation and circular bioeconomy, since it does not require no chemical inputs other than liquid water or steam and heat. This review focuses on the fundamentals of hydrothermal pretreatment, structure changes of biomass during this pretreatment, multiproduct strategies in terms of biorefinery, reactor technology and engineering aspects from batch to continuous operation. The treatise includes a case study of hydrothermal biomass pretreatment at pilot plant scale and integrated process design.

Combined liquid hot water with sodium carbonate-oxygen pretreatment to improve enzymatic saccharification of reed.

In this work, two-stage combination of liquid hot water (LHW) and Na2CO3-O2 pretreatment was performed efficiently on reed to obtain fermentable sugar. Reed was first treated with LHW at 170 °C for 60 min and then with Na2CO3-O2. The optimal conditions for Na2CO3-O2 pretreatment were as follow: reaction temperature of 150 °C, residence time of 40 min, Na2CO3 concentration of 33.3 g/L and oxygen pressure of 0.6 MPa. The total sugar yield of 79.1% was achieved with a cellulase of 20 FPU/g-pretreated solid for 48 h. The total sugar yield improved 36.0% compared with single Na2CO3-O2 pretreatment. The combined pretreatment could avoid the loss of carbohydrate degradation. The total sugar yield was increased by 48.6% compared to only LHW pretreatment. Owing to advantages of the combined pretreatment breaking the restraint of lignin and cellulose, LHW combined with Na2CO3-O2 pretreatment was a promising method for the production of fermentable sugar.

Hot water pretreatment of lignocellulosic biomass: Modeling the effects of temperature, enzyme and biomass loadings on sugar yield.

Experimental conditions of liquid hot water (LHW) pretreatment were tested for two dedicated energy crops, Napiergrass (Pennisetum purpureum) and Energycane (Saccharum officinarum × Saccharum robustum). Both crops showed differential resistance to temperature during pretreatment and differences in response to biomass and enzyme loadings during subsequent enzymatic hydrolysis. Sugar response surfaces, for both glucose release per g pretreated biomass and as percent yield of glucose present in the initial biomass, were estimated using a General Additive Model (GAM) in R to compare non-linear sugar release as temperature, and biomass and enzyme loadings were manipulated. Compared to Napiergrass, more structural glucose is estimated to be recovered from Energycane per g of pretreated biomass under relatively less harsh pretreatment conditions, however, Napiergrass had the highest measured glucose yield. Sugar degradation products (furfural and hydroxymethylfurfural), pH, and biomass recovery differed significantly between crops across pretreatment temperatures, which could adversely affect downstream biochemical processes.

Effects of Liquid Hot Water Combined with 1, 4-Butanediol on Chemical Composition and Structure of Moso Bamboo.

The effects of liquid hot water combined with 1, 4-butanediol (LHW-BDO) on the chemical composition and structure of moso bamboo were investigated. The structure changes of moso bamboo fibers were characterized by infrared spectroscopy, X-ray diffraction, and electronic scanning electron microscopy. The results showed that the delignification rates of 1, 4-butanediol (BDO) and LHW-BDO pretreatment methods were at the same level (91.42-93.08%). However, compared with BDO pretreatment, the cellulose content in solid residue after LHW-BDO pretreatment was increased by 17.06% with a recovery rate of 75.68%, while the hemicellulose removal rate increased by 115.33% and reached 50.34%. After LHW-BDO pretreatment, the intramolecular hydrogen bonds, intermolecular hydrogen bonds, methylene bonds, and aromatic ether bonds of the fibers were broken, which contributed to the depolymerization and separation of cellulose, hemicellulose, and lignin molecules. However, LHW-BDO pretreatment does not destroy the ß-glycoside bond which links the glucose molecule inside the fiber molecule, which was also beneficial to the separation of cellulose. In addition, the amorphous zone of bamboo fibers was destroyed by the above treatments, and the fiber structure of bamboo samples mostly exists in crystalline form. The crystallinity of bamboo pretreated with LHW-BDO was increased by 32.15%. It can be found by scanning electron microscopy that the surface of the pretreated bamboo samples showed uniformly distributed bubbly protuberance.

Liquid hot water pretreatment to enhance the anaerobic digestion of wheat straw-effects of temperature and retention time.

Wheat straw is an abundant agricultural waste that is rich in lignocellulose. However, its waxy surface, highly crystallized structure, and limited surface area make it difficult to be hydrolyzed and used efficiently by microorganisms. Liquid hot water (LHW) pretreatment was studied to explore the feasibility of improving the methane yield of wheat straw in anaerobic digestion (AD). The results showed that the crosslinking structure of wheat straw was broken by LHW pretreatment. Some pores and cracks appeared on the surface of the pretreated wheat straw, increasing the microbial attachment sites. Under different hydrothermal temperatures (150-225 °C) and retention times (5-60 min), the degradation of hemicellulose ranged from 27.69 to 99.07%. The maximum methane yield (201.81 mL CH4/g volatile solids) was achieved after LHW pretreatment at 175 °C for 30 min, which was a 62.9% increase compared with non-treated straw. LHW at high temperatures such as 225 °C was not suitable for the AD of wheat straw. Methane yield results were fitted with the first-order and modified Gompertz equations to evaluate the hydrolysis rate and inhibitory effects of the pretreated materials in AD.

Anaerobic bioprocessing of wastewater-derived duckweed: Maximizing product yields in a biorefinery value cascade.

This study integrated the sugar and carboxylate platforms to enhance duckweed processing in biorefineries. Two or three bioprocesses (ethanol fermentation, acidogenic digestion, and methanogenic digestion) were sequentially integrated to maximize the carbon-to-carbon conversion of wastewater-derived duckweed into bioproducts, through a series of laboratory-scale experiments. Reactors were fed either raw (dried), liquid-hot-water-pretreated, or enzymatically-saccharified duckweed. Subsequently, the target bioproduct was separated from the reactor liquor and the residues further processed. The total bioproduct carbon yield of 0.69 ±â€¯0.07 g per gram of duckweed-C was obtained by sequential acidogenic and methanogenic digestion. Three sequential bioprocesses revealed nearly as high yields (0.66 ±â€¯0.08 g of bioproduct-C per duckweed-C), but caused more gaseous carbon (dioxide) loss. For this three-stage value cascade, yields of each process in conventional units were: 0.186 ±â€¯0.001 g ethanol/g duckweed; 611 ±â€¯64 mg volatile fatty acids as acetic acid/g VS; and 434 ±â€¯0.2 ml methane/g VS.