• Journal of the Korean Wood Science and Technology
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• v.52 no.2
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• pp.101-117
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• 2024

The conversion characteristics of the major components of Liriodendron tulipifera were investigated during acid-catalyzed organosolv pretreatment. Glucan in L. tulipifera was slowly hydrolyzed, whereas xylan was rapidly hydrolyzed. Simultaneous hydrolysis and degradation of xylan and lignin occurred; however, after complete hydrolysis of xylan at higher temperatures, lignin remained and was not completely degraded or solubilized. These conversion characteristics influence the structural properties of glucan in L. tulipifera. Critical hydrolysis of the crystalline regions in glucan occurred along with rapid hydrolysis of the amorphous regions in xylan and lignin. Breakdown of internal lignin and xylan bonds, along with solubilization of lignin, causes destruction of the lignin-carbohydrate complex. Over a temperature of 160℃, the lignin that remained was coalesced, migrated, and re-deposited on the surface of pretreated solid residue, resulting in a drastic increase in the number and content of lignin droplets. From the results, the characteristic conversions of each constituent and the changes in the structural properties in L. tulipifera effectively improved enzymatic hydrolysis in the range of 140℃-150℃. Therefore, it can be concluded that significant changes in the biomass recalcitrance of L. tulipifera occurred during organosolv pretreatment.

• 한국신재생에너지학회:학술대회논문집
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• 2009.11a
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• pp.520-520
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• 2009

Organic by-products derived from cellulose and lignin during organosolv pretreatments of yellow poplar wood (Liriodendron tulipifera) in the presence of $H_2SO_4$ and NaOH as catalysts, respectively, were subjected to various analyses to elucidate their effects on further performance of biological ethanol fermentation and provide preliminary data for the structure and utilization of organosolv lignin. Monomeric sugars amounted to ca. 2.2-7.7% in the organosoluble fraction of the organosolv pretreatment with $H_2SO_4$, while significantly low amount of sugars (0.2-0.3%) were determined in that of the organosolv pretreatment with NaOH. In case of addition of $H_2SO_4$ during organosolv pretreatment of biomass, a fermentation of the organosoluble fraction could be considered as an essential process to increase an efficiency of biomass utilization as well as yield of bioethanol. Precipitates, insoluble by-products in the solvent mixture, were also cficiency oed by diverse analytical methods and revealed that these were typically composed of a lignin moiety regardless of catalyst. According to the results of nuclear magnetic resonance (NMR), Fourier Tcinsform Infrared Spectroscopy (FT-IR) and Gel permeation chromatograp r (GPC), the main components of precipitates seem to be lignin polymers. However, their structures could be slightly modified during pretreatment and mixed with some carbohydrates by chemical bonds and/or physical associations.

• Journal of Korean Society of Environmental Engineers
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• v.39 no.10
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• pp.568-574
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• 2017

The purpose of this study was to optimize experimental conditions (time ($X_1$) (ranging of 26.36 - 93.64 min), concentration of sulfuric acid ($X_2$) (ranging of 0-2.5%) and temperature ($X_3$) (ranging of $136.4-203.6^{\circ}C$) for an organosolv pretreatment process to extract lignin from waste wood. The resulting quadratic model equation using RSM (response surface methodology) represented y (lignin yield) = $-79.89+0.91X_1+9.8X_2-2.54{\times}10^{-3}X_1{^2}-2.11X_2{^2}$. The $R^2$ (coefficient of determination) value of 0.8531 for a model indicates this model has statistically significant predictors at the 10% levels. The predictive results optimized by quadratic model produced a lignin yield of 12.46 g/100 g of dry wood under conditions of $178.2^{\circ}C$ and 2.32% $H_2SO_4$. The lignin yield was more affected by the acid catalyst concentrations than the reaction temperature, but the reaction time was not an influential factor for improving lignin extraction from waste wood in this organosolv pretreatment. According to ANOVA (analysis of variance), the significance probability (p-value) of model was smaller than 0.001 and simulation of obtained model equations showed a good reproducibility based on actual organosolv tests under optimal conditions.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.47 no.4
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• pp.21-29
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• 2015

In this study, the feasibility of utilizing wood chips from pitch pine (Pinus rigida) was evaluated for bioethanol production by an organosolv pretreatment and enzymatic saccharification. When wood chips from pitch wood were pretreated with 75% (v/v) ethanol and 1.7% sulfuric acid as a catalyst at H-factor 2000, average pulp yield was 43.3%, which pretreated wood fibers showed higher glucan (55.8%) and lower lignin (12.2%) contents than untreated control (43.9% glucan and 27.8% lignin). After enzymatic saccharification, the organosolv pulps with 56.2% delignification rate reached above 97% conversion rate of cellulose to glucose. These results indicated that increasing the delignification rate causes micro pores on the surface of organosolv pulps resulting in improved the accessibility of enzyme onto the substrate. Moreover, it was in agreement with the SEM examination of wood fibers.

• Journal of the Korean Wood Science and Technology
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• v.41 no.1
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• pp.19-32
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• 2013

In this study, outstanding white rot fungi for biodegradation of organosolv lignin were selected on the basis of their ligninolytic enzyme system. Fifteen white rot fungi were evaluated for their ability to decolorize Remazol Brilliant Blue R (RBBR) in SSC and MEB medium, respectively. Six white rot fungi (Ceriporiopsis subvermispora, Ceriporia lacerate, Fomitopsis insularis, Phanerochaete chrysosporium, Polyporus brumalis, and Stereum hirsutum) decolorized RBBR rapidly in SSC medium within 3 days. The protein contents as well as the activities of manganese peroxidase (MnP) and laccase for 6 selected fungi were determined on the SSC medium with and without organosolv lignin. Interestingly, extracellular protein concentrations were determined to relative higher for S. hirsutum and P. chrysosporium in the presence of organosolv lignin than others. On the other hands, each fungus showed a different ligninolytic enzyme pattern. Among them, F. insularis resulted the highest ligninolytic enzyme activities on incubation day 6, indicating of 1,545 U/mg of MnP activity and 1,259 U/mg of laccase activity. In conclusion, $STH^*$ and FOI were considered as outstanding fungi for biodegradation of organosolv lignin, because $STH^*$ showed high extracellular protein contents and ligninolytic enzyme activities over all, and ligninolytic enzyme activities of FOI were the highest among white rot fungi used in this study.

• Membrane and Water Treatment
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• v.11 no.1
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• pp.25-29
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• 2020

The purpose of this study was to investigate the characteristics of lignin fractionated from waste wood (WW) using a two-step process of ethanol organosolv pretreatment followed by ultrafiltration with membranes of different molecular weight cut-offs (1, 5 and 20 kDa). The different permeates obtained were characterized by fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA) and gel permeation chromatography (GPC). The analysis by FT-IR and NMR of these lignins showed that the lignin core was successfully separated from WW. TGA curves confirmed that the thermal properties of lignin fractionated by ultrafiltration were almost identical to each other. The results from GPC confirmed that fractionating of lignin was achieved by ultrafiltration. For the membrane fractionation process, values of molecular weight decreased as the cut-offs used to obtain the fractions became smaller. As a result, fractionating lignin by a two-step process allowed separating different fractions of lignin of different molecular weights yielded high purity without interference from existing pollutants in WW. The two-step process offers the possibility of using fractionated WW as an untapped source of lignin.

• Journal of the Korean Wood Science and Technology
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• v.38 no.2
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• pp.149-158
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• 2010

Organosolv pretreatments which utilized sulfuric acid, sodium hydroxide and ammonia as catalysts were conducted to screen the effective catalyst for organosolv pretreatment of Liriodendron tulipifera. The enzymatic hydrolysis was achieved effectively with sulfuric acid (74.2%) and sodium hydroxide (63.7%). They were thus considered as effective catalysts for organosolv pretreatment of L. tulipifera. The organosolv pretreatments with sulfuric acid and sodium hydroxide showed a different behavior on the reaction mechanism. The pretreatment with sulfuric acid increased the biomass roughness and pore numbers. On the other hand, the pretreatment with sodium hydroxide enhanced the surface area due to the size reduction and minor defiberization which were caused by hemicellulose degradation at an initial stage and more defiberization by lignin degradation at a later stage. The organosolv pretreatment with sodium hydroxide was performed at several different conditions to evaluate effectiveness of sodium hydroxide as a catalyst for organosolv pretreatment. According to the results of enzymatic digestibility, the changes of chemical composition and the morphological analysis of pretreated biomass, it was suggested that the pretreatment time impacted primarily on enzymatic hydrolysis. Increase in surface area during the pretreatment was a major cause for improvement in enzymatic digestibility when sodium hydroxide was used as a catalyst.

• Journal of the Korean Wood Science and Technology
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• v.16 no.4
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• pp.70-78
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• 1988

To separate and utilize the main components of hardwood (Quercus mongolica) by organosov pulping (ester pulping), chips were cooked at various conditions such as; the solvent ratio (acetic acid: ethylacetate: water, 50:25:25; 33:33:34; 25:50:25), maximum temperature (165, 170, $175^{\circ}C$), and cooking times (2, 2.5, 3 hr). The pulps were bleached by the sequences of CEDED, C/DEDED, PEDED. Lignin, sugars, and acetic acid were separated from black liquor and washing liquors. 1. The selective delignification at optimal pulp yield (43-45%) was obtained by cooking at acetic acid: ethylace tate: water ratio of 33:34:34 for 3 hr at $170^{\circ}C$. But in this case, kappa no. of the pulp was not reduced under 60 points. 2. Kappa no. of the pulp could be dropped by an acetone wash to remove reprecipitated lignin a t cooked pulp. 3. The unbleached pulps had a brightness of 45-50%, whereas the bleached pulps gave at 88-93% brightness. Tensile, burst, and tear strengths of the bleached pulps were lower than those of kraft pulp, especially in tear strength. The pulps which were bleached with CEDED sequence were higher in strengths than another bleaching sequences. 4. Lignin of 90-95%(lignin base on wood)was separated from black liquor and washing liquors, while the purified sugars and recovery of acetic acid were a low. An organic phase composed of acetic acid, ethylacetate, and water was separated to a two-phase system by proper adjustment of the solvent ratios.

• Journal of the Korean Wood Science and Technology
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• v.43 no.5
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• pp.600-612
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• 2015

We investigated the optimization of the organosolv pretreatment of yellow poplar for bioethanol production. Response surface methodology was used to determine the optimal conditions of three independent variables (reaction temperature, reaction time, and sulfuric acid (SA) concentration). Reaction temperature is the most significant variable in the degradation of xylan and lignin in the presence of an acid catalyst, and ethanol production increased with a decrease in the lignin content. The highest ethanol concentration ($42.80g/{\ell}$) and theoretical ethanol yield (98.76%) were obtained at $152^{\circ}C$ (2.5 bar) with 1.6% SA for 16 min. However, because of excessive degradation of the raw material, the overall ethanol yield was less than under other pretreatment conditions which has approximately 50% of WIS recovery rate after pretreatment. The optimal conditions for the maximum overall ethanol yield ($146^{\circ}C$ with 1.22% SA for 15.9 min) were determined with a predicted yield of 17.11%, and the experimental values were very close (17.15%). Therefore, the quadratic model is reliable.

• Korean Chemical Engineering Research
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• v.59 no.1
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• pp.54-59
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• 2021

The pretreatment of cellulosic biomass is essentially needed because it has more lignin compared with a starch biomass. Ethanol as an organosolv for pretreatment can easily separate some components which can inhibit enzymatic hydrolysis and be re-usuable by distillation. The flow-through process have some strength, separating components continuously, development for scale up. In this research, two-kinds (wheat straw, miscanthus) of biomass was pretreated for development of enzymatic hydrolysis by adoption of pretreatment process of corn stover.