• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.46 no.3
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• pp.37-43
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• 2014

Kinetics of holocellulose hydrolysis in concentrated sulfuric acid was analyzed using $^1H$-NMR spectroscopy with different reaction time, temperature and acid concentration in secondary hydrolysis. In this work, reaction condition of secondary hydrolysis was similar to concentrated sulfuric acid process with electrodialysis or simulated moving bed chromatography process for sulfuric acid recycling. By $^1H$-NMR spectroscopy, acid hydrolyzates from higher secondary acid hydrolysis (25-35% acid concentration) was successfully analyzed without any difficulties in neutralization or adsorption of acid hydrolyzate to solid salt. Higher acid concentration, higher temperature and longer reaction time led to more cellulose for glucose conversion but accompanied with glucose to galactose isomerization, glucose to unknown compounds and degradation of glucose to organic acid via furans.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.43 no.4
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• pp.67-75
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• 2011

Sulfuric acid hydrolysis is a typical approach for producing cellulose nanocrystals. The method has been widely used, but it has a disadvantage of low yield of cellulose nanocrystals compared to mechanical method. To expand the application of cellulose nanocrystals in practical, we should be able to produce them with higher yield and the controlled properties. In this study, therefore, we intended to investigate the effect of sulfuric acid hydrolysis condition on the characteristics of the prepared cellulose nanocrystals. The concentration of sulfuric acid, temperature and hydrolysis time were varied, and the yield as well as diverse properties including the morphology, size and zeta potential were examined. We could obtain cellulose nanocrystals up to 70% of yield and found that the properties were dependent on the reaction condition. It would be helpful to select an appropriate condition for producing cellulose nanocrystals.

• Journal of the Korean Wood Science and Technology
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• v.41 no.2
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• pp.87-99
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• 2013

Waste paper stands for the major biodegradable organic fraction of most of municipal solid waste. The potential of waste paper for glucose production was investigated in this current work. The pretreatment was accomplished by first subjecting waste paper to disintegration time (30 s), followed by ink removal of disintegrated waste paper using an deinking agent. Concentrated acid hydrolysis of waste paper with sulfuric acid was optimized to maximize glucose conversion. The concentrated acid hydrolysis conditions for waste paper (disintegrated time: 30 s, deinking agent loading : 15 ml) were optimized by using central composite design and response surface methodology. The optimization process employed a central composite design, where the investigated variables were acid concentration (60~80%), loading sulfuric acid (1~5 ml) and reaction time (1~5 h). All the tested variables were identified to have significant effects (p < 0.05) on glucose conversion. The optimum concentrated acid hydrolysis conditions were acid concentration of 70.8%, loading sulfuric acid of 3.2 ml and a reaction time of 3.6 h. This research of concentrated acid hydrolysis was a promising method to improve glucose conversion for waste paper.

• Journal of the Korean Wood Science and Technology
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• v.40 no.6
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• pp.389-396
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• 2012

In this study, we investigated the kinetics of acid-catalyzed hydrolysis of xylan over a 60 min at $120^{\circ}C$. Sulfuric, oxalic and maleic acids were used as acid catalyst for hydrolysis. The calculated degradation rate constants ($k_1$) showed a correlation with the acid concentration, meaning that the stronger the acid, the higher the xylan degradation rate. Among sulfuric, oxalic and maleic acid catalyzed hydrolysis, the xylan degradation rate to xylose was highest with sulfuric acid. At equivalent solution pH, acid catalyzed hydrolysis was proportional to $H^+$ concentration. The $k_1$ of dicarboxylic acid such as oxalic and maleic acid was higher than that of sulfuric acid at same pH values during hydrolysis.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.48 no.3
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• pp.57-65
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• 2016

Indigo (Polygonum tinctorium L.) is a typical blue dye which had been used from ancient times. This study was going to shade the complicated traditional methods extracting indigo dye by the fermentation and producing as adsorbate on calcium hydroxide, which says so called as the 'Indigo lime'. Accordingly we were going to make indigo through the hydrolysis of the hot water extractives of indigo leaves simply. During hot-water extraction, ${\beta}$-glucosidase which required hydrolysis of the linkage between indigo and glucose was not activated. To achieve this goal, indican was acid-hydrolyzed to glucose and indigo. The acetic acid, citric acid, hydrochloric acid, and sulfuric acid were used for the hydrolysis of hot water extractives. The hydrolysis conditions of extractives performed in water bath at $80^{\circ}C$ for 120 minutes and in an autoclave for 120 minutes. In the acid hydrolysis of extracted indican by hot water, the indican yields of acetic acid and hydrochloric acid hydrolysis were higher than sulfuric acid in water bath. Also, the indican yield of hydrochloric acid hydrolysis was better than sulfuric acid in autoclave. The hot water extracted indican was confirmed by HPLC analysis and its structure was confirmed by UV-Vis and FT-IR spectroscopy, compared with isolated indigo and commercial synthesized indigo. This improved extraction and hydrolysis methods can be replace the traditional indigo making method.

• Korean Chemical Engineering Research
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• v.52 no.2
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• pp.226-232
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• 2014

In this study, we investigated kinetic model for the acid-catalyzed xylan hydrolysis at temperature $120{\sim}150^{\circ}C$. Also, we analyzed the kinetic parameters for xylose production and furfural decomposition. The hydrolysis of xylan and the degradation of xylose were promoted by high reaction temperature and acid concentration. The optimal hydrolysis condition for the highest reaction rate constants ($k_1$) was different depending on the acid catalysts. Among sulfuric, oxalic and maleic acid, the xylan reaction rate constants ($k_1$) to xylose had the highest value of $0.0241min^{-1}$ when 100 mM sulfuric acid was used at $120^{\circ}C$. However, sulfuric acid induced more xylose degradation compared to oxalic and maleic acid hydrolysis. The activation energy for xylan degradation was the highest when sulfuric acid was used.

• Journal of the Korean Wood Science and Technology
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• v.17 no.3
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• pp.1-7
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• 1989

This study was performed to obtain the optimal condition that hydrolyzed exploded pine(Pinus densiflora), oak(Quercus serrata) and birch wood(Betula platyphylla var. japonica) by using sulfuric acid. The results obtained were summarized as follows: In hydrolysis of wood meal with sulfuric acid. maximum yield of sugar appeared that pine was 12 hours. oak and birch were 24 hours with 65% sulfuric acid. Futhermore, when wood meal and exploded woods were hydrolyzed with 65% sulfuric acid at $23^{\circ}C$ for 6 hours(primary hydrolysis), diluted to 3% and hydrolyzed again at $100^{\circ}C$ for 2 hours(secondary hydrolysis), the maximum sugar yield of wood meals were 6 hours. those of higher steam exploded pine wood was 3 hours. of lower steam exploded oak and birch woods were 6 hours. The sugar analyses of exploded wood showed that the amount of arabinose and xylose residue rapidly decreased. content of nemicelluose decreased with increase of steaming time and pressure.

• Korean Journal of Agricultural Science
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• v.36 no.2
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• pp.225-232
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• 2009

The ratio of saccharification and formation of furans during the acid hydrolysis of agar with oxalic acid and sulfuric acid were examined base on the contents of the agar and acids. The ratio of saccharification in oxalic acid appeared to be 51~59% somewhat higher than 49~61% of sulfuric acid. Formation of the furans during the acid hydrolysis increased proportional to the contents of agar and acid. The relative formation ratio was high 10~47% for furfural (FUR) and 15~29% for hydroxy-methyl furfural (HMF) in 0.5~1.25% sulfuric acid rather than those of oxalic acid. When comparing the removal efficiency of the furans using an alkali treatment, steam stripping and hydrophobic resins, FUR was eliminated 60% by the alkali treatment, 62~90% by steam stripping and 71~75% by Amberlite XAD4 and 7HP, while HMF was removed to low levels of 10.5%, 4~17% and 13~25%, respectively. The loss of reducing sugar was also observed in process of the removal of furans, and the loss rate was the level of 2~4% in alkali treatment, 11~16% in steam stripping and 7~9% in Amberlite resins.

• KSBB Journal
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• v.13 no.3
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• pp.312-319
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• 1998

The dilute-acid pretreatment/hydrolysis of hemicellulose in oak wood using a percolation reactor was investigated. The experimental conditions ranged 160∼180$^{\circ}C$ and 0.05∼0.2 wt.% sulfuric acid. XMG(xylan+mannan+galactan) recovery was higher when sulfuric acid was used as leaching solvent than water. Also it was important for high XMG recovery to keep leaching temperature higher after reaction. XMG recovery was decreased as the size of wood chips was increased. At an optimum condition (reaction condition= 170$^{\circ}C$, 0.1% sulfuric acid, 1ml/min, 10min, leaching condition=0.1% sulfuric acid, 2mL/min, 20 min), the product yield and the sugar concentration were about 92% and 2.7%, respectively.

• Journal of the Korean Wood Science and Technology
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• v.41 no.1
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• pp.1-11
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• 2013

In this study, we investigated chemical characteristics of solid residues obtained from inorganic acid hydrolysis of hybrid poplar (Populus alba ${\times}$ glandulosa). Different concentration (72, 36, 18%) of sulfuric acid and hydrochloric acid were used for first hydrolysis step and second hydrolysis step were carried out after equally dilution to 4%. Solid residues after consecutive two step hydrolysis were named to RS72 (Residue from Sulfuric acid 72%), RS36, RS18, as well as RC36 (Residue from hydroChloric acid 36%) and RC18, respectively. The yield of RS decreased from 71.2% to 21.4% with increasing sulfuric acid concentration in the first hydrolysis step, whereas that of RC showed little difference (67.0% to 65.0%), irrespective of hydrochloric acid concentration. The lignin content in solid residue was 23.6% for both of RS36 and RS18, 25.6% for RC36 and 27.3% for RC18, respectively. The results of pyrolyzer-GC/MS showed that 24 cellulose derivatives (Levoglucosan, Furfural) and 21 lignin derivatives (Guaiacol, Syringol) were detected. Thermogravimetric analysis indicated that the yield of char increased and maximum wieght loss rate decreased with increasing lignin portion of solid residue. Therefore, structure of lignin was condensed effectively by sulfuric acid and by high concentration of acid.