• 펄프종이기술
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• 제46권3호
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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.

• 펄프종이기술
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• 제43권4호
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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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• 제41권2호
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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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• 제40권6호
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• pp.389-396
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• 2012

본 연구는 산 촉매에 의한 자이란 분해속도를 분석하는 것으로 $120^{\circ}C$에서 60분 동안 가수분해를 수행하여 자이란 분해속도를 조사하였다. 산 촉매로는 황산, 옥살산, 말레산을 사용하였다. 자이란 분해에 관여하는 분해속도상수($k_1$)는 산 농도에 비례하여 증가하였으며 이것은 산 농도가 증가할수록 자이란 가수분해가 빠르게 진행된다는 것을 의미한다. 황산, 옥살산, 말레산 중에서 자이란에서 자이로스로 분해되는 속도는 황산을 촉매로 사용하였을 때 가장 높았다. 하지만 수소농도인 pH를 기준으로 하였을 때, 즉 같은 pH 조건에서 가수분해를 수행하였을 때 자이란에서 자이로스로 분해되는 속도는 옥살산, 말레산과 같은 dicarboxylic acid 촉매에서 황산을 사용하였을 때 보다 높은 분해속도상수를 나타냈다.

• 펄프종이기술
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• 제48권3호
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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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• 제52권2호
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• pp.226-232
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• 2014

본 연구에서는 $120{\sim}150^{\circ}C$에서 다양한 산 촉매에 의한 자이란 가수분해 거동을 조사하였다. 또한 자이란에서 자이로스 생성과 자이로스로부터 푸르푸랄 분해에 대한 kinetic 인자를 분석하였다. 높은 반응온도와 산 촉매 농도는 자이란 가수분해와 자이로스 분해를 촉진하였다. 최대 반응속도상수($k_1$)에 대한 가수분해 조건은 산 촉매에 따라 다르게 나타났다. 황산, 옥살산, 말레산 중에서 자이란 반응속도상수($k_1$)는 황산 100 mM로 $120^{\circ}C$에서 반응하였을 때 $0.0241min^{-1}$로 가장 높게 나타났다. 하지만 황산은 옥살산, 말레산과 비교하여 자이로스 분해를 더욱 유도하여 상대적으로 높은 푸르푸랄을 생성하였다. 자이란 분해에 관여하는 활성화 에너지는 황산에서 가장 높게 나타났다.

• Journal of the Korean Wood Science and Technology
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• 제17권3호
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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.

• 농업과학연구
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• 제36권2호
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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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• 제13권3호
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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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• 제41권1호
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• pp.1-11
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• 2013

본 연구에서는 은수원사시나무의 산 당화공정에서 생성되는 고형 부산물의 화학적, 구조적 특성을 관찰하였다. 산 가수분해는 황산과 염산을 사용하였고, 1차 가수분해농도를 72%, 36%, 18%로 변화를 주었고, 2차 가수분해에서 4%로 동일하게 희석하였다. 가수분해 후 액상 가수분해액과 고형 부산물을 각각 분리하였고 고형 부산물을 각각 RS72, RS36, RS18, RC36, RC18이라고 하였다. 황산의 농도가 높아짐에 따라 생성된 고형부산물은 감소(71.2~21.4%)하였지만, 염산의 농도는 고형 부산물의 생성량(65.0~67.0%)에 큰 영향을 주지 않았다. 또한 RS36과 RS18은 고형 부산물 질량 대비 23.6%, RC36과 RC18은 각각 25.6%, 27.3%가 리그닌으로 이루어져 있었다. 고형 부산물의 열분해산물 분석 결과 Levoglucosan, Furfural 등 탄수화물 유래 물질과 리그닌 유래 물질인 Guaiacol, Syringol 등이 검출되었지만 RS72에서는 리그닌 유래 물질만이 검출되었다. 또한 열중량분석결과 고형 부산물 내 리그닌 함량이 높아질수록 다량의 탄이 생성되고 최대 중량 감소율이 감소하여 염산에 비해 황산이, 또한 산의 농도가 높을수록 화학적으로 축합된 구조를 형성하는 것을 확인하였다.