• 제목/요약/키워드: concentrated acid hydrolysis

검색결과 26건 처리시간 0.024초

1H-NMR 분광분석을 통한 진한 산 가수분해 반응 2차 반응 조건 분석 (Analysis of secondary reactions in concentrated sulfuric acid hydrolysis of hollocellulose by 1H-NMR spectroscopy)

  • 이재성;신수정
    • 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.

Optimization of Concentrated Acid Hydrolysis of Waste Paper Using Response Surface Methodology

  • Jung, Ji Young;Choi, Myung Suk;Yang, Jae Kyung
    • 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.

$^1H$-NMR에 의한 Xylan의 황산가수분해 과정에서 나타나는 반응 동력학 연구 (Kinetic Study of Xylan Hydrolysis and Decomposition in Concentrated Sulfuric Acid Hydrolysis Process by $^1H$-NMR Spectroscopy)

  • 조대행;김용환;김병로;박종문;성용주;신수정
    • 펄프종이기술
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    • 제43권3호
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    • pp.52-58
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    • 2011
  • Proton-NMR spectroscopic method was applied to kinetic study of concentrated sulfuric acid hydrolysis reaction, especially focused on 2nd step of acid hydrolysis with deferent reaction time and temperature as main variables. Commercial xylan extracted from beech wood was used as model compound. In concentrated acid hydrolysis, xylan was converted to xylose, which is unstable in 2nd hydrolysis condition, which decomposed to furfural or other reaction products. Without neutralization steps, proton-NMR spectroscopic analysis method was valid for analysis of not only monosaccharide (xylose) but also other reaction products (furfural and formic acid) in acid hydrolyzates from concentrated acid hydrolysis of xylan, which was the main advantages of this analytical method. Higher temperature and longer reaction time at 2nd step acid hydrolysis led to less xylose concentration in xylan acid hydrolyzate, especially at $120^{\circ}C$ and 120 min, which meant hydrolyzed xylose was converted to furfural or other reaction products. Loss of xylose was not match with furfural formation, which meant part of furfural was degraded to other undetected compounds. Formation of formic acid was unexpected from acidic dehydration of pentose, which might come from the glucuronic acid at the side chain of xylan.

진한 황산 가수분해 반응조건에서 xylose와 glucuronic acid의 반응 특성 (Characteristics of xylose and glucuronic acid at concentrated sulfuric acid hydrolysis)

  • 조대행;김용환;박종문;심재훈;김병로;신수정
    • 펄프종이기술
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    • 제44권3호
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    • pp.9-14
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    • 2012
  • Formed fermentation inhibitors during acid saccharification leads to poor alcohol production based on lignocellulosic bio-alcohol production process. In this work, it is focused on the formation of fermentation inhibitors from xylan, which is influenced by reaction tempearature and time of acidic sacharifiaction of xylose and glucuronic acid. In second step of concentrated acid hydrolysis, part of xylose and glucuronic acid was converted to furfuraldehyde and formic acid by dehydration and rearrangement reactions. Furfural was form from xylose, which was highly sensitive to reaction temperature. Formic acid was come from both xylose and glucuronic acid, which supposed to main inhibitor in biobutanol fermentation. Reaction temperature of second hydrolysis was main variables to control the furfural and formic acid generation. Careful control of acid saccharification can reduce generation of harmful inhibitors, especially second step of concentrated sulfuric acid hydrolysis process.

진한 황산 가수분해에서 2단계 산 가수분해 반응에서 일어나는 반응 동역학(Kinetics)을 $^1H-NMR$을 사용한 연구 (Kinetics Study of $2^{nd}$ Hydrolysis in Concentrated Sulfuric Acid Hydrolysis Process by $^1H-NMR$ Spectroscopy)

  • 신수정;김용환;조대행;성용주;김병로;조남석
    • 한국펄프종이공학회:학술대회논문집
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    • 한국펄프종이공학회 2011년도 춘계학술발표회 논문집
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    • pp.93-99
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    • 2011
  • Proton-NMR spectroscopic method was applied to kinetics study of concentrated sulfuric acid hydrolysis reaction. Xylan was used as model compounds. Without neutralization steps in proton-NMR methods, this analysis method is valid for analysis of xylose, furfural and formic acid in acid hydrolyzates.

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Beta-D-Galactosidase에 의한 유청에 함유된 유당의 가수분해 (Hydrolysis of Lactose in Whey by the BetavD-Galactosidase)

  • 최미진;허태련
    • 한국미생물·생명공학회지
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    • 제20권1호
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    • pp.46-52
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    • 1992
  • 농축유청으로부터 유청음료 제조를 위한 최적조건을 조사하기 위해 역삼투장치(reverse osmosis system)를 사용하여 치즈유청 속의 유당을 농축한 수 $\beta$-D-glactosidase로 가수분해시켜 그 분해정도를 HPLC(high performance liquid chromatography)로 측정하였다. 유당의 가수분해 정도는 농축적 유청, 2배 농축 유청과 3배 농축 유청 순으로 가수분해되었고 일정량의 효소첨가에 의해 농축된 염이 $\beta$-D-Galactosidase에 대한 약간의 저해작용을 일으켰다.

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A Complete, Reductive Depolymerization of Concentrated Sulfuric Acid Hydrolysis Lignin into a High Calorific Bio-oil using Supercritical Ethanol

  • Riaz, Asim;Kim, Jaehoon
    • KEPCO Journal on Electric Power and Energy
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    • 제2권3호
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    • pp.447-452
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    • 2016
  • It is imperative to develop an effective pathway to depolymerize lignin into liquid fuel that can be used as a bioheavy oil. Lignin can be converted into liquid products either by a solvent-free thermal cracking in the absence air, or thermo-chemical degradation in the presence of suitable solvents and chemicals. Here we show that the solvent-assisted liquefaction has produced promising results in the presence of metal-based catalysts. The supercritical ethanol is an efficient liquefaction solvent, which not only provides better solubility to lignin, but also scavenges the intermediate species. The concentrated sulfuric acid hydrolysis lignin (CSAHL) was completely liquefied in the presence of solid catalysts (Ni, Pd and Ru) with no char formation. The effective deoxy-liquefaction nature associated with scEtOH with aid hydrodeoxygenation catalysts, resulted in significant reduction in oxygen-to-carbon (O/C) molar ratio up to 61%. The decrease in oxygen content and increase in carbon and hydrogen contents increased the calorific value bio-oil, with higher heating value (HHV) of $34.6MJ{\cdot}Kg^{-1}$. The overall process is energetically efficient with 129.8% energy recovery (ER) and 70.8% energy efficiency (EE). The GC-TOF/MS analysis of bio-oil shows that the bio-oil mainly consists of monomeric species such as phenols, esters, furans, alcohols, and traces of aliphatic hydrocarbons. The bio-oil produced has better flow properties, low molecular weight, and high aromaticity.

백합나무를 이용한 고농도 단당류 생산을 위한 산 가수분해 특성 연구 (Acid Hydrolysis Characteristics of Yellow Poplar for High Concentration of Monosaccharides Production)

  • 신수정;박종문;조대행;김용환;조남석
    • Journal of the Korean Wood Science and Technology
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    • 제37권6호
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    • pp.578-584
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    • 2009
  • 백합나무 목분으로 고농도 단당류를 생산하기 위하여 진한 황산을 사용하는 산 가수분해 특성을 연구하였다. 목분과 황산의 비율을 달리하거나 2차 가수분해의 온도와 시간을 달리하여 당화액 제조의 최적 조건을 탐구한 결과, 1차 가수분해의 목분과 72% 황산 비율은 1 : 2.61(w/w)였으며, 2차 가수분해 온도와 시간은 $105^{\circ}C$에서 70분 가수분해 조건이었다. 이때 생성된 당화액의 농도는 glucose가 44.8 g/L였고 xylose는 25.2 g/L였다. 산 가수분해를 통하여 얻어진 당화액을 발효할 때 발효 저해물질로 알려진 furfural, 5-HMF (5-hydroxymethylfurfural), 저분자량 페놀성 화합물들이 생성되었는데 furfural과 5-HMF는 2차 가수분해 온도가 높아짐에 따라, 그리고 반응시간이 길어짐에 따라 생성량이 증가하였다. $110^{\circ}C$ 2차 가수분해 조건에서 반응시간이 40분을 지남에 따라서 xylose농도는 감소하였고 glucose 농도는 일정하였는데, xylose는 생성속도보다 furfural로 전이 속도가 더 빠른 것으로 생각되고, glucose의 경우 생성속도와 5-HMF로 전이속도가 비슷하여 농도가 일정하게 나타났다.

Changes in Solution Properties of Pectins by Enzymatic Hydrolysis of Sidechains

  • Hwang, Jae-Kwan;Jozef L. Kokini
    • 한국식품영양과학회지
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    • 제24권3호
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    • pp.389-395
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    • 1995
  • The neutral sugar sidechains of apple pectins were hydrolyzed by commercial hemicellulase produced from Aspergillus niger, and the corresponding changes in solution viscosity were investigated in dilute(cc*) pectin solutions. Pectinase activity included in hemicellulases was removed by Epoxy-activated Sepharose 6B affinity chromatography using polygalacturonic acid as a ligand. Enzymatic hydrolysis of sidechains did not affect the specifc viscosity of dilute(0.5%) pectin solutions, while viscosity significantly decreased in concentrated(2.0∼6.0%) region. These results strongly suggest that the sidechains of pectins exists as an entangled state in concentrated solutions. It was also found that in the concentrated region the extent of viscosity reduction was dependent on pectin concentrations.

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3,3-Bis(methylthio)-2-propen-1-phenyl-1-one 유도체들의 산-촉매 가수분해 반응 메카니즘 (Acid-Catalyzed Hydrolysis Mechanism of 3,3-Bis(methylthio)-2-propen-1-phenyl-1-one Derivatives)

  • 권기성;박찬훈;성낙도
    • 대한화학회지
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    • 제41권3호
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    • pp.138-143
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    • 1997
  • 30$^{\circ}C$의 센(-Ho < 2.23) 과염소산 수용액 속에서 3,3-bis(methylthio)-2-propen-1-phenyl-1-one 유도체들의 산-촉매 가수분해 반응을 속도론적으로 연구하였다. 치환기 효과, 가수분해 생성물의 분석, Bunnett식 및 Bunnett-Olsen식의 hydration 파라미터(${\omega}$${\phi}$)로부터 3.8 M 이하의 묽은 산 용액에서는 A-1형 반응($3.3 >{\omega},\;0.58 > {\phi}$${\rho} < 0$)이 그리고 3.8 M 이상의 진한 산 용액에서는 A-2형 반응($0 <{\omega},\;0 < {\phi}$${\rho} > 0$) 메카니즘으로 산-촉매 가수분해 반응이 일어난다.

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