• Title/Summary/Keyword: concentrated acid hydrolysis

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

  • Lee, Jai-Sung;Shin, Soo-Jeong
    • 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.

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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    • 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.

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

  • Cho, Dae-Haeng;Kim, Yong-Hwan;Kim, Byung-Ro;Park, Jong-Moon;Sung, Yong-Joo;Shin, Soo-Jeong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.43 no.3
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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.

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

  • Cho, Dae-Haeng;Kim, Yong-Hwan;Park, Jong-Moon;Sim, Jae-Hoon;Kim, Byung-Ro;Shin, Soo-Jeong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.44 no.3
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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.

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

  • Shin, Soo-Jeong;Kim, Yong-Hwan;Cho, Dae-Haeng;Sung, Yong-Joo;Kim, Byung-Ro;Cho, Nam-Seok
    • Proceedings of the Korea Technical Association of the Pulp and Paper Industry Conference
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    • 2011.04a
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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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Hydrolysis of Lactose in Whey by the BetavD-Galactosidase (Beta-D-Galactosidase에 의한 유청에 함유된 유당의 가수분해)

  • 최미진;허태련
    • Microbiology and Biotechnology Letters
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    • v.20 no.1
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    • pp.46-52
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    • 1992
  • The optimum condition for the developement of a whey beverage from the concentrated whey was studied. Reverse osmosis system was used to obtain concentrated lactose from cheese whey. The hydrolysis degree of lactose by $\beta$-D-galactosidase was determined using HPLC (high performance liquid chromatography). The order of hydrolysis degree was 1:1, 2:l and 3:l concentrated lactose. It resulted from the concentrated salt which slightly inhibited $\beta$-D-galactosidase with constant enzyme dosage. The optimum condition for enzyme dosage was 2% in non-concentrated lactose, 3% in 2:l and 3% in 3:l concentrated lactose after 4 hours of reaction. When the 3:l concentrated lactose was used, more than 70% was hydrolyzed by 3% enzyme dosage. Furthermore the change of fermented whey by lactic acid bacteria was investigated. Based on the result of sensory test, the most favorable response was obtained at pH 4.2 and titratable acidity of 0.7% about 6 hours of fermentation at $37^{\circ}C$ with 2%: thermophilic starter.

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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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    • v.2 no.3
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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.

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

  • Shin, Soo-Jeong;Park, Jong-Moon;Cho, Dae Haeng;Kim, Yong Hwan;Cho, Nam-Seok
    • Journal of the Korean Wood Science and Technology
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    • v.37 no.6
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    • pp.578-584
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    • 2009
  • We investigated acid hydrolysis characteristics of yellow poplar woodmeal with concentrated sulfuric acid for high concentration of monosaccharides production. Woodmeal to 72% sulfuric acid ratio (w/w), $2^{nd}$ hydrolysis temperature and time were main variables for finding optimum reaction condition. Optimum woodmeal to 72% sulfuric acid ratio was 1 : 2.61 (w/w) and $2^{nd}$ hydrolysis temperature and time was $105^{\circ}C$ and 40 min as 44.8 g/L of glucose and 25.2 g/L of xylose in hydrolysis solution. In this acid hydrolysis solution, furfural, 5-HMF, low molecular weight phenolic compounds were identified. Furfural and 5-HMF concentration were increased as increasing $2^{nd}$ hydrolysis time. More than 40 min of $2^{nd}$ hydrolysis at $110^{\circ}C$, xylose concentration was decreased but glucose concentration was leveled out because xylose to furfural reaction was faster than xylan to xylose, but cellulose to glucose reaction was similar rate with glucose to 5-HMF at that $2^{nd}$ hydrolysis reaction condition.

Changes in Solution Properties of Pectins by Enzymatic Hydrolysis of Sidechains

  • Hwang, Jae-Kwan;Jozef L. Kokini
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.24 no.3
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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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Acid-Catalyzed Hydrolysis Mechanism of 3,3-Bis(methylthio)-2-propen-1-phenyl-1-one Derivatives (3,3-Bis(methylthio)-2-propen-1-phenyl-1-one 유도체들의 산-촉매 가수분해 반응 메카니즘)

  • Kwon, Ki Sung;Park, Chan Hun;Sung, Nack Do
    • Journal of the Korean Chemical Society
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    • v.41 no.3
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    • pp.138-143
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    • 1997
  • Acid-catalyzed hydrolysis of 3,3-bis(methylthio)-2-propen-1-phenyl-1-one derivatives were studied kinetically in concentrated aqueous hydroperchloric acid(-Ho < 2.23) at $30^{\circ}C.$ The substituent effect, analysis of hydrolysis product, hydration $parameter({\omega} & {\phi}$) from the Bunnett equation and the Bunnett-Olsen equation on the rate indicate that the acid-catalyzed hydrolysis of the substrates below 3.8 M hydroperchloric acid media occurs through A-1 type reaction($3.3 >{\omega},\;0.58 >{\phi} & {\rho}< 0$) mechanism and above 3.8 M hydroperchloric acid, the reaction proceeds A-2 type reaction($0 <(\omega)$, $0 <{\phi} & (\rho)> 0$) mechanism.

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