• Journal of the Korean institute of surface engineering
• /
• v.53 no.3
• /
• pp.87-94
• /
• 2020

Herein, sulfonated carbon nanotubes (CNT) have been prepared in dilute sulfuric acid (H₂SO₄) via a novel sulfonation approach based on gas-liquid interfacial plasma (GLIP) at room temperature. The sulfonic acid groups and total acid groups densities of CNT after GLIP treatment in 2 M H₂SO₄ for 45 min can reach to 0.53 mmol/g and 3.64 mmol/g, which is higher than that of sulfonated CNT prepared under 0.5 M / 1 M H₂SO₄. The plasma sulfonated CNT has been applied as catalysts for the conversion of microcrystalline cellulose to glucose. The effect of hydrolysis temperature and hydrolysis time on the conversion rate and product distribution have been discussed. It demonstrates that the total conversion rate of cellulose increasing with hydrolysis temperature and hydrolysis time. Furthermore, the GLIP sulfonated CNT prepared in 2 M H₂SO₄ for 45 min has shown high catalytic stability of 85.73 % after three cycle use.

• New & Renewable Energy
• /
• v.19 no.4
• /
• pp.11-19
• /
• 2023

Levulinic acid (LA) derived from cellulosic biomass, serves a crucial intermediate that can be used in various chemical conversions. This study focused on optimizing the production of LA using two types of pretreated rice husk (de-ashed and delignificated cellulosic biomass) in a batch reaction system through catalytic conversion with sulfuric acid. To determine the optimal conditions, the conversions of glucose and α-cellulose were examined to compare the effects of pretreatment on the rice husk. The experimental parameters covered a broad spectrum, including temperatures ranging from 140℃ to 200℃, a reaction time was up to 600 minutes, and a substrate to catalyst (acid solution) ratio of 100 g/L. The highest LA yield was 44.8%, achieved from de-ashed rice husk with 3.0 wt.% of sulfuric acid at 180℃ and with a reaction time of 180 minutes. In the case of the delignificated rice husk, a LA yield of 43.6% was obtained with 3.0 wt.% of sulfuric acid at 200℃ and with reaction time of 30 minutes.

• Journal of Korea Technical Association of The Pulp and Paper Industry
• /
• v.45 no.6
• /
• pp.17-23
• /
• 2013

The reduction of metal ion from the cotton linter for the preparation of NMMO (N-methylmorpholine N-oxide)-based dissolving pulp was investigated. The NMMO-based dissolving pulp was usually used for the manufacture of high quality fabrics, and need to have high alpha cellulose content and high brightness. NMMO, which is environmentally friendly, and reusable after recovering process, is very sensitive to the metal ions such as Cu, Fe, Mg, and Cr. Electron beam, sulfuric acid, acetic acid, and ozone treatment before bleaching were used and the concentration changes of the metal ions were compared to that of EDTA, a chelating agent. It was found that both acid treatments (sulfuric and acetic acid) were very effective and comparable to EDTA treatment at the same dosage in metal ion reduction, but electron beam and ozone treatment were not. The sulfuric acid treatment turned out to be effective in metal ion reduction, and most inexpensive.

• Journal of Ginseng Research
• /
• v.17 no.2
• /
• pp.139-144
• /
• 1993

The method for colorimetric determination of acidic polysaccharide from Panax ginseng was investigated. It is possible to apply the method of carbazole-sulfuric acid to determination of pectin, and also to measure the amount of pectin in the mixture of various high molemlu compounds such as starch. cellulose and gum, etc. When the method of carbazole-sulfuric acid was applied to determine the amount of acidic polysaccharide, optical density at 525 nm increased linearly with an increase in the concentration of pure acidic polysaccharide. Effective extraction temperature with water for the determination of the amount of ginseng acidic polysaccharide (GAP) was $80{\circ}C$. In order to separate or concentrate GAP it was appropriate to precipitate the extract only once with 80% ethyl alcohol. GAP was very stable at $100{\circ}C$ for 4 hrs in aqueous solution and between pH values of 5.0~ 12.0.

• Journal of Korea Technical Association of The Pulp and Paper Industry
• /
• v.41 no.5
• /
• pp.26-32
• /
• 2009

As a part of utilizing the nanocellulose (NC) from lignocellulosic components of wood biomass, this paper reports preliminary results on the products of sulfuric acid hydrolysis. The purpose of this study was to investigate the morphology of both NC and micro-sized cellulose fiber (MCF) isolated by acid hydrolysis from commercial microcrystalline cellulose (MCC). Field emission.scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were employed to observe the acid hydrolysis suspension, NC, and MCF. The electron microscopy observations showed that the acid hydrolysis suspension, before separation into NC and MCF by centrifugation, was composed of nano-sized NCs and micro-sized MCFs. The morphology of isolated NCs was a whisker form of rod-like NCs. Measurements of individual NCs using TEM indicated dimensions of 6.96$\pm$0.87 nm wide by 178$\pm$55 nm long. Observations of the MCFs showed that most of the MCC particles had de-fibered into relatively long fibers with a diameter of 3-9 ${\mu}m$, depending on the degree of acid hydrolysis. These results suggest that proper technologies are required to effectively realize the potentials of both NCs and MCFs.

• Journal of Korea Technical Association of The Pulp and Paper Industry
• /
• v.35 no.1
• /
• pp.41-47
• /
• 2003

Recently, interest in utilization plan of recycling paper have been enhanced. Therefore, this research aimed to develop the manufacture process of cellulose acetate using old newsprint by acetosolv pulping process. And the manufactured cellulose acetate was also analyzed, especially based on chemical properties. The summarized results in this research were as follows; Reaction time, kind and amount of catalyst, and ratio of liquor to material were varied during acetosolv pulping process of old newsprint. Ratio of liquor to material did not give the significant difference in reaction product. Delignification rate was increased with increasing reaction time during acetosolv pulping, but yield and degree of substitution decreased with increasing reaction time. Sulfuric acid are better catalyst than hydrochloric acid in acetosolv pulping process for old newsprint, and optimal addition amount of catalyst was 1% based on reaction material. Delignification, yield, and degree of substitution were influenced by the catalyst and reaction time. Under pulping condition of $120^{\circ}C$ in 1/12 liquor to material ratio and 60min, degree of substitution was about 0.7. The acetylation reaction was not completely caused by these reaction condition. The examination of the FT-IR spectra revealed that absorption band(1200$\textrm{cm}^{-2}$, 1,750$\textrm{cm}^{-1}$) caused by carbonyl group were confirmed.

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

• Analytical Science and Technology
• /
• v.30 no.4
• /
• pp.205-212
• /
• 2017

Rice endosperm, the portion that remains after milling, is the part of the rice seed that is primarily consumed as a source of nutrients. There have been many studies on polysaccharides, such as hemicellulose, cellulose, and pectins, derived from the cell walls of various plant groups. It has been reported that the acidic polysaccharide fractions, which contain water-soluble pectins that have been shown to have pharmacological effects in vivo and in vitro, have common chemical structures that include galacturonic acid polymers, rhamnose, arabinose, and galactose. However, few studies have been conducted on the acidic polysaccharides contained in the endosperm of rice. In this study, we quantitatively compared the differences in the acidic polysaccharide contents from samples from two of the main varieties of rice consumed as staple foods, japonica and indica, using a colorimetric method. Rice samples were collected from 39 different regions in Korea, China, Thailand and Vietnam. Acidic polysaccharide fractions were obtained by precipitation of the alcohol-insoluble residue (AIR) and enzyme treatment of each sample. The total amount of carbohydrates and uronic acid in each acidic polysaccharide fraction were measured using the phenol-sulfuric acid method and the carbazole-sulfuric acid method, respectively. The differences in the total polysaccharide contents in the acidic polysaccharide fractions were not statistically significant (p = 0.07), but the uronic acid contents were significantly different between the two groups (p = 0.04).

• Journal of Korea Foresty Energy
• /
• v.19 no.2
• /
• pp.86-92
• /
• 2000

The liquefactions of $\alpha$-cellulose(Sigma Chemical, C-8002, 47H0383) was prepared in the presence of phenol using sulfuric acid as a catalyst under $N_2$ gas protection at $180^{\circ}C$ for 60minutes to examine its components. The ratio of $\alpha$-cellulose to phenol was 1: 6.2(w/w), and that to sulfuric acid was 1: 0.05(g/$m\ell$). The yields of liquefaction were calculated after the liquefied mixtures were passed through 1G4 glass filter. The luquefied product of $\alpha$-cellulose was analyzed using GC-MS Spectormeter. The 12 compounds identified by GC-MS Spectrometer, of which peak area covers 54% as 2,4-dimethyl phenol, p-isopropyl phenol, 1-ethyl-3,5-dimethyl benzene, o-isopropyl phenol, (E)-2,4\` dihydroxy-stilbene, 2,2\`-methylene-bisphenol, 4,4\`-methylenebisphenol, 3-methyl-2-hydroxyphenyl-(E)-2-hydroxyl-4\`-methoxy-stilbene, 1-phyenyl-1-(4\`hydroxyphenyl)methanol phenol derivatives. From this results, the reaction pathways of the liquefaction of cellulose were proposed through electrophilic substitution reaction. Phenol as a solvent might react with the reaction intermediates as well in the cellulose liquefaction.

• Current Research on Agriculture and Life Sciences
• /
• v.31 no.4
• /
• pp.250-255
• /
• 2013

As a renewable nanomaterial, cellulose nanocrystal (CNC) isolated from wood grants excellent mechanical properties in developing high performance nanocomposites. This study was undertaken to compare the reinforcing efficiency of two different CNCs, i.e., cellulose nanowhiskers (CNWs) and cellulose nanofibrils (CNFs) from hardwood bleached kraft pulp (HW-BKP) as reinforcing agent in polyvinyl alcohol (PVA)-based nanocomposite. The CNWs were isolated by sulfuric acid hydrolysis while the CNFs were isolated by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. Based on measurements using transmission electron microscopy, the individual CNWs were about $6.96{\pm}0.87nm$ wide and $178{\pm}55nm$ long, while CNFs were $7.07{\pm}0.99nm$ wide. The incorporation of CNWs and CNFs into the PVA matrix at 5% and 1% levels, respectively, resulted in the maximum tensile strength, indicating different efficiencies of these CNCs in the nanocomposites. Therefore, these results suggest a relationship between the reinforcing potential of CNCs and their physical characteristics, such as their morphology, dimensions, and aspect ratio.