• 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.

• Bulletin of the Korean Chemical Society
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• 제31권7호
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• pp.1927-1930
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• 2010

A fast, efficient, and high yielding method for the preparation of amines by reductive amination of aldehydes and ketones using sodium borohydride in the presence of cellulose sulfuric acid in EtOH and under solvent-free conditions at room temperature is described.

• 펄프종이기술
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• 제46권4호
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• pp.37-43
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• 2014

The crystallinity and molecular weight of cotton linter need to be controlled to be more easily dissolved in NMMO during manufacture of clothing fabrics. Electron beam irradiation and sulfuric acid treatment were used as pre-treatment to reduce molecular weight of cotton linter more efficiently, and after the pre-treatment, peroxide bleaching was followed in alkaline condition. After those processes, the crystalline indices of the cotton linters were measured by XRD method, and other properties such as their alpha cellulose contents and degree of polymerization were measured. It was found that the crystallinity index of cotton linter was decreased as the irradiation of electron beam increased while increased as the dose of sulfuric acid increased. These results strongly suggested that electron beam damaged the crystalline structure of the cellulose directly while sulfuric acid dissolved mostly non-crystalline area of the cellulose structure.

• 한국신재생에너지학회:학술대회논문집
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• 한국신재생에너지학회 2011년도 춘계학술대회 초록집
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• pp.179.1-179.1
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• 2011

Pretreatment of cellulosic biomass is necessary before enzymatic saccharification and fermentation. The objective of this study was to evaluate the effect of combined aqueous ammonia-dilute sulfuric acid treatment on cellulosic biomass. Miscanthus was pretreated using aqueous ammonia and dilute sulfuric acid solution under high temperature and pressure conditions to be converted into bioethanol. Aqueous ammonia treatment was performed with 15 %(w/w) ammonia solution at $150^{\circ}C$ of reaction temperature and 20 minutes of reaction time. And then, dilute sulfuric acid treatment was performed with 1.0 %(w/w) sulfuric acid solution at $150^{\circ}C$ of reaction temperature and 10 minutes of reaction time. The compositional variations of this combined aqueous ammonia-dilute sulfuric acid treatment resulted in 68.0 % of cellulose recovery and 95.7 % of hemicellulose, 81.3 % of lignin, 89.1 % of ash removal respectively. The enzymatic digestibility of 90.5 % was recorded in the combined pretreated Miscanthus sample and it was 14.7 times higher than the untreated sample. The ethanol yield in the Simultaneous Saccharification and Fermentation was 90.4 % of maximum theoretical yield based on cellulose content of the combined pretreated sample and it was about 98 % compared to the ${\alpha}$-cellulose ethanol yield.

• 펄프종이기술
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• 제45권3호
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• pp.27-35
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• 2013

Cotton linter pre-treatment methods using electron beam and sulfuric acid were investigated to prepare high quality regenerated fibers for fabrics. So far, NaOH was used to reduce the degree of polymerization (DP) of the cotton linter for ease of dissolving by cellulose solvent. Two pre-treatment methods were developed to reduce the consumption of the chemicals (NaOH) and to control the DP of cellulose more precisely. Changes in ${\alpha}$-cellulose contents and brightness by the pre-treatments were also important concerns. Both electron beam irradiation and sulfuric acid were shown to be effective on controlling the DP of cellulose and to reduce the chemical consumption, but reduced ${\alpha}$-cellulose contents as well in this study. Sulfuric acid pre-treatment, which needed additional washing process after the pre-treatment when comparing to the electron beam irradiation method, gave the highest brightness and the highest reduction of ${\alpha}$-cellulose content.

• 임산에너지
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• 제22권1호
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• pp.37-43
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• 2003

천연셀룰로오스의 탄화과정에서 탄화수율에 영향을 미치는 인자는 탄화온도, 승온속도 및 탄화로 내의 분위기를 들 수 있다. 일반적으로 탄화수율을 높이기 위해서는 탄화목표온도를 낮추고, 승온속도를 느리게 하면 탄화로의 분위기를 불활성가스의 조건에서 탄화수율이 높아진다고 보고되어 있다. 본 연구에서는 탄화조건 중에서 가장 유동성을 가지고 있는 승온속도를 조절하고, 탈수촉매제로서 황산을 첨가함으로서 탄화수율의 향상과 탄화과정에서 천연셀룰로오스를 재료로 하여 탄화특성에 대하여 조사하였다. 그 결과 황산무처리시료에 대하여는 승온속도가 증가함에 따라 수율이 상당히 감소하였지만 황산처리 시료는 승온속도가 증가하여도 수율 감소 폭이 크지 않았다. 본 연구의 결과에서 탄화과정에 있어서 승온속도의 조절과 적당한 탈수제의 첨가는 탄화재료의 수율 향상과 탄화시간 단축에 유용한 기초자료가 될 것으로 생각된다.

• 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.

• Korean Chemical Engineering Research
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• 제54권1호
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• pp.114-119
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• 2016

본 연구에서는 박테리아 셀룰로오스(BC)와 같은 천연고분자에 전도성 고분자 PEDOT:PEG와 graphene, 은나노와이어(AgNW)를 코팅하여 전도성을 부여하고자 하였다. 미리 PEDOT:PEG와 황산을 10~20%를 혼합하여 그 용액을 전자 스핀 코팅으로 BC 기판에 코팅하였다. 그 후, 전도성을 향상시키고자 graphene과 AgNW로 코팅하여 hall effect로 측정하였다. 그 결과, 대조군 PEDOT:PEG로 코팅한 BC 막의 전자농도($2.487{\times}10^{10}/cm^3$)에 비해 PEDOT:PEG에 황산을 10%로 혼합하여 코팅시킨 BC막($8.093{\times}10^{15}/cm^3$) 쪽이 $3.25{\times}10^5$배 높은 값을 나타내는 것으로 전도도가 대폭 향상되었음을 알 수 있었다. 또한, SEM분석으로 PEDOT:PEG가 황산처리에 의해 폴리머 형상으로 변화된 것을 확인 할 수 있었다. 분자구조의 변화를 FTIR분석결과 $1200cm^{-1}$ 파장의 S-O그룹이 황산처리 전에 비해 황산 혼합한 쪽에서 크게 상승된 것이 확인되었다. 이 방법을 이용하여 소량의 PEDOT:PEG사용으로 투명성을 확보할 수 있으며 미리 황산을 처리하는 것으로 제조공정을 단순하게 할 것으로 사료된다.

• Elastomers and Composites
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• 제45권1호
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• pp.51-57
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• 2010

본 연구에서는 친환경적인 특징을 가지면서도 우수한 기계적 특성을 가지고 있어 고분자 복합재료의 보강제로 주목 받고 있는 Cellulose nanowhisker (CNW) 를 염산 혹은 황산을 사용한 산가수분해 방법을 이용하여 Microcrystalline cellulose (MCC) 로 부터 추출하였다. 염산 혹은 황산을 사용하여 추출된 CNW는 직경이 20 에서 30nm 정도였고, 길이가 200 에서 300 nm 로써, 형상학적 측면에서 유사한 특성을 가지는 것을 확인하였다. 또한 전해질 용액의 전기전도도를 이용한 적정 (conductometric titration) 결과 황산을 이용하여 제조되어진 CNW의 경우, 셀룰로오스 표면의 sulfate group 에 의해 나타나는 표면전하 값이 각각 140, 197.78 mmol/kg으로 나타났으며, 염산을 이용하여 제조되어진 CNW 의 경우 셀룰로오스 표면에 약한 전하 값을 가져 표면전하 값을 구할 수 없었다. 황산을 이용하여 추출된 CNW의 열중량 분석 결과 염산을 이용하여 추출된 CNW와 비교하여 열분해 온도가 급격히 감소하는 것을 확인할 수 있었으며, Broido's method를 이용하여 정의 되어진 열분해 거동에 대한 활성화 에너지 역시 상대적으로 낮음을 확인할 수 있었다.

• Carbon letters
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• 제2권2호
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• pp.109-112
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• 2001

For the adsorption of ammonia, activated carbon fibers (ACFs) were subjected to sulfuric acid treatment in order to modify the surface functional groups. The surface acid and base value of ACFs were measured using titration and FT-IR spectrometry. SEM was used to investigate the surface morphology. Acid treatments by $H_3PO_4$, $H_2SO_4$, and $HNO_3$ were performed to increase the adsorption capacity of $NH_3$. As a result, Cellulose-based ACF has high adsorption capacity for ammonia. The ammonia removal efficiency of ACF was the maximum which was treated by 15 wt% sulfuric acid at $100^{\circ}C$ for 60 min. The average pore diameter little increased from $19{\AA}$ to $20.8{\AA}$ and the specific surface area of ACF considerably decreased and acid values increased by 15 wt% sulfuric acid treatment. Ammonia reacted with sulfonyl radicals. After adsorption of ammonia, white material was grown on the surface of ACF through the adsorption of ammonia and it was determined to ammonium sulfate.