• 제목/요약/키워드: D.S. (degree of substitution)

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Siloxylcellulose 유도체의 합성 (Synthesis of Various Siloxylcellulose Derivatives)

  • 홍재진;양재건
    • 공업화학
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    • 제10권2호
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    • pp.275-280
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    • 1999
  • 일반적으로 셀룰로오스는 그 골격구조 안에 서로 다른 반응성을 갖는 3개의 히드록시기를 가지고 있다. 이 기능기에 trimethylsiloxyl-, vinyldimethylsiloxyl-, allyldimethylsiloxyl-, phenyldimethylsiloxyl-, 3,3,3-trifluoropropyldimethylsiloxyl-과 tris(trimethylsiloxy)siloxyl-기를 치환반응을 이용하여 도입하였다. IR, NMR, 그리고 원소분석을 이용하여 그 구조분석 및 치환도, 그리고 siloxylation agent의 반응성을 검토하였다. 치환도는 각각 2.5, 2.2, 2.1, 2.2, 2.6, 0.7이었다.

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폭쇄법(爆碎法)을 이용(利用)한 목질계(木質系) biomass의 종합적(綜合的) 이용(利用)(II) -폭쇄재(爆碎材)로부터 Carboxymethyl cellulose의 제조(製造)- (Total Utilization of Woody Biomass by Steam Explosion(II) -The Preparation of Carboxymethylcellulose from Exploded Wood-)

  • 한상열;장준복;이종윤
    • Journal of the Korean Wood Science and Technology
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    • 제22권2호
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    • pp.30-36
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    • 1994
  • Steam explosion process is one of the most efficient, pretreatment method for the utilization of lignocellulosic biomass. The carbxymethyl-cellulose(CMC) was prepared with steam exploded wood(EXW), pine(Pinus densiflora) and oak(Quercus mongolica), by standard method using isopropyl alcohol and monochloroacetic acid. The range of water solubility of carboxymethylated pine exploded wood was 45.2~66.8 % and those of oak was 60.7~84.7 %. The degree of substitution(D.S) of carboxymethylated pine exploded wood was 0.11~0.33 and oak exploded wood was 0.48~0.76. The color of carboxymethylated pine and oak exploded wood was brown-black. When carboxymethylated EXW was purified by sulfuric acid, the yield of carboxymethylated wood was lower than non-treated one. However, the color was still brown-black although after delignification. In carboxymethylated EXM prepared after delignification, the water solubility and degree of substitution(D.S) of pine were 81.4~95.9 % and 0.71~0.79, and those of oak were 76.2~89.5 % and 0.79~1.05. The values were higher than non-treated. The degree of substitution of purified carboxymethylated wood prepared with delignified EXM, pine and oak were 0.50~0.71 and 0.70~0.88. The color of carboxymethylated wood was white. In carboxymethylated wood preparde after delignification of EXM, swelling ratio and water retention value of pine were 95.9~96.5 and 580.0~751.2, those of oak were 76.2~89.5 and 124.3~307.6.

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폭쇄법을 이용한 목질계 바이오매스의 종합적 이용 (III) - 소나무와 신갈나무 폭쇄재로부터 셀룰로오스 아세테이트의 제조 - (Total Utilization of Woody Biomass by Steam Explosion (III) - The Preparation of Acetate from Pine and Oak Exploded Wood -)

  • 이종윤;장준복;양재경
    • Journal of the Korean Wood Science and Technology
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    • 제23권2호
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    • pp.26-31
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    • 1995
  • Acetylcellulose(AC) was prepared with steam exploded wood(EXW) and EXW after delignification with sodium chlorite, pine (Pinus densiflora) and oak (Quercus mongolica) woods. The color of acetylated pine and oak exploded wood was brown, degree of substitution(D.S) of pine was 1.47~2.09, and this of oak was 1.49~2.29. The hemicellulose content of acetylated pine and oak exploded wood was 0~3.4% and 1.49~11.3%, individually. The degree of substitution of acetylated wood prepared from delignified EXW in the pine and oak wood was 0.50~0.71 and 0.70~0.88, individually. Hemicellulose content of acetylated EXW with sodium chlorite after delignification in the pine and oak wood was less than 1% and 0.6~2.5%. The color of acetylated wood after delignification was white. IR-spectra of acetylated pine and oak EXW after delignification were found that peaks at around 1740$cm^{-1}$ and 1200$cm^{-1}$ increase markedly, due to ester carbonyl group.

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Carboxymethylcellulose 제조공정을 이용한 상온에서의 수용성 섬유에 관한 연구 (A Study on the Water-soluble Fiber at the Room Temperature using Carboxymethylcellulose(CMC) Synthesis)

  • 송호준;최영민;박진원
    • 청정기술
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    • 제11권2호
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    • pp.105-116
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    • 2005
  • 본 연구는 NaOH 용액에 의한 머서화(mercerization) 반응과 모노클로로아세트산에 의한 에테르화 반응에 의해 carboxymethylcellulose(CMC)를 제조하고 각 제조단계에서의 반응시간, 시약 농도, 온도 등을 변수로 설정하여 결과물에 대한 영향을 고찰하였다. 제조된 샘플을 용해도와 카르복실기의 치환도를 통해 분석하였으며 부직포로서의 응용을 위해 제조된 수용성 섬유의 인장강도를 알아보았다. 섬유의 표면 변화는 SEM(scanning electron microscope) 사진을 통해 알아보았다. 제조된 섬유는 30분 이내에 80% 이상 용해되었으며 반응시간이나 반응 온도보다 시약의 농도에 의한 영향이 더욱 컸다. 또한 용해도가 80% 이상이었던 시편은 0.6 ~ 0.7의 치환도를 보였으며 모노클로로아세트산의 농도의 영향이 가장 크며 용해도가 증가할수록 치환도가 증가하는 경향을 보였다.

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저압(低壓) 폭쇄처리(爆碎處理)에 의한 목재주성분(木材主成分)의 분리(分離)·정제(精製) 및 이용(利用) (II) - 탄수화물(炭水化物)의 화학적(化學的) 성상(性狀)및 이용(利用) - (The Separation, Purification and Utilization of Wood Main Components by Steam Explosion in Low Pressure (II) - Characterization and Utilization of Separated Wood Polysaccharides -)

  • 엄찬호;엄태진;이정윤
    • Journal of the Korean Wood Science and Technology
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    • 제24권2호
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    • pp.20-25
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    • 1996
  • Wood chips of oak(Quercus mongolica) and larch(Larix leptolepis) were exploded with the optimum condition. Main components of exploded wood were separated with hot hot water and methanol. The hemicelluloses were purified from hot water extracts and alditol complexs were prepared from purified hemicellulose. And also, cellulose nitrate was prepared from extractive residue and characterized. The results can be summarized as follows. 1. Amounts of carbohydrate(72~79%) in the crude hemicellulose of larch wood was more than those of oak wood(55~66%). 2. The crude hemicelluloses were mainly composed of oligosaccharides in oak wood but those in larch wood contained about 50% monosaccharides. 3. Decolorization of hemicellulose was successful with activated charcoal and ion-exchange resin treatment. The alditol yields were 56.3~82.9%. 4. The degree of substitution(D.S.) of cellulose nitrate was 1.95~2.87 and it showed a good acetone solubility.

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게껍질로부터 CM-Chitin의 합성 (Synthesis of CM-Chitin from Crab Shells)

  • 안종일;김승환;유영진;박창호;임헌선;박찬구;박은경
    • 한국응용과학기술학회지
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    • 제10권2호
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    • pp.41-47
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    • 1993
  • Chitin was isolated from crab shells by modified Hackman's method, which was treated again with aqueous sodium hydroxide solution to give alkali chitin(sodium alkoxide of chitin). And after, the alkali chitin is allowed to react with monochloroacetic acid to synthesize 6-O-(carboxymethyl) chitin [CM-Chitin] under diminished pressure. In order to synthesize high performance CM-Chitin as hygroscopic agent, it was measured that the yield and degree of subsititution of each CM-Chitin according to molar ratio(monochloroacetic acid equivalent mol/N-acetyl-D-glucosamine residue) and their moisture-absorption and moisture-release properties were measured and compared with those of hyaluronic acid. The moisture-absorption and moisture-release properties of CM-Chitin, especially 0.8 in degree of substitution, were found quite similar to those of hyaluronic acid. The preliminary results show that CM-Chitin might be used as hygroscopic agent instead of hyaluronic acid in field of cosmetics.

찰옥수수 산화전분의 이화학적 특성 (Physicochemical Properties of Oxidized Waxy Maize Starches with Sodium Hypochlorite)

  • 정만곤;전영승;이서구;박종문;임번삼
    • 한국식품과학회지
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    • 제30권1호
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    • pp.42-48
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    • 1998
  • 찰옥수수 전분을 차아염소산 나트륨$(0{\sim}60{\;}mg/s{\;}starch)$과 반응시켜 제조한 찰옥수수 산화전분의 이화학적 특성 및 유화 안정성에 미치는 영향에 대하여 연구하였다. 찰옥수수 산화전분의 일반성분 중 조지방질 및 조단백질 함량은 차아염소산 나트륨 처리량의 증가에 따라 감소하여 조단백질 함량과 백색도와 부의 상관관계$(R^2=0.9847)$를 나타내었고 조회분 함량은 증가하여 염소 함량과정의 상관관계$(R^2=0.9693)$를 나타내었다. 산화전분의 카르복시기 함량은 활성염소 첨가 농도에 비례하여 증가하였다. 호화액의 점도는 차아염소산 나트륨 처리량에 따라 현저히 감소하였고, 용해도와 팽윤력은 산화도가 높을 수록 증가하었으며, 광투과도는 치환도가 증가할 수록 낮은 온도에서 높은 투과도를 나타내어 화화개시온도가 약 $15^{\circ}C$낮아졌고, 호화액의 투명도 또한 개선되었다. 물결합능력은 치환도가 증가할 수록 생성된 카르복시기로 인하여 감소하였다. 찰옥수수 전분의 입자는 다각형과 원형의 혼합물로 크기는 $3.7{\sim}20\;{\mu}m$였으며, 차아염소산 나트륨 처리량이 증가할 수록 전분 표면이 거칠어졌다. 찰옥수수 산화전분과 옥배유를 균질화하여 저장하는 동안 유화액은 산화전분의 치환도가 높을 수록 전분의 농도가 증가할 수록 유화 안정성이 증가하였다.

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Electronic Properties and Conformation Analysis of π-Conjugated Distyryl Benzene Derivaties

  • Kim, Cheol-Ju
    • Bulletin of the Korean Chemical Society
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    • 제23권2호
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    • pp.330-336
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    • 2002
  • A quantum-chemical investigation on the conformations and electronic properties of bis[2-{2-methoxy-4,6-di(t-butyl)phenyl}ethenyl]benzenes (MBPBs) as building block for ${\pi}$-conjugate polymer are performed in order to display the effects of t-butyl and methoxy group substitution and of kink(ortho and meta) linkage. The conjugation length of the polymers can be controlled by substituents and kink linkages of backbone. Structures for the molecules, o-, m-, and p-MBPBs as well as unsubstituted o-, m-, and p-DSBs were fully optimized by using semiempirical AM1, PM3 methods, and ab initio HF method with 3-21G(d) basis set. The potential energy curves with respect to the change of single torsion angle are obtained by using semiempirical methods and ab initio HF/3-21G(d) basis set. The curves are similar shape in the molecules with respect to the position of vinylene groups. It is shown that the conformations of the molecules are compromised between the steric repulsion interaction and the degree of the conjugation. Electronic properties of the molecules were obtained by applying the optimized structures and geometries to the ZINDO/S method. ZINDO/S analysis performed on the geometries obtained by AM1 method and HF/3-21G(d) level is reported. The absorption wavelength on the geometries obtained by AM1 method is much longer than that by HF/3-21G(d) level. The absorption wavelength of MBPBs are red shifted with comparison to that of corresponding DSBs in the same torsion angle because of electron donating substituents. The absorption wavelength of isomers with kink(orth and meta) linkage is shorter than that of para linkage.

Chemical Modification of Botryosphaeran: Structural Characterization and Anticoagulant Activity of a Water-Soluble Sulfonated ($1{\rightarrow}3$)($1{\rightarrow}6$)-${\beta}$-D-Glucan

  • Brandi, Jamile;Oliveira, Eder C.;Monteiro, Nilson K.;Vasconcelos, Ana Flora D.;Dekker, Robert F.H.;Barbosa, Aneli M.;Silveira, Joana L.M.;Mourao, Paulo A.S.;Silva, Maria De Lourdes Corradi Da
    • Journal of Microbiology and Biotechnology
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    • 제21권10호
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    • pp.1036-1042
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    • 2011
  • The exopolysaccharide botryosphaeran ($EPS_{GLC}$; a ($1{\rightarrow}3$)($1{\rightarrow}6$)-${\beta}$-D-glucan from Botryosphaeria rhodina MAMB-05) was sulfonated to produce a water-soluble fraction ($EPS_{GLC}$-S) using pyridine and chlorosulfonic acid in formamid. This procedure was then repeated twice to produce another fraction ($EPS_{GLC}$-RS) with a higher degree of substitution (DS, 1.64). The purity of each botryosphaeran sample (unsulfonated and sulfonated) was assessed by gel filtration chromatography (Sepharose CL-4B), where each polysaccharide was eluted as a single symmetrical peak. The structures of the sulfonated and re-sulfonated botryosphaerans were investigated using ultraviolet-visible (UV-Vis), Fourier-transform infrared (FT-IR), and $^{13}C$ nuclear magnetic resonance ($^{13}C$ NMR) spectroscopies. $EPS_{GLC}$ and $EPS_{GLC}$-RS were also assayed for anticoagulation activity, and $EPS_{GLC}$-RS was identified as an anticoagulant.

A Systematic NMR Determination of α-D-Glucooligosaccharides, Effect of Linkage Type, Anomeric Configuration and Combination of Different Linkages Type on 13C Chemical Shifts for the Determination of Unknown Isomaltooligosaccharides

  • Goffin, Dorothee;Bystricky, Peter;Shashkov, Alexander S.;Lynch, Mary;Hanon, Emilien;Paquot, Michel;Savage, Angela V.
    • Bulletin of the Korean Chemical Society
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    • 제30권11호
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    • pp.2535-2541
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    • 2009
  • Prebiotic isomaltooligosaccharide preparations contain $\alpha$-D-glucooligosaccharides comprising isomaltooligosaccharides (IMOs) and non-prebiotic maltooligosaccharides (MOs). They are both glucose oligosaccharides characterized by their degree of polymerization (DP) value (from 2 to $\sim$10), linkages types and positions (IMOs: $\alpha$-(1$\rightarrow$2, 3, 6 and in a lower proportion internal 1$\rightarrow$4) linkages, MOs: α-(1$\rightarrow$4) linkages). Their structure is the key factor for their prebiotic potential. In order to determine and elucidate the exact structure of unknown IMOs and MOs, unambiguous assignments of $^{13}C$ and $^1H$ chemical shifts of commercial standards, representative of IMOs and MOs diversity, have been determined using optimized standard one and two-dimensional experiments such as $^1H$ NMR, $^{13}C$ NMR, APT and ${^1}H-{^1}H$ COSY, TOCSY, NOESY and <$^1H-{^{13}}C$ heteronuclear HSQC, HSQC-TOCSY, and HMBC. Here we point out the differential effect of substitution by a glucose residue at different positions on chemical shifts of anomeric as well as ring carbons together with the effect of the reducing end configuration for low DP oligosaccharides and diasteroisotopic effect for H-6 protons. From this study, structural $^{13}C$ specific spectral features can be identified as tools for structural analysis of isomaltooligosaccharides.