• Title/Summary/Keyword: 탈용매 반응

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A Study on the Preparation of Hollow Microbeads Using Hydroxypropyl Chitosan (키토산 유도체를 이용한 화장품용 중공 마이크로비드의 제조에 관한 연구)

  • 하병조
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.24 no.1
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    • pp.7-24
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    • 1998
  • 게 껍질로부터 얻은 키틴을 탈아세틸화하여 키토산을 얻었으며, 얻어진 키토산의 유기용매에 대한 용해성을 향상시키기 위해 알칼리 조건에서 고압반응ㅇ기를 사용하여 프로필렌옥사이드와 반응시켜 치환율 3.5의 히드록시프로필 키토산을 합성하였다. 합성된 히드록시프로필 키토산은 고체상 CP/MAS 13C-NMR, 1H-NMR, FT-IR을 통해 반응이 키토산의 6번 탄소의 수산기와 2번 탄소의 아민기에 주로 일어났음을 알 수 있었다. 또한 X-선 회절분석을 통해 키토산의 결정성이 프로필렌옥사이드와의 반응에 의해 크게 감소하였음을 알 수 있었고, 그 결과 유기 용매에 대한 용해성이 현저히 증가되는 현상을 나타내었다. 한편, 히드록시프로필 키토산을 수상에 녹인 후 W/O 에멀젼상에 서 알칼리 촉매를 사용항 에피클로로히드린과 가교반응을 실시한 결과 내부가 비어있는 중공 마이크로비드를 얻을 수 있었다. 전자현미경을 통한 분석결과 중공 마이크로비드의 껍질의 내부에는 스킨층이 형성되어 있었으며, 외부 표면은 다공성이 높은 비대칭 막으로 되어 있음을 확인할 수 있었다.

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Preparation and Characterizations of Various Chitosan from Chitin (Chitin으로부터 다양한 chitosan의 제조와 특성)

  • 조형재;황성규;이기창;이한섭;김판기
    • Journal of Food Hygiene and Safety
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    • v.13 no.1
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    • pp.34-40
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    • 1998
  • Chitin is known as biodegradable natural polymer. But, in spite of various application of chitin from waste marine sources, commercial use of chitin has been limited due to highly resistance to chemicals and the absense of proper solvents. Therefore, we studied that another viscosity chitosan were prepared from chitin which were deacetylated under various concentration of NaOH solution, reaction time and temperature by the application of Mirna's method. The major parameters for these manufacturing methods were found to be concentration of alkali solution, reaction time and temperature etc. Besides, we studied that various chitosan derivatives were prepared from chitin by crosslinkage with epichlorohydrin and 1,3-dichloropropanol. The effects of these parameters on another viscosity(molecular weight) chitosan and crosslinked chitosan dervatives were investigated by various analysis apparatus. SEM analysis showed that both chitin and chitosan had a particle shaped morphology and another molecular weight chitosan according to the particle size was much smaller than that of chitin.

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Mechanistic Studies on the Reaction of Thioxanthylium Ion with Dimedone (티오크잔틸이움 이온과 디메돈의 반응메카니즘에 관한 연구)

  • Kwang Hyun Ahn;Kyongtae Kim
    • Journal of the Korean Chemical Society
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    • v.26 no.2
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    • pp.107-113
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    • 1982
  • Addition of dimedone to thioxanthylium ion generated from the oxidation of thioxanthene by thianthrene cation radical perchlorate in acetonitrile gave 9-(4,4-dimethylcyclohexane-2,6-dionyl)thioxanthylium perchlorate (2), whereas from the reverse addition between two reactants was obtained initially 9-(4,4-dimethylcyclohexane-2,6-dionyl)thioxanthene (1), which then underwent further reaction to give 2. The compound 2 was readily deprotonated in aq acetone to give 9-(4,4-dimethylcyclohexane-2,6-dionylidene)thioxanthene (3). However, 3 turned out to be in equilibrium with 2 in which three isosbestic points at 219, 289, and 348 nm were recorded in aq acetonitrile. The intensity and the position of the maximum absorption of 3 near 380 nm vary depending on the solvents which has been explained in terms of the solvent-solute interactions.

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Synthesis of The Diethylaminoethyl Chitin Derivatives and Their Flocculating Behavior (Diethylaminoethyl Chitin 유도체의 제조와 그들의 응집거동에 관한 연구)

  • Kim, Chun-Ho;Kim, So-Yeon;Jung, Byung-Ok;Kim, Jae-Jin;Choi, Kyu-Suk
    • Applied Chemistry for Engineering
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    • v.8 no.2
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    • pp.237-245
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    • 1997
  • A DEAE-chitin was prepared with DEAE HCl in an aqueous alkali-chitin solution. The resulting DEAE-chitin exhibited a highly improved affinity to water and organic solvents, It was N-deacetylated by heating in aqueous 10% sodium hydroxide containing sodium borohydride for 9h at $80^{\circ}C$ to produce DEAE-chitosan. These conditions were milder than those for the N-deacetylation of chitin. In order to increase its cationic character, the DEAE-chitin was treated with ethyl halide to give TEAE-chitin. The structural changes in the chitin derivatives were confirmed by using both FT-IR and $^1H$ NMR, and their flocculating behavior, in kaoline suspension showed the optimum property at a weak alkaline pH and 8 ppm concentration of resin conditions.

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Biomodification of Ethanol Organolsolv Lignin by Abortiporus biennis and Its Structural Change by Addition of Reducing Agent (Abortiporus biennis에 의한 유기용매 리그닌의 생물학적 변환과 환원제 첨가에 따른 구조 변화)

  • Hong, Chang-Young;Park, Se-Yeong;Kim, Seon-Hong;Lee, Su-Yeon;Ryu, Sun-Hwa;Choi, In-Gyu
    • Journal of the Korean Wood Science and Technology
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    • v.44 no.1
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    • pp.124-134
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    • 2016
  • The main goal of this study was to investigate biomodification mechanism of lignin by white rot fungus, Abortiporus biennis, and to depolymerize ethanol organosolv lignin for industrial application. In nitrogen-limited culture, A. biennis polymerized mainly lignin showing a rapid increase of molecular weight and structural changes depending on incubation days. At the initial incubation days, cleavage of ether bonds increased phenolic OH content, while the results were contrary in of the later part of the culture. Based on these results, ascorbic acid as a reducing agent was used to induce depolymerization of lignin during cultivation with white rot fungus. As a result, the degree of increase of average molecular weight of lignin was significantly declined when compared with those of the ascorbic acid free-experiment, although the molecular weight of fungus treated sample slightly increased than that of control. Furthermore, lignin derived oligomers in culture medium were depolymerized with the addition of ascorbic acid, showing that the average molecular weight was 381 Da, and phenolic OH content was 38.63%. These depolymerized lignin oligomers were considered to be applicable for industrial utilization of lignin. In conclusion, A. biennis led to the polymerization of lignin during biomodification period. The addition of ascorbic acid had a positive effect on the depolymerization and increase of phenolic OH content of lignin oligomers in medium.

Controlling of Molecular Weight and Degree of Deacetylation of Chitosan and Its Characteristics in Film Formation (키토산 분자량과 탈아세틸화도 조절 및 이에 따른 필름 특성)

  • Hwang, Kwon-T.;Park, Hyun-J.;Jung, Soon-T.;Ham, Kyung-S.;Yoo, Yong-K.;Cho, Gun-S.
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.5 no.1
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    • pp.47-55
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    • 1999
  • Applications of chitosan are related to molecular weight and degree of deacetylation(DOD) of chitosan completely. The molecular weight and DOD were greatly affected by the concentration of solution time and temperature. The degree of demineralization was not significantly different at $50^{\circ}C\;and\;70^{\circ}C$ after 30 minutes. Deproteinization decreased as process time increased. The nitrogen content was reached to 6.92% after 90 minute at $80^{\circ}C$, which is similar to theoretical nitrogen content of chitin. The DOD was 82.84% after 2 hours reaction and increased as the reaction time increased in the process. Viscosity and molecular weight are increased as recycling number of concentrated NaOH solution increased. Chemical, biological and physical properties of chitosan depend on the DOD and molecular size of the molecule. Tensile strength of the films from acetic acid solutions was between $28.9{\sim}33.6$ MPa and was generally higher than that of the films from lactic acid. Elongation of the films from lactic acid was between $97.0{\sim}109.7%$ and was generally higher than that of the films from the acetic acid. Water vapor permeability of the films prepared from lcetic acid solutions was between $1.9{\sim}2.3ng{\cdot}m/m^2{\cdot}s{\cdot}Pa$ and was generally higher than that of the films from the acetic acid.

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Reductive Degradation of hexachloroethane by using Iron Minerals: Kinetics studies (철 광물에 의한 헥사클로에탄의 환원적 분해: 반응 속도 연구)

  • Kim, Sung-Kuk;Park, Sang-Won
    • Journal of Soil and Groundwater Environment
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    • v.9 no.2
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    • pp.20-27
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    • 2004
  • Kinetic characteristics dependent on several factors such as iron mineral and organic solvents were investigated. When F $e^{0}$ , FeS and Fe $S_2$ were used as mediators, minerals affecting reaction rate were in the following order : $Fe_{0}$ 0/ > FeS > $FeS_2$ when in contact $C_2$C $l_{6}$ . The more chloride substituted, the higher reaction rate were observed. The reaction rates were dependent on pH, shaking rate, temperature and specific surface area. 1, 10-phenanthroline and EDTA degradation rates were fast, indicating that they adsorbed on the surface of the iron which makes the electron transfer reaction easy. Nitrate which has $\pi$* orbital of molecular can increase electron transfer rate because it is delocalized in its entity. The reaction rates were not affected by hydroquinone. Degradation rates were much enhanced with naturally occurring kaolinite because of the surface corrosion of Fe mineral. However, The reaction rate was not affected by F $e^{2+}$ or S $O_4$$^{2-}$ presented in solution.n.

Characteristics of Degradation and Improvement of Properties with Conducting Polypyrrole (전도성 Polypyrrole의 분해 특성과 물성 개선)

  • Lee, Hong-Ki;Eom, Jung-Ho;Park, Soo-Gil;Shim, Mi-Ja;Kim, Sang-Wook;Lee, Ju-Seong
    • Applied Chemistry for Engineering
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    • v.5 no.5
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    • pp.764-771
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    • 1994
  • Electrochemical synthesis of conductive polypyrrole films was carried out in nucleophilic solvent containing p-toluenesulfonic acid or bezensulfonic acid as supporting electrolyte and dopant. Also characteristics of degradation and improvement of mechanical properties were studied. The conductivity, tensile strength and elongation of the films obtained in dimethyformamide/p-toluenesulfonic acid had the highest value of 10-40S/cm, $25N/mm^2$ and 10%, respectively. The optimum condition of electrochemical synthesis was $2mA/cm^2$ for constant current method and 0.9V for constant potential method containing 0.5M pyrrole and 0.5M p-TSA. The obtained films showed good stability in air and electrode characteristics of secondary battery by reversibility in doping and undoping. The degradation process was 1st order reaction at various temeprature. The activation energy and rate constant of degradation reaction were $1.01JK^{-1}mol^{-1}$ and $3.1{\times}10^{-7}min^{-1}$ respectively at $25^{\circ}C$. For the improvement of mechanical properties, composition of polypyrrole films with various host polymer were investigated and increase of tensile strength and elongation was confirmed.

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