• Title/Summary/Keyword: Alkali agent

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Alkali-Metal Ion Catalysis in Alkaline Ethanolysis of 2-Pyridyl Benzoate and Benzyl 2-Pyridyl Carbonate: Effect of Modification of Nonleaving Group from Benzoyl to Benzyloxycarbonyl

  • Um, Ik-Hwan;Kang, Ji-Sun;Kim, Chae-Won;Lee, Jae-In
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.519-523
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    • 2012
  • A kinetic study is reported on nucleophilic displacement reactions of benzyl 2-pyridyl carbonate 6 with alkalimetal ethoxides, EtOM (M = Li, Na, and K), in anhydrous ethanol at $25.0{\pm}0.1^{\circ}C$. The plots of pseudo-firstorder rate constant $k_{obsd}$ vs. [EtOM] curve upward, a typical phenomenon reported previously for alkaline ethanolysis of esters in which alkali-metal ions behave as a Lewis-acid catalyst. The kobsd value for the reaction of 6 with a fixed EtOK concentration decreases rapidly upon addition of 18-crown-6-ether (18C6), a complexing agent for $K^+$ ion up to [18C6]/[EtOK] = 1.0 and then remains constant thereafter, indicating that the catalytic effect exerted by K+ ion disappears in the presence of excess 18C6. The reactivity of EtOM towards 6 increases in the order $EtO^-$ < EtOLi < EtONa < EtOK, which is contrasting to the reactivity order reported for the corresponding reactions of 2-pyridyl benzoate 4, i.e., $EtO^-$ < EtOK < EtONa < EtOLi. Besides, 6 is 1.7 and 3.5 times more reactive than 4 towards dissociated $EtO^-$ and ion-paired EtOK, respectively. The reactivity difference and the contrasting metal-ion selectivity are discussed in terms of electronic effects and transition-state structures.

Development of Curdlan Separation Process with Density Gradient Centrfugation (Density Gradient를 이용한 식품소재를 커들란의 분리공정개발)

  • 김봉영;이중헌
    • KSBB Journal
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    • v.16 no.5
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    • pp.523-525
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    • 2001
  • Curdlan is one biopolymer composed of ${\beta}$1,3-glucan and dissolved in a alkali solution but formed salt under neutral or acid condition. It was produced by Agrobactrium species and the separation process is necessary to make pure curdlan from the culture broth. The pH swing separation method was as feasible separation process using solubility changes with the pH difference. however, this method requires a lot of acid and alkali solution also produces a lot of waste. Therefore, an efficient process which could save energy and minimize toxic waste was developed. A density gradient separation process was developed in this research. High density sucrose solution was used as a separation agent. Curdlan was separated from the culture broth when the density of the sucrose solution was 1.15 g/L. Since the curdlan was produced on the surface of cell wall. the pre-treatment of culture broth was necessary. Curdlan recovery yield was increased up to 83% with the homogenization of the culture broth and further increased up to 87% with the treatment of alkai-acid solution.

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Studies on the quantitative determination of Capsaicin in various species of the genus Capsicum (고추중의 Capsaicin 정량(定量)에 관(關)한 연구(硏究))

  • Lee, Tae-Yeong;Park, Seong-O
    • Applied Biological Chemistry
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    • v.4
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    • pp.23-28
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    • 1963
  • Various species of the genus Capsicum contain in their fruits an intensively sharp and pungent substance, Capsaicin, which was first isolated in an almost pure state by Thresh. Containing the pungent principle, Capsicums are used extensively in food as a spice and in medicine as a rubefacient and carminative. Numerous methods have been proposed for the isolation, the chemical structure and the quantitative determination of Capsaicin. Modifying the several methods described before, the Capsaicin contents in various species of the genus Capsicum were determined as follows. (1) The isolation of pure Capsaicin was the essential first step for the determination of Capsaicin contents. Powdered cayenne pepper was extracted with acetone. By the method of ether alkali partition extraction slightly modified at this laboratory and by the recrystallization with light petroleum ether that was repeated ten times, the pure crystalline Capsaicin was obtained. Using this Capsaicin, the standard absorption curve was drawn with Beckman spectrophotometer model DU for the quantitative determination of Capsaicin. 92) The powdered sample was extracted in a Soxhlet extractor with ether-acetone solvent system(3:1) for 25 hours. Capsaicin in this ether-acetone extracts was efficiently separated in a pure state by paper partition chromatography using 58% methanol solution as developing agent. It was found that 58% methanol was one of the most valuable solvent to separate Capsaicin from impurities such as sterols, fatty acids, waxes and carotenoid pigments. (3) The colorimetric method modifying the Schulte-Kruger's method which consists of measuring the red color produced with diazobenzenesulphonic acid was used. Capsaicin in various species of the genus Capsicum was determined quantitatively with use of Beckman spectrophotometer model DU at $480\;m{\mu}$.

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Metal Ion Catalysis in Nucleophilic Substitution Reaction of 4-Nitrophenyl Picolinate with Alkali Metal Ethoxides in Anhydrous Ethanol

  • Hong, Yeon-Ju;Kim, Song-I;Um, Ik-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2483-2487
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    • 2010
  • Pseudo-first-order rate constants ($k_{obsd}$) were measured spectrophotometrically for nucleophilic substitution reactions of 4-nitrophenyl picolinate (6) with alkali metal ethoxides (EtOM, $M^+\;=\;K^+$, $Na^+$ and $Li^+$) in anhydrous ethanol at $25.0{\pm}0.1^{\circ}C$. The plot of $k_{obsd}$ vs. [EtOM] exhibits upward curvature regardless of the nature of $M^+$ ions. However, the plot for the reaction of 6 with EtOK is linear with significantly decreased $k_{obsd}$ values when 18-crown-6-ether (18C6, a complexing agent for $K^+$ ion) is added in the reaction medium. Dissection of $k_{obsd}$ into $k_{EtO^-}$ and $k_{EtOM}$ (i.e., the second-order rate constant for the reaction with dissociated $EtO^-$ and ion-paired EtOM, respectively) has revealed that ion-paired EtOM is 3~17 times more reactive than dissociated $EtO^-$. The reaction has been proposed to proceed through a 5-membered cyclic transition state, in which $M^+$ ion increases the electrophilicity of the reaction site. Interestingly, $Na^+$ ion exhibits the largest catalytic effect. The presence of a nitrogen atom in the pyridine moiety of 6 has been suggested to be responsible for the high $Na^+$ ion selectivity.

A Study on the Engineering Properties of Micro Fine Hybrid Silicate Grout Materials (마이크로 복합실리카 그라우트재의 공학적 특성에 관한 연구)

  • Chun, Byung-Sik;Kim, Jin-Chun;Choi, Young-Chul;Jung, Jong-Ju;Yoon, Nam-Sik;Shin, Sang-Jae
    • Journal of the Korean GEO-environmental Society
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    • v.2 no.1
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    • pp.67-79
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    • 2001
  • The objective of this study is to determine the engineering properties of micro fine hybrid silicate grout materials that were developed recently. In this study, MSG-N type was mainly used as grout materials, and the chemical components, grain size distribution, mineral characteristics were analyzed. Moreover, the properties of active silica and ordinary portland cement acting as coagulating agent were analyzed and compared with each other. To determine the engineering properties, the bleeding test, viscosity test, coagulation test, examination with naked eye, photographing by using SEM, uniaxial compression test and in-situ application test for reclaimed ground were carried out. A series of test results showed that the strength of micro fine hybrid silicate grout materials was about twice that of ordinary sodium silicate grout materials, and alkali leakage decreased dramatically when MSG method was utilized. Especially, based on the evaluation of the application of the MSG method to field, this method would be very effective in reducing coefficient of permeability due to its excelent permeability.

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Fabrication of lightweight geopolymer based on the IGCC slag (IGCC 용융 슬래그를 이용한 경량 지오폴리머 제조)

  • Park, Soo-bin;Kim, Kang-duk;Kang, Seung-gu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.6
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    • pp.319-326
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    • 2017
  • In this study, a lightweight geopolymer was prepared using by slag discharged from IGCC (Integrated Gasification Combined Cycle) power plant and its physical properties, the density and compressive strength, were analyzed as a function of the concentration of alkali activators, W/S ratio and aging times. Also the possibility of applying it to lightweight materials by adding Si sludge as a foaming agent to the geopolymerg was investigated. In particular, a complex composition of alkali activator and a pre-curing process were applied to improve the strength properties of lightweight geopolymers. While the compressive strength of the lightweight geopolymer using a single activator was 9.5 MPa, the specimen made with a complex composition of alkali activator had compressive strength of 2~5 times higher. In addition, the lightweight geopolymer with pre-curing process showed a compressive strength value of 18~48 % higher than that of specimen made with no precuring process. In this study, by using a complex activator and a pre-curing process. the maximum compressive strength of lightweight geopolymer was obtained as 40 MPa (The specimen was aged for 3 days and had density of $1.83g/cm^3$), which is comparable to cement concrete. By analyzing the crystal phase and microstructure of geopolymers obtained in this study using by XRD and SEM, respectively, it was confirmed that the flower-bud-like zeolite crystal was homogeneously distributed on the surface of the C-S-H gel (sodium silicate hydrate gel) in the geopolymer.

Synthesis of Zn-intermediate from alkali agents and its transformation to ZnO crystallinity (알칼리 침전제에 의해 제조된 아연 중간생성물 및 산화아연 결정화)

  • Jang, Dae-Hwan;Kim, Bo-Ram;Kim, Dae-Weon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.6
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    • pp.270-275
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    • 2021
  • ZnO was synthesized according to the transformation behavior and crystallization conditions of Zn-intermediate obtained by zinc sulfate as a precursor and NaOH, Na2CO3 as a alkali agents. For ZnO crystallization, Zn4(OH)6SO4·H2O and Zn5(OH)6(CO3)2·H2O as a Zn-intermediate were calcined at 400℃ and 800℃ for 1 h, respectively, based on decomposition temperature from TGA. Zn4(OH)6SO4·H2O was confirmed to have mixed Zn4(OH)6SO4·H2O and ZnO at 400℃, and was completely thermally decomposed at 800℃ to form ZnO phase. The prepared Zn5(OH)6(CO3)2·H2O as a Zn-intermediate by the reaction with Na2CO3 was transformed to a complete ZnO crystallization over 400℃. Nano-sized ZnO can be synthesized at a relatively lower calcination temperature through the reaction with Na2CO3.

Optimization of Cellulose Dyeing with Natural Indigo: Ramie dyeing by One-step Reduction/dyeing Process (천연인디고를 이용한 셀룰로오스계 직물 염색의 표준화 연구: 일단계 환원/염색에 의한 마직물 염색)

  • Son, Kyung-Hee;Shin, Youn-Sook;Yoo, Dong-Il
    • Fashion & Textile Research Journal
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    • v.13 no.2
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    • pp.263-268
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    • 2011
  • One-step reduction/dyeing method was applied for ramie dyeing with natural indigo powder. The effect of reduction/dyeing conditions including the pH of bath, dye temperature and time, and concentration of indigo powder and reduction agent on dye uptake and color properties were investigated. Regardless of addition of alkali, the dyed fabrics appeared in the PB Munsell color range(${\lambda}_{max}$: 660 nm) and the dye uptake was much higher with no addition of sodium hydroxide. Dyeing was carried out through the use of only sodium hydrosulfite in the bath. The maximum dye uptake was obtained at 60 for 30min. Saturated dye uptake was obtained at 2 g/L of sodium hydrosulfite concentration up to 2 g/ L of indigo powder. Whereas, at higher indigo powder concentration (4 g/L), more than 3 g/L of reducing agent concentration was required for obtaining the saturated dye uptake. Color reproducibility was reliable with color difference in the range of 0.03~0.16. Regardless of color strength, fastness to rubbing was acceptable with a 3/4~4/5. Fastness to washing, dry cleaning, and light of samples with low color strength were poor. Whereas, fastness to washing, dry cleaning, and light of samples with high color strength were very good.

Stability Improvement of Esomeprazole Magnesium Dihydrate Enteric-Coated Tablet by Adding Alkalizing Agents (에스오메프라졸 마그네슘 이수화물을 함유하는 장용성 제제의 안정성 개선)

  • Cho, Young Ho;Jeon, Hyo Bin;Lee, Jong-Hwa;Lee, Gye Won
    • KSBB Journal
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    • v.32 no.2
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    • pp.108-116
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    • 2017
  • Omeprazole, a benzimidazole derivative, suppresses gastric acid secretion by inhibiting $H^+/K^+$ ATPase in gastric parietals cells, and by reducing $H^+$ concentration. To improve stability of esomeprazole magnesium dihydrate (ESMD), enteric-coated preperation was composed of core tablet, subcoating and enteric coating layer. We were evaluated in vitro dissolution characteristics between test and reference ESMD preparation and stability. We could prepare enteric-coated formulation of ESMD by controlling disintegrating agent and coating ratio which could rapidly dissolved in neutral or alkali medium. The formulation D5 with crospovidone of 1.25% and coating ratio of 16.25% had a similar dissolution behavior compare to reference preparation. Difference factor ($f_1$) and similarity factor ($f_2$) were 0~15 and 50~100 and there was no significant difference in bioequivalence between formulations. The content and dissolution rate of formulation D5 were $96.54{\pm}0.21$ and $78.56{\pm}0.87%$ without change of color in accelerated condition ($40^{\circ}C$, RH 75%, high density polyethylene (HDPE) container) for 6 months. This study concluded that our enteric coated preparation of ESMD could be an useful method to improve stability of unstable drug without direct contact with coating material.

An Experimental Study on the Dyeability of Indigo and Indigo Pulberata Levis (쪽과 청대의 염색성에 관한 연구)

  • Shin, Young-Joon
    • Journal of the Korea Fashion and Costume Design Association
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    • v.12 no.4
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    • pp.149-157
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    • 2010
  • After observing various changed colors by some dyeing conditions in case of the Indio and Indigo Pulberata Levis, we had below result. 1. Best reduction temperature for Indigo was $50^{\circ}C$, and the reduction temperature had an effect on level dyeing and dye-uptake. For the Indigo Pulberata Levis, best reduction temperature was $60^{\circ}C$, and best reduction time for Indigo was 20 minutes, for the Indigo Pulberata Levis was 30~40 minutes. 2. Both Indigo and Indigo Pulberata Levis showed high K/S without using alkali, but it was almost not possible to be dyed without reduction agent. The best amount of potassium carbonate concentration and soldium hydrosulfite concentration was $2{\sim}3g/{\ell}$ and $2g/{\ell}$ each for dyeing. 3. The best dyeing temperature for Indigo was $30^{\circ}C$ and $60^{\circ}C$ for Indigo Pulberata Levis. 4. In case of Indigo, K/S increased slightly at $5g/{\ell}$ concentration. Thus, $5g/{\ell}$ is efficient amount. However, it needed $50g/{\ell}$ to increase K/S for Indigo Pulberata Levis. It tells that we need a lot of Indigo Pulberata Levis for dyeing dark color. 5. Indigo dyed cotton looked more greener than silk. Since silk absorbs lots of red color, it looked strong red color. However, Indigo Pulberata Levis looked greenish on both cotton and silk. 6. Since the hue's range of Munsell's value was PB for both Indigo and Indigo Puberata Levis, we are able to know that red color's indirubin is contained as well as blue color's indigo.

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