• Title/Summary/Keyword: 용매화 수

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Kinetics of the Oxidation of Substituted Benzyl Alcohols with 4-(Dimethylamino)pyridinium Dichromate (4-(Dimethylamino)pyridinium Dichromate를 이용한 치환 벤질 알코올류의 산화반응 속도)

  • Choi, Sun do;Park, Young Cho
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.153-157
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    • 2005
  • 4-(Dimethylamino)pyridinium dichromate was synthesized by the reaction of 4-(dimethylamino)pyridine with chromium(VI)trioxide in $H_2O$, and characterized by IR, EA and ICP. The oxidation of benzyl alcohol using 4-(dimethylamino)pyridinium dichromate in various solvents showed that the reactivity increased with the increase of the dielectric constant, in the order: cyclohexen < chloroform < acetone < N,N-dimethylformamide. In the presence of hydrochloric acid(HCl), 4-(dimethylamino)pyridinium dichromate oxidized benzyl alcohol and its derivatives ($p-CH_3$, H, m-Br, $m-NO_2$) smoothly in N,N-dimethylformamide. Electron-donating substituents accelerated the reaction, whereas electron-withdrawing groups retarded the reaction. The Hammett reaction constant($\rho$) was -0.70 at 303K. The observed experimental data have been rationalized as follows: the proton transfer occurs after the prior formation of a chromate ester in the rate-determining step.

Solvent Effect on the Aquation of $trans-[Cr(en)_2Br_2]^+$ Ion and its Mechanism ($trans-[Cr(en)_2Br_2]^+$ 착이온의 수화반응에 미치는 용매효과와 그 반응메카니즘)

  • Jeong, Jong Jae;Lee, Seong Ho;Baek, Seong O
    • Journal of the Korean Chemical Society
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    • v.34 no.2
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    • pp.123-129
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    • 1990
  • The rate constants for the solvolysis of $trans-[Cr(en)_2Br_2]^+$ ion were determined by the spectrophotometric method in methanol-, ethanol-, acetone-, and acetonitrile-water mixtures, at 20, 25, 30, and 35$^{\circ}C$, respectively. The rate constants increased with increasing co-solvent compositions. The rate constant did not show any relation with the reciprocal of dielectric constant of the solvent-mixtures. The m values of Grunwald-Winstein equation for methanol-, ethanol-, acetonitrile-, and acetone-water mixtures are 0.109, 0.103, 0.101, and 0.095, respectively. A free energy cycle for the process from the initial state to the transition state in water and water + co-solvent mixtures shows that the change in solvation at the transition state has a dominant effect on the rate. From the above results, it is believed that the mechanism for the aquation of this complex is the Id mechanism.

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The Electrochemical Characteristics of 9-methyl-2,3,6,7-tetramethoxyfluorene in CH3CN and CH2Cl2/TFA/TFAn-solvent Mixture (CH3CN과 CH2Cl2/TFA/TFAn-혼합용매계에서의 9-methyl-2,3,6,7-tetramethoxyfluorene의 전기화학적 특성)

  • Kim, Duk-Hyun;Kim, Su-Jin
    • Applied Chemistry for Engineering
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    • v.10 no.2
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    • pp.196-200
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    • 1999
  • The electrochemical properties of 9-methyl-2,3,6,7-tetramethoxyfluorene have been investigated by cyclic voltammetry in acetonitrile, dichloromethane, trifluoroacetic acid (TFA) and trifluoroacetic acid anhydride (TFAn). The first charge transfer for the compound in $CH_3CN$ appeared to be a quasi-reversible one-electron step. The second oxidation step from cation to dication was irreversible. However, the oxdition of the compound in a mixture of solvents containing $CH_2Cl_2$, TFA and TFAn was reversible for both the first and second charge transfer reactions. Since the electrolytic products display a darkblue color and can be stabilized in the solvent mixture, they may be used as an electrochromic material.

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Kinetics of the Oxidation of Substituted Benzyl Alcohols using 6-Methylquinolinium Dichromate (6-Methylquinolinium Dichromate를 이용한 치환 벤질 알코올류의 산화반응 속도)

  • Kim, Young-Sik;Park, Young-Cho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.12 no.12
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    • pp.5990-5996
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    • 2011
  • 6-Methylquinolinium dichromate[$(C_{10}H_9NH)_2Cr_2O_7$] was synthesized by the reaction of 6-methylquinoline with chromium trioxide in $H_2O$, and characterized by IR, ICP. The oxidation of benzyl alcohol using 6-methylquinolinium dichromate in various solvents showed that the reactivity increased with the increase of the dielectric constant(${\varepsilon}$), in the order: cyclohexene < chloroform < acetone < N,N- dimethylformamide. In the presence of hydrochloric acid($H_2SO_4$ solution), 6-methylquinolinium dichromate oxidized benzyl alcohol and its derivatives(p-$OCH_3$, m-$CH_3$, H, m-$OCH_3$, m-Cl, m-$NO_2$) smoothly in DMF. Electron-donating substituents accelerated the reaction, whereas electron acceptor groups retarded the reaction. The Hammett reaction constant(${\rho}$) was -0.67(303K). The observed experimental data was used to rationalize the hydride ion transfer in the rate-determining step.

Simultaneous Treatment of Tar and Particles Using Oil Scrubber and Bag Filter in Biomass Gasification (오일 스크러버 및 집진장치를 통한 바이오매스 가스화 공정 발생 타르 및 입자 제거 연구)

  • Kim, Joon Yub;Jo, Young Min;Kim, Sang Bum
    • Applied Chemistry for Engineering
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    • v.30 no.6
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    • pp.712-718
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    • 2019
  • A combustible producer gas composed of H2, CO and CH4 could be obtained by the thermal-chemical conversion of biomass. However, a large amount of particulate matters including tar generated causes the mal-function of turbines and engines or the fouling of pipelines. In this study, a wet scrubber using the soybean oil and bag filter were installed, and the removal efficiency was investigated. Hydrate limestone and wood char base activated carbon were pre-coated on the filter medium to prevent clogging of open pores. The removal efficiencies by the bag filter were 86 and 80% for the hydrated limestone and activated carbon coating, respectively. Overall, the collection when using a series of oil scrubbers and bag filters were 88%, while 83% for the filter coating material.

마이크로웨이브 공정에 의한 마늘 올레오레진의 추출조건 설정 및 특성

  • 강덕순
    • Proceedings of the Korean Society of Postharvest Science and Technology of Agricultural Products Conference
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    • 2000.06a
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    • pp.26-86
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    • 2000
  • 마늘을 MAE(microwave-assisted extractiona)방법에 의하여 물, 30% 에탄올 및 50% 에탄올로 추출하고 그 특성을 비교하였다. 마늘과 각 용매의 비율은 1:2.5로 하여 마이크로웨이브 60W로 각각 5분 및 20분 동안 추출하였다. 마늘 올레오레진 수율은 50% 에탄올로 20분동안 추출한 추출물이 14.1%로 가장 높았으며 polyphenol함량도 물로 20분동안 추출한 경우가 579.0mg%로 가장 많은 함량을 나타내었다. 전자공여작용 효과 및 피르브산 함량도 물로 20분 동안 추출한 추출물이 각각 32.7% 및 마늘 1g당 13.4$\mu$molus로 가장 높게 나타났다. 각 용매에 대해 20분동안 추출한 추출물들을 37$^{\circ}C$에서 8일동안 저장하면서 피르브산 함량과 전자공여작용의 변화를 조사한 결과, 피르브산 함량은 물 추출물이 에탄올 추출물보다 높은 함량을 나타내었고 저장 시간이 증가할수록 그 함량은 감소하는 경향을 나타내었다. 전자공여작용도 물 추출물이 가장 높은 효과를 나타내었으며 추출시간에 비례하여 증가하다가 저장 6일째부터 감소하는 경향을 나타내었다. 각 용매에 대한 추출물의 색깔을 조사한 결과 물 추출물이 가장 밝고 옅은 갈색을 나타내었으며 30% 에탄올 추출물이 가장 어둡고 푸르스름한 노란색을 나타내었다. 또한 각 추출물들을 37$^{\circ}C$에서 10일간 저장하면서 갈색화 정도를 측정해 본 결과 물 추출물이 에탄올 추출물이 에탄올 추출물보다 갈색화가 많이 진행되었으며 0.1% cysteine을 첨가한 추출물과 에탄올 추출물의 갈색화는 비슷한 경향을 나타내었다. 마늘 추출물을 추출한 후에 0.1% cysteine을 첨가하여 저장한 것 보다 추출하기 전에 첨가하는 경우가 갈색화 억제 효과가 뚜렷하였다.문에 밀가루에 일부를 대용한 wheat flour dough를 사용하고 가정용 제빵기로 구워 최종 단계에까지의 제빵성 결과를 산출했다. amarans folur 5%의 대체에는 빵의 비용적이 비교적 증대했지만 그 이상 amarans flour을 대처하면 확연히 비용적은 감소했다. amarans flour 10% 대체에 hemicellulase 1250U 이상을 첨가하면 비용적은 눈에 띄게 증대했다. farinograph에 있어서 반죽의 안정성은 amarans flour 10% 대용에 현저히 감소했다. 반죽의 점탄성(아축응력, 탄성률, 점성계수)는 amarans flour 10%를 대용한 것이 무첨가한 것보다 많이 단단해졌음을 알 수 있었다. 혼합중의 반죽의 조사형 전자현미경 관찰로 amarans flour로 대체한 gluten이 단단해졌음을 알수 있었다. 유화제 stearly 칼슘, 혹은 hemicellulase를 amarans 10% 대체한 밀가루에 첨가하면 확연히 비용적을 증대시킬 수 있다는 사실을 알 수 있었다. quinoa는 명아주과 Chenopodium에 속하고 페루, 볼리비아 등의 고산지에서 재배 되어지는 것을 시료로 사용하였다. quinoa 분말은 중량의 5-20%을 quinoa를 대체하고 더욱이 분말중량에 대하여 0-200ppm의 lipase를 lipid(밀가루의 2-3배)에 대하여 품질개량제로서 이용했다. 그 결과 quinoa 대량 7.5%에서 비용적, gas cell이 가장 긍정적 결과를 산출했고 반죽의 조직구조가 강화되었다. 또 quinoa 대체에 의해 전분-지질 복합제의 흡열량이 증대된 것으로부터 전분-지질복합제의 형성 촉진이 시사되었다.이것으로 인하여 호화억제에 의한 노화 방지효과가 기대되었지만 실제로 빵의 노화는 현저히 진행되었다. 이것은 quinua 대체량 증가에 따른 반죽의 안정성이 저하되어 버린 것으로 생

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Optimum Conditions for Extracting Flavanones from Grapefruit Peels and Encapsulation of Extracts (자몽껍질 유래 플라바논의 최적 추출 및 기능성 소재 캡슐화)

  • Ko, Min-Jung;Kwon, Hye-Lim;Chung, Myong-Soo
    • Korean Journal of Food Science and Technology
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    • v.46 no.4
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    • pp.465-469
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    • 2014
  • The extraction of flavanones such as naringin, narirutin, naringenin, hesperidin, and hesperetin from grapefruit peels was performed using subcritical water extraction (SWE), hot water extraction, and conventional methods such as methanol and ethanol extraction. We analyzed the total flavanone content using high-performance liquid chromatography (HPLC) for each extracting method. Among the three methods, SWE was the optimal method with optimal operating conditions of $170^{\circ}C$ temperature and 10 min operating time. The maximum total flavanone extracted was $86.539{\pm}3.52mg/g$ grapefruit peels. Moreover, we treated the extracts with 60% ${\beta}$-cyclodextrin and then analyzed the surface structure of the encapsulated compounds by field emission-scanning electron microscopy (FE-SEM). The results indicated that the encapsulation in ${\beta}$-cyclodextrin improved solubilization, and the inclusion complex could serve as food supplements.

Study of NIR in-line Monitoring of Physicochemical Changes during the Crystallization Process of Aspirin (Aspirin 결정화 과정 중 특성변화의 NIR 인라인 모니터링 연구)

  • Lee, Hea-Eun;Wang, In-Chun;Lee, Min-Jeong;Seo, Da-Young;Shin, Sangmun;Choi, Yongsun;Choi, Guang-Jin
    • Korean Chemical Engineering Research
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    • v.48 no.6
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    • pp.757-762
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    • 2010
  • Since the quality and performance of medicinal products are heavily dependent upon the size, shape and polymorphism of active pharmaceutical ingredients(APIs), their crystallization has been regarded as one of the most important pharmaceutical processes. In this study, NIR-based inline measurements were employed to monitor key attributes of API particles real-time during the crystallization process. Principal component analysis(PCA) method was selected to correlate inline NIR spectra while the well-known aspirin was studied as a model drug. According to our characterization results, the ratio of ethanol to acetone did not cause any change in polymorphism, but resulted in a significant difference in the nucleation time, crystal growth and crystal shape. These phenomenological changes were well correlated with the PCA's implications. It turned out that the NIR-based inline monitoring technology can be employed well in observing and predicting key quality attributes such as crystal size during pharmaceutical crystallization processes.

Synthesis and Characterization of Square Planar Mixed-Ligand Complexes (Ⅰ) : Synthesis and Spectroscopic Property of M(S-S)(N-N) Type Complexes with Ni (Ⅱ), Pd (Ⅱ), and Pt (Ⅱ) (평면사각형 혼합 리간드 착물의 합성과 그 특성 (제 1 보) : Ni (Ⅱ), Pd (Ⅱ) 및 Pt (Ⅱ) 의 M(S-S)(N-N) 형 착물의 합성과 분광학적 성질)

  • O, Sang O;Jeong, Deok Yeong
    • Journal of the Korean Chemical Society
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    • v.34 no.6
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    • pp.593-599
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    • 1990
  • A series of new, square planar, and mixed-ligand complexes of Ni(Ⅱ), Pd(Ⅱ), and Pt(Ⅱ) have been prepared. From the observation of electronic spectrum for the variation of the ligand substituents, the very intense absorption band in the visible range is by the electronic transition of dithiolene to diimine ligand, HOMO to LUMO. In the various solvent systems the IT band shows the similar behavior to IT transition of mixed-valence dinuclear complexes followed with Hush theory, happens rto dominently by the inner sphere charge transfer transition. The negative solvatochromism represents that the excited-state electric dipole is reduced or reversed by the electronic transition.

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Supercritical Fluids and Preparation of Porous Materials (초임계 유체 및 다공성 소재 제조 기술)

  • Lee, Jun-Young;An, Joon-Hyun;Kim, Jung-Hyun
    • Applied Chemistry for Engineering
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    • v.16 no.2
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    • pp.169-179
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    • 2005
  • Porous materials are useful in a wide range of applications including bio/electronic products. The preparation and processing of these materials are mainly progressed by using an organic solvent, which gives rise to air pollution by its emissions. Alternatively, supercritical fluids are well suited to the production of functional porous materials due to a number of specific physical, chemical, and toxicological advantages. In this review, we will introduce the preparation and processing techniques for the formation of the nano/macro pore structure and their morphology, which can be controled by using supercritical fluids.