• Title/Summary/Keyword: 고체 NMR

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Synthesis, Chemical Characterization and Catalytic Activity of Transition Metal Complexes Having Imine Based Nitrogen Donor Ligand (이민에 기초한 질소주개 리간드의 전이금속 착물 합성, 화학적 특성 및 촉매활성)

  • Hussain, Raja Azadar;Badshah, Amin;Asma, Maliha
    • Journal of the Korean Chemical Society
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    • v.54 no.1
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    • pp.23-26
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    • 2010
  • A Schiff base ligand (Z)-N-((Z)-2-(sec-butylimino)-1,2-diphenylethylidene)butan-2-amine was synthesized by condensation of benzil with sec-butyl amine. Complexation of the ligand was carried out with first row transition elements, manganese(II) and nickel(II). Ligand and complexes were characterized by FTIR, elemental analysis and thermogravimetric analysis in solid state and by NMR ($^1H,\;^{13}C$) in solution form. Both the complexes demonstrate good catalytic activity for butadiene oligomerization under mild conditions with methylaluminoxane (MAO) as co-catalyst.

Synthesis and Characterization of Tetrazine Derivatives as High Energy Propellants (테트라진 계열의 추진 물질 합성 연구)

  • Lee, Woonghee;Park, Youngchul;Joo, Young-Hyuk
    • Journal of the Korean Society of Propulsion Engineers
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    • v.17 no.6
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    • pp.38-47
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    • 2013
  • Traditional propellants release toxic gases during combustion that are harmful to the environment. This study describes a novel synthetic process of two high nitrogen containing tetrazines, TATTz and BTATz, which can be adapted as solid fuels for a solution to environmental concerns. The compounds were characterized by NMR, IR spectroscopy, and differential scanning calorimetry(DSC). Detonation properties were calculated with the EXPLO5 program based on calculated heats of formation and measured densities.

The Effect of Iron Content on the Atomic Structure of Alkali Silicate Glasses using Solid-state NMR Spectroscopy (비정질 알칼리 규산염 원자구조의 철 함량 효과에 관한 고체 NMR 분광학 연구)

  • Kim, Hyo-Im;Lee, Sung-Keun
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.4
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    • pp.301-312
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    • 2011
  • The study on the atomic structure of iron-bearing silicate glasses has significant geological implications for both diverse igneous processes on Earth surface and ultra-low velocity zones at the core-mantle boundary. Here, we report experimental results on the effect of iron content on the atomic structure in iron-bearing alkali silicate glasses ($Na_2O-Fe_2O_3-SiO_2$ glasses, up to 16.07 wt% $Fe_2O_3$) using $^{29}Si$ and $^{17}O$ solid-state NMR spectroscopy. $^{29}Si$ spin-lattice ($T_1$) relaxation time for the glasses decreases with increasing iron content due to an enhanced interaction between nuclear spin and unpaired electron in iron. $^{29}Si$ MAS NMR spectra for the glasses show a decrease in signal intensity and an increase in peak width with increasing iron content. However, the heterogeneous peak broa-dening in $^{29}Si$ MAS NMR spectra suggests the heterogeneous distribution of $Q^n$ species around iron in iron-bearing silicate glasses. While nonbridging oxygen ($Na-O-Si$) and bridging oxygen (Si-O-Si) peaks are partially resolved in $^{17}O$ MAS NMR spectrum for iron-free silicate glass, it is difficult to distinguish the oxygen clusters in iron-bearing silicate glass. The Lorentzian peak shape for $^{29}Si$ and $^{17}O$ MAS NMR spectra may reflect life-time broadening due to spin-electron interaction. These results demonstrate that solid-state NMR can be an effective probe of the detailed structure in iron-bearing silicate glasses.

Property and Catalytic Activity of Heteropoly Acid Supported on MCM-41, 48 Mesoporous Material and SiO2 (MCM-41, 48 메조포러스 물질 및 SiO2에 담지한 헤테로폴리산의 특성 및 촉매적 활성)

  • Park, Jung-Woo;Kim, Beom-Sik;Lee, Jung-Min;Lee, Kwan-Young
    • Applied Chemistry for Engineering
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    • v.10 no.7
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    • pp.1020-1027
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    • 1999
  • Heteropoly acid(HPW) catalysts supported on three different carriers, an amorphous silica, MCM-41 and MCM-48, with different loadings and calcination temperatures have been prepared and characterized by X-ray diffraction, nitrogen physorption, infrared spectroscopy, and $^{31}P$ magic angle spinning NMR. From the result of IR and NMR, it was shown that HPW retains the Keggin structure on the supported catalysts. No HPW crystal phase was developed even at HPW loadings as high as 35 wt % on the MCM-41 and 65 wt % MCM-48. Thus, HPW appeared to form finely dispersed species. In the hydrolysis reaction of di, bis, tri-pentaerythritol, HPW/MCM-41, 48 exhibited higher catalytic activity than $HPW/SiO_2$ or HPW.

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Physical Properties of Gelucire-based Solid Dispersions Containing Lacidipine and Release Profiles (Lacidipine 함유 Gelucire 고체분산체의 물성 및 방출)

  • Park, Jun-Bom;Choi, Jong-Seo;Lee, Seung-Chul;Lee, Ho;Lee, Beom-Jin;Kang, Chin-Yang
    • Journal of Pharmaceutical Investigation
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    • v.40 no.1
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    • pp.9-14
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    • 2010
  • Lacidipine used for the treatment of hypertension has low water solubility and is classified as BCS Class II category. Gelucire-based solid dispersions (SD) containing lacidipine were prepared by solvent evaporation method to enhance drug dissolution. The powdered forms of SD showed irregularly spherical shape. Thermal behaviors of SD from differential scanning calorimetry indicated that distinct endothermic peak of lacidipine ($184^{\circ}C$) was shifted to lower region ($150.1^{\circ}C$). Drug was present in a crystalline form. NMR spectra also showed some molecular interaction between drug and Gelucire. There was no significant difference in DSC and NMR behaviors between Gelucire 44/14 and Gelucire 50/13. The initial dissolution rate of SD-loaded tablet linearly increased both in water and in water containing 1% tween 20, and much higher than the commercial tablet, $Vaxar^{(R)}$. When the amount of SD was increased, the release rate was greater. The Gelucire 50/13 showed higher dissolution than the Gelucire 44/14. The produced solid dispersion with various kinds of excipients and making tablets, it was found that solid dispersions can increase the solubility in artificial gastric juice and finally increases dissolution rate.

Synthesis and Spectroscopic Characterization of Vanadium-Incorporated V-AlMCM-48 Mesoporous Material (바나듐이 들어있는 Mesoporous V-AlMCM-48 분자체의 합성 및 분광학적 특성 조사)

  • Back, Gernho;Yu, Jong-Sung;Park, Sung-Kun;Lee, Chul Wee;Won, Taejin
    • Korean Chemical Engineering Research
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    • v.44 no.4
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    • pp.369-374
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    • 2006
  • A solid-state reaction of $V_2O_5$ with AlMCM-48 followed by calcination generated very weak paramagnetic $VO^{2+}$ species in the mesoporous material. Dehydration and subsequent reduction with CO result in the formation of vanadyl $VO^{2+}$ species that can be characterized by EPR. The chemical environment of vanadium centers in $VO^{2+}-AlMCM-48$ was investigated by XRD, EDX, DR-UV-Vis, EPR,$^{29}Si$ and $^{27}Al$ and $^{51}V$ NMR. Vanadium species in MCM-48 are existed as pseudotetrahedral $VO^{2+}$ state when they were dehydrated or reduced with CO. The coordination of water on vanadyl ions transformed their structure to distorted octahedral.

Structural Studies on Complexes of Substituted B15C5 with Nd(Ⅲ) (Nd(Ⅲ)과 B15C5 치환체와의 착물의 구조에 관한 연구)

  • Kim, Hae-Joong;Shin, Young-Kook;Kim, Si-Joong
    • Journal of the Korean Chemical Society
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    • v.39 no.9
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    • pp.692-697
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    • 1995
  • The chemical compositions and possible structure for the complex of B15C5 with Nd(Ⅲ) have been determined by NMR spectrophotometry in acetone-d6. On the stepwise additions of Nd(Ⅲ) to B15C5 solution of constant concentration, all the resonances shifted to downfield and the mole ratio of B15C5 to Nd(Ⅲ) was found to be 1 : 1. From the line broadening of proton peaks of NMR spectra, it was found that oxygen atoms in B15C5 interact with Nd(Ⅲ) ion. And in IR spectra of Nd(Ⅲ)-B15C5 complex, the band of asymmetric C-C-O stretching vibration shifted to a lower frequency region upon complexation. We have proposed the possible structure of the Nd(Ⅲ)-B15C5 coordinated with the five ether oxygen atoms and with the three bidentate nitrato groups.

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High Pressure Effects on 1,3-Dipolar Cycloaddition of Azides with Alkynes (아자이드와 알킨의 1,3-쌍극자 고리첨가반응에서 고압이 반응속도에 미치는 영향에 대한 연구)

  • Kwon, Jinju
    • Journal of the Korea Institute of Military Science and Technology
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    • v.18 no.6
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    • pp.736-742
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    • 2015
  • The effect of pressure on 1,3-dipolar cycloaddtion has been studied by means of FT-IR and NMR spectroscopy. Pressure accelerates 1,3-dipolar cycloaddition without solvent or catalyst. This simple and inexpensive method eliminates the need for work-up or purification. The method is expected to be applied to the synthesis of binders for solid rocket propellants.

Isolation and Identification of Antimicrobial Active Substances from Rhodiola sachlinensis (홍경천(Rhodiola sachlinensis)에서 항균성 물질의 분리 및 동정)

  • 심창주;이규희;정재홍;이상덕;김영호;오만진
    • Food Science and Preservation
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    • v.11 no.1
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    • pp.63-70
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    • 2004
  • The antimicrobial substances from Rhodiola sachalinensis were extncted, isolated and identified. The highest level of antimicrobial activity and its yield were obtained in methanol extract. The minimum inhibition concentrations of the methanol extract were 500 $\mu\textrm{g}$mL on agar plate and 100 $\mu\textrm{g}$mL in broth media for four gram positive and four gram negative microbials. The methanol extract was fractionated by n-hexane, chloroform, ethyl ether, ethyl acetate, and butanol, orderly. The separate was developed on the TLC plate with different solvent system ratio of chloroform and methanol. Nine substances were isolated from chloroform and methanol mixture(9:1, v/v). Among them, three isolates showed antimicrobial activity. Three substances separated by HPLC were identified by GC/MS(EI) spectrum and $^1$H, /sup13/C-NMR spectrum. They were gallic acid, (-)-epicatechin and kaempferol. The antimicrobial activities of each substances were shown gallic acid, (-)-epicatechin, kaempferol orderly.

Effect of Low-temperature Thermal Treatment on Degree of Crystallinity of a Low Density Polyethylene: $^{1}H$ Nuclear Magnetic Resonance Study (저밀도 폴리에틸렌의 결정화도에 대한 저온 열처리 효과: 수소 핵자기공명 연구)

  • Lee, Chang-Hoon;Choi, Jae-Kon
    • Elastomers and Composites
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    • v.43 no.4
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    • pp.259-263
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    • 2008
  • An effect of low-temperature long-term thermal degradation on a degree of crystallinity of a low density polyethylene (LDPE) was investigated by using $^1H$ solid state nuclear magnetic resonance (SSNMR). Firstly, the long-term thermal treatment makes a color of LDPE from white to pale yellow which is indicative of thermal oxidation. Secondly, it makes the $^{1}H$ NMR spin-spin and spin-lattice relaxation times ($T_1$) to be long. Lastly, the degree of crystallinity of the semicrystalline aged-LDPE also decreases with thermal treatment. Above all, the $T_1$ increase is envisaged to be due to either a decrease of the amorphous regions governing overall spin-lattice relaxation mechanism in LDPEs or a dynamically restricted motion of specific molecular motions by intermolecular hydrogen bonding or crosslinking. However, since the decrease of crystallinity implies an increase of amorphous regions by the thermal treatment, the former case is contrast to our results. Accordingly, we concluded that the latter effect is responsible for the $T_1$ increase.