• 제목/요약/키워드: 1H-NMR spectroscopy

검색결과 576건 처리시간 0.029초

Synthesis of Poly(alkyl methacrylate)s Containing Various Side Chains for Pour Point Depressants (서로 다른 측쇄 구조를 가진 폴리(알킬 메타크릴레이트)계의 저온유동성 향상제 합성)

  • Hong, Jin-Sook;Kim, Young-Wun;Chung, Keun-Wo;Jeong, Soo-Hwan
    • Applied Chemistry for Engineering
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    • 제21권5호
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    • pp.542-547
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    • 2010
  • n-Paraffin and saturated fatty acid methyl esters in the diesel and bio-diesel fuel crystallize at low temperature. Many articles have addressed various solutions for the low temperature crystallization problem and one of them is the use of methacrylate copolymers. In this work, we synthesized a series of copolymers in the reaction condition of 70 : 30 molar ratio of lauryl methacrylate (LMA) (or stearyl methacrylate (SMA)) and alkyl methacrylates. The structures of the copolymers were characterized by $^1H$-NMR and FT-IR spectroscopy, and the molecular weight of copolymers were obtained from Gel Permeation Chromatography (GPC) method. The concentrations of additives were 500~1000 ppm and 1000~10000 ppm in diesel fuels and bio-diesel fuel (BD5 and BD20), respectively. The addition of copolymers changes the many properties of fuel such as the pour point (PP), cloud point (CP) and cold filtering plugging point (CFPP). For example, the low temperature properties of the copolymers containing SMA ($PSMAmR_2n$) were excellently improved about 15, 7, and $10^{\circ}C$ for PP, CP and CFPP, respectively.

Synthesis of Renewable Resource-derived Furan-based Epoxy Compounds and Their Adhesive Property (재생자원 유래 퓨란계 에폭시 화합물의 합성 및 접착 특성)

  • Lee, Jae-Soung;Lee, Sang-Hyeup;Jeong, Jaewon;Kim, Baekjin;Cho, Jin Ku;Kim, Hyun Joong
    • Journal of Adhesion and Interface
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    • 제11권2호
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    • pp.41-49
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    • 2010
  • Furan-containing epoxide monomers (8, 9) were designed and synthesized as carbon-neutral, environment-friendly adhesion material. Bicyclic skeleton were constructed using the Diels-Alder reaction of furan and methyl acrylate, both readily accessible starting material from a biomass via bio-refinery process. After reduction of ester functionality, resulting hydroxyl moieties were coupled to epichlorohydrin to provide the epoxy-functionalized furanic monomers (8, 9). The structure of new furanic monomers was confirmed by $^1H$ and $^{13}C$ NMR spectroscopy. As UV-curable monomers, basic properties such as UV curing time and the extent of UV curing were evaluated by photo DSC. Photo-curing shrinkages were measured by linear variable differential transformer transducer (LVDT) and the effect of molecular structure on shrinkage was considered. In addition, new synthetic compounds showed the shear strength over 3 MPa when they were photo-cured between polycarbonate plates, which indicates these compounds are feasible to use as photo-curable adhesive materials.

CD34 Monoclonal Antibody-Immobilization on Polyurethane Surface by Poly(PEGA-co-BMA) Coating (PEGA/BMA 공중합체의 코팅을 통해 CD34 단일클론항체가 고정화된 폴리우레탄 표면)

  • Joung, Yoon-Ki;Hwang, In-Kyu;Park, Ki-Dong
    • Polymer(Korea)
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    • 제33권6호
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    • pp.602-607
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    • 2009
  • A polyurethane (PU) surface enabling in vivo endothelialization via endothelial progenitor cell (EPC) capture was prepared for cardiovascular applications. To introduce CD34 monoclonal antibody (mAb) inducing EPC adhesion onto a surface, poly (poly (ethylene glycol) acrylate-co-butyl methacrylate) and poly (PEGA-co-BMA) were synthesized and then coated on a surface of PU, followed by immobilizing CD34 mAb. $^1H$-NMR analysis demonstrated that poly(PEGA-co-BMA) copolymers with a desired composition were synthesized. Poly(PEGA-co-BMA)-coated PU was much more effective for the immobilization of CD34 mAb, comparing with PEG-grafted PU prepared in our previous study, as demonstrated by that surface density and activity of CD34 mAb increased over 32 times. Physico-chemical properties of modified PU surfaces were characterized by X-ray photoelectron spectroscopy (XPS), water contact angle, and atomic force microscopy (AFM). The results demonstrated that the poly(PEGA-co-BMA) coating was effective for CD34 mAb immobilization and feasible for applying to cardiovascular biomaterials.

Preparation and Characterization of Lithocholic Acid Conjugated Chitosan Oligosaccharide Nanoparticles for Hydrophobic Anticancer Agent Carriers (소수성 항암제의 전달체로 응용하기 위한 리소콜릭산이 결합된 키토산 나노입자의 제조와 특성)

  • Park, Jun-Kyu;Kim, Dong-Gon;Choi, Chang-Yong;Jeong, Young-Il;Kim, Myung-Yul;Jang, Mi-Kyeong;Nah, Jae-Woon
    • Polymer(Korea)
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    • 제32권3호
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    • pp.263-269
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    • 2008
  • To develop carriers of hydrophobic anticancer agents based on chitosan, chitosan oligosaccharide lactate (COS) was chemically modified with lithocholic acid (LA) which is one of the bile acids as a hydrophobic group. The physicochemical properties of the lithocholic acid conjugated chitosan nanoparticles (COS-LA) were investigated using $^1H$-NMR spectroscopy, dynamic light scattering (DLS) and spectrofluorophotometer. COS-LA-paclitaxel (CLs-Tx) nanoparticles loading paclitaxel as an anticancer agent were prepared by a dialysis method and its loading efficiency was measured through HPLC. On the basis of DLS results, the estimated particle sizes of CLs-Tx were around 300 nm. Also, the critical micelle concentration (CMC) was proven to be dependent on the degree of substitution of lithocholic acid. It showed that the CLs-Tx has the superior potential for the application as a paclitaxel carrier.

The Effect of Thermal Stability of Cu(I) Precursors on the Deposition in the Metal Organic Chemical Vapor Deposition (MOVCD에 있어서 구리(l)전구체들의 열적 안정성이 증착에 미치는 영향)

  • Park, Man-Young;Lee, Shi-Woo
    • Korean Journal of Materials Research
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    • 제8권4호
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    • pp.345-353
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    • 1998
  • Metal organic chemical vapor deposition (MOCVD) of copper using three Cu( I ) precursors. (hfac)Cu (VTMS) (hfac= hexafluoroacetylacetonate, VTMS= vinyltrimethylsilane), (hfac)Cu(VTMOS) (VTMOS= vinyltri¬methoxysilane) and (hfac)Cu(A TMS) (A TMS= allyltrimethylsilane) was studied. The thermal stability and the gase¬ous phase reaction mechanism of Cu( I ) precursors were identified using $^1H$-, $^I3C$-NMR and Fourier transform infra¬red spectroscopy. It was found out that thermal stability of liquid phase (hfac)Cu(VTMS) and (hfac)Cu(VTMOS) were better than that of (hfac)Cu(A TMS) using FT - NMR. From in-situ FT - IR experiments, the disproportion reaction of Cu(hfac). the decomposition reaction of Cu(hfac), and cracking of free hfac ligand were observed. Also the effect of gaseous phase reaction on the deposition rates and film properties was investigated. The minimum temperature that deposition of copper films from (hfac)Cu(A TMS) was as low as 60$^{\circ}$C and such a low deposition temperature compared with those of other Cu( I ) precursors is believed to be related with weaken Cu- A TMS bond.

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Metal-Nitrosyl Complexes(II) : Synthesis and Characterization of Dinitrosyltungsten(O) Complexes (금속-니트로실 착물 (제 2 보) : 디니트로실 텅스텐(O) 착물의 합성과 특성)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • 제36권6호
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    • pp.906-913
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    • 1992
  • The polymeric compound [{$W(NO)_2Cl_2$}$_n$] were prepared by reductive nitrosylation of $WNaNO_2$ and acidified $WFeSO_4$ with $WWCl_6$ at room temperature. The reactions of [{$W(NO)_2Cl_2$}$_n$] with unidentate and bidentate ligands afforded neutral monomeric [$W(NO)_2Cl_2L_2$(or L-L)] in a relative high yields (70$\sim$90%). 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene and 8-hydroxyquinoline were used as coordinating ligands. These dinitrosyltungsten complexes were characterized by elemental analysis, $^1H$-NMR, infrared, and UV-visible spectroscopy are reported. The spectral data indicated that geometric structures of the products were cis-dinitrosyl-trans-dichloro-cis-$L_2$ of $C_{2v}$ symmetry.

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Synthesis and Characterization of Swallow-Tail Perylene Bisimide as Organic Phosphor for Hybrid LED (Hybrid LED용 유기 형광체로서의 Swallow-Tail Perylene Bisimide 제조 및 특성 연구)

  • Jung, Sung Bong;Jeong, Yeon Tae
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • 제32권1호
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    • pp.86-92
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    • 2019
  • Although perylene bisimide derivatives have advantages such as excellent thermal stability and high luminance efficiency, they have poor solubility characteristics in organic solvents. In this research, in order to improve the solubility characteristics, we prepared perylene bisimide derivatives (1C) and (2C) with swallow-tail substituted imide, which is known to lead to excellent solubility. The structures and properties of swallow-tail perylene bisimide (1C) and (2C) were analyzed by $^1H-NMR$, FT-IR, UV/Vis spectroscopy, and thermogravimetric analysis (TGA). The maximum absorption wavelengths of (1C) and (2C) in the UV/Vis spectrum were 558 nm and 556 nm, respectively, and the maximum emission wavelengths were 602 nm and 600 nm, respectively. In the TGA, (1C) demonstrated good thermal stability with less than 5 wt% weight loss up to $242^{\circ}C$. In the solubility test, (1C) and (2C) exhibited solubilities of more than 5 wt% in chloroform, ethyl acetate, and dimethylformamide, but not in methanol. When the compounds (1C) and (2C) were mixed with PMMA (polymethyl methacrylate), thin films showed peaks at 679 nm and 677 nm, respectively, in the photoluminescence spectra. (1C) was found to be a possible candidate as red organic phosphor for hybrid LEDs.

Structural Characteristics and Anti-inflammatory Activities of Chemically Sulfated-hyaluronic Acid from Streptococcus dysgalactiae (Streptococcus dysgalactiae로부터 분리된 히알루론산과 황화된 유도체의 구조와 항염증 활성)

  • Hong, Chang-Il;Jung, Eui-Gil;Han, Kook-Il;Kim, Yong Hyun;Lee, Sung Hee;Lee, Hong Sub;Han, Man-Deuk
    • Journal of Life Science
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    • 제26권5호
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    • pp.545-554
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    • 2016
  • Hyaluronic acid (HA) is an important macromolecule in medical and pharmaceutical fields. HA is a natural and linear polymer composed of repeating disaccharide units of β-1, 3-N-acetyl glucosamine and β-1, 4-glucuronic acid. This work aimed to confirm the structural characteristics and anti-inflammatory activities of HA and its chemically sulfated-HA. HA was produced from a fed-batch fermentation process using Streptococcus dysgalactiae in a 5 l bioreactor. HA was isolated water-soluble form (HA-WS) and water-insoluble form (HA-WI) from culture medium, and was obtained chemically sulfated-derivative (S-HA) that resulted in a 90% yield from HA-WI. The structural features of the sulfated- HA (S-HA) were investigated by FT-IR and 1H-NMR spectroscopy. The FT-IR and NMR patterns revealed the similarity in both the FTIR spectrum as well as NMR spectrum of both reference standard and purified HA from S. dysgalactiae. The anti-inflammatory activities of HA and S-HA were examined on LPS-induced RAW 264.7 cells. S-HA was significantly inhibited production of pro-inflammatory mediators such as nitric oxide (NO) and PGE2 and the gene levels of iNOS and COX-2, which are responsible for the production of NO and PGE2, respectively. Furthermore, S-HA also suppressed the overproduction of pro-inflammatory cytokine TNF-α (<80 pg/ml) and IL-6 (<100 pg/ml) compared to that of HA-WI. The present study clearly demonstrates that HA-S exhibits anti-inflammatory activities in RAW 264.7 macrophage cells.

Cloning, Nucleotide Sequence and Expression of Gene Coding for Poly-3-hydroxybutyric Acid (PHB) Synthase of Rhodobacter sphaeroides 2.4.1

  • Kim, Ji-Hoe;Lee, Jeong-Kug
    • Journal of Microbiology and Biotechnology
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    • 제7권4호
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    • pp.229-236
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    • 1997
  • A gene, $phbC_{2.4.1}$ encoding poly-3-hydroxybutyric acid (PHB) synthase of Rhodobacter sphaeroides 2.4.1 was cloned by employing heterologous expression in Escherichia coli. R. sphaeroides chromosomal DNA partially digested with MboI was cloned in pUC19 followed by mobilization into E. coli harbouring $phbA,B_{AC}$ in pRK415, which code for ${\beta}$-ketothiolase and acetoacetyl CoA reductase of Alcaligenes eutrophus, respectively. Two E. coli clones carrying R. sphaeroides chromosomal fragment of $phbC_{2.4.1}$ in pUC19 were selected from ca. 10,000 colonies. The PHB-producing colonies had an opaque white appearance due to the intracellular accumulation of PHB. The structure of PHB produced by the recombinant E. coli as well as from R. sphaeroides 2.4.1 was confirmed by [$H^{+}$]-nuclear magnetic resonance (NMR) spectroscopy. Restriction analysis of the two pUC19 clones revealed that one insert DNA fragment is contained as a part of the other cloned fragment. An open reading frame of 601 amino acids of $phbC_{2.4.1}$ with approximate M.W. of 66 kDa was found from nucleotide sequence determination of the 2.8-kb SaiI-PstI restriction endonuclease fragment which had been narrowed down to support PHB synthesis through heterologous expression in the E. coli harbouring $phbA,B_{AC}$. The promoter (s) of the $phbC_{2.4.1}$ were localized within a 340-bp DNA region upstream of the $phbC_{2.4.1}$ start codon according to heterologous expression analysis.

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Metal-Nitrosyl Complexes (I) Synthesis and Characterization of Dinitrosylmolybdenum (O) Complexes (금속-니트로실 착물 (제 1 보) 디니트로실몰리브덴(O) 착물의 합성과 특성)

  • Oh Sang-Oh;Mo Seong-Jong
    • Journal of the Korean Chemical Society
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    • 제36권5호
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    • pp.661-668
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    • 1992
  • The polymeric compound [{Mo(NO)_2Cl_2}n] was prepared by reductive nitrosylation of NaNO_2 and acidified FeSO_4 with MoCl_5. The reactions of [{Mo(NO)_2Cl_2}n] with unidentate and bidentate ligands afforded neutral monomeric $[Mo(NO)_2Cl_2L_2(or L-L)] in high yield (80∼90%). 3,5-Lutidine, {\gamma}-Cyanopyridine, 1,2-Phenylenediamine, 1,10-Phenanthroline, sym-Diphenylethylenediamine, 9,10-Phenanthrenequinone, 1,3-Bis(diphenylphosphino)propane and 8-Hydroxyquinoline were used as coordinating ligands. The preparation and characterization of these dinitrosylmolybdenum complexes by elemental analysis, 1H NMR, infrared, and UV-Visible spectroscopy are reported. The infrared spectra indicate that in all of the compounds prepared, the NO groups occupy cis-positions in the octahedral group of ligands.

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