• Title/Summary/Keyword: Solid phase synthesis

Search Result 313, Processing Time 0.03 seconds

Synthesis and Phase Relations of Potassium-Beta-Aluminas in the Ternary System K2O-MgO-Al2O3 (K2O-MgO-Al2O3 3성분계에서 K+-β/β"-Al2O3의 합성 및 상관계)

  • Ham, Choul-Hwan;Lim, Sung-Ki;Lee, Chung-Kee;Yoo, Seung-Eul
    • Applied Chemistry for Engineering
    • /
    • v.10 no.7
    • /
    • pp.1086-1091
    • /
    • 1999
  • $K^+-{\beta}/{\beta}"-Al_2O_3$ in the ternary system $K_2O-MgO-Al_2O_3$ was directly synthesized by solid state reaction. The phase formation and phase relation were carefully investigated in relation to starting composition, calcining temperature and time, and dispersion medium. The optimal synthetic condition was also examined for the formation of ${\beta}"-Al_2O_3$ phase with a maximum fraction. As a composition range, the mole ratio of $K_2O$ to $Al_2O_3$ was changed from 1:5 to 1:6.2 and the amount of MgO used as a stabilizer was varied from 4.2 wt % to 6.3 wt %. The calcining temperature was selected between $1000^{\circ}C$ and $1500^{\circ}C$. At $1000^{\circ}C$, the ${\beta}/{\beta}"-Al_2O_3$ phases began to form resulted from the combining of ${\alpha}-Al_2O_3$ and $KAlO_2$ and increased with temperature rising. All of ${\alpha}-Al_2O_3$ phase disappeared to be homogenized to the ${\beta}/{\beta}"-Al_2O_3$ phase at $1200^{\circ}C$. Near the temperature at $1300^{\circ}C$, the fraction of ${\beta}"-Al_2O_3$ phase showed a maximum value with the composition of $K_{1.67}Mg_{0.67}Al_{10.33}O_{17}$. At temperatures above $1300^{\circ}C$, the fraction of ${\beta}"-Al_2O_3$ phase decreased gradually owing to $K_2O$ loss caused by a high potassium vapor pressure, and the appropriate calcining time was about 5 hours. Acetone was more effective than distilled water as a dispersion medium for milling and mixing.

  • PDF

Conformation and Biological Activity of the Neuropeptide $\gamma$ (Neuropeptide $\gamma$의 구조 및 생리활성)

  • Ku Hee-Jung;SEO Jung-Kil;KIM Eun-Hi;HUH Min-Do;CHUNG Joon-Ki;PARK Jang-Su;KANG Shin-Won;PARK Nam Gyu
    • Korean Journal of Fisheries and Aquatic Sciences
    • /
    • v.30 no.2
    • /
    • pp.244-251
    • /
    • 1997
  • The relationship between structure and biological activity was studied on the three neuropeptides (mammalian, trout- and goldfish-neuropeptide $\gamma$) that were syntheized by the solid-phase method. Circular dichroism spectra showed that mammalian, trout- and goldfish-neuropeptide $\gamma$ adopted an unordered structure in buffer solution. In the-presence of neutral and acidic liposomes, mammalian and trout-neuropeptioe $\gamma$ also took a random structure. However, goldfish-neuropeptide $\gamma$ took an $\alpha-helical$ structure in acidic liposomes. The intestinal motility response was investigated with carp intestines, guinea-pig ileums and rat duodenums. In case of carp intestine, contractile activity was as follows : goldfish-neuropeptide $\gamma\simeq$ trout-neuropeptide $\gamma>$ mammalian-neuropeptide $\gamma$, On the other hand, the contractile activity of mammalian-neuropeptide $\gamma$ was more potent than trout- and goldfish-neuropeptide $\gamma$ in the guinea-pig ileums and rat duodenums. These results suggest that neuropeptide $\gamma$ show the species-specific activity.

  • PDF

Development and Characterization of Trans Free Margarine Stock from Lipase-Catalyzed Interesterification of Avocado and Palm Oils (팜유와 아보카도유로부터 효소적 interesterification을 통한 trans free margarine stock 제조 및 이화학적 특성 연구)

  • Lee, Yun-Jeung;Lee, Ki-Teak
    • Korean Journal of Food Science and Technology
    • /
    • v.41 no.3
    • /
    • pp.231-237
    • /
    • 2009
  • Trans free margarine stock (TFMS) was produced by lipase-catalyzed synthesis of fully hydrogenated soybean oil (FHSBO), avocado oil (AO) and palm oil (PO). A blend of FHSBO, AO, and PO with a 1:5:4 (30:150:120 g, respectively) ratio was interesterified with lipozyme RM IM(from Rhizomucor miehei) in a 1 L-batch type reactor at 65 for 12 hr, and the physicochemical and melting properties of TFMS were compared with commercial margarine. The solid fat content (%) of the TFMS was analyzed at 25, 30, and $35^{\circ}C$, respectively, while its melting point was $37.8^{\circ}C$. The trans fatty acid content of the TFMS was below 0.1%. It also had acid, saponification, and iodine values of 0.4, 173.9, and 58.6, respectively. In HPLC chromatograms of the TFMS, newly synthesized peaks of triacylglycerol molecules were observed by using reverse-phase HPLC with evaporative light-scattering detection. Normal-phase HPLC with UV detection was used to quantify tocopherols in the TFMS, indicating that its ${\alpha}-$, ${\gamma}-$ and ${\delta}$-tocopherol contents were 5.7, 2.1, and 1.7 mg/100 g, respectively.

Synthesis and characterization of perovskite nano-sized (Pb, La)$TiO_3$ powder using mechano chemical process (기계화학공정을 이용한 Perovskite 구조의 (Pb, La)$TiO_3$ 나노 분말 합성 및 특성)

  • Lim, Bo-Ra-Mi;Yang, Jae-Kyo;Lee, Dong-Suk;Noh, Tae-Hyung;Seo, Jung-Hye;Lee, Youn-Seoung;Kim, Hee-Taik;Choa, Yong-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.18 no.5
    • /
    • pp.200-204
    • /
    • 2008
  • Mechano Chemical Process (MCP) skips the calcinations steps at an intermediate temperature that is always required in the conventional solid-state reaction because forming phase from raw powder is activated by mechanical energy. In this study, we prepared (Pb, La)$TiO_3$ nanopowder with perovskite structure by only high energy MCP. Especially, the PLT nanopowder was synthesized without any thermal treatment using oxides, not salts as raw powder. This process is also very simple due to dry milling method, unnecessary to dry of powder. The oxide powder was milled up to 12 hr at intervals of an hour using MCP and the pure PLT phase of perovskite structure was formed after milling time of 3 hr. And the average particle size was 20 nm with narrow distribution after milling time of 3 hr from raw powder of several $\mu m$ with inhomogeneous distribution.

Adipic Acid Assisted Sol-Gel Synthesis of Li1+x(Mn0.4Ni0.4Fe0.2)1-xO2 (0 < x < 0.3) as Cathode Materials for Lithium Ion Batteries

  • Karthikeyan, Kaliyappan;Amaresh, Samuthirapandian;Son, Ju-Nam;Kim, Shin-Ho;Kim, Min-Chul;Kim, Kwang-Jin;Lee, Sol-Nip;Lee, Yun-Sung
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.1
    • /
    • pp.89-94
    • /
    • 2013
  • Layered $Li_{1+x}(Mn_{0.4}Ni_{0.4}Fe_{0.2})_{1-x}O_2$ (0 < x < 0.3) solid solutions were synthesized using solgel method with adipic acid as chelating agent. Structural and electrochemical properties of the prepared powders were examined by means of X-ray diffraction, Scanning electron microscopy and galvanostatic charge/discharge cycling. All powders had a phase-pure layered structure with $R\bar{3}m$ space group. The morphological studies confirmed that the size of the particles increased at higher x content. The charge-discharge profiles of the solid solution against lithium using 1 M $LiPF_6$ in EC/DMC as electrolyte revealed that the discharge capacity increases with increasing lithium content at the 3a sites. Among the cells, $Li_{1.2}(Mn_{0.32}Ni_{0.32}Fe_{0.16})O_2$ (x = 0.2)/$Li^+$ exhibits a good electrochemical property with maximum initial capacity of 160 $mAhg^{-1}$ between 2-4.5 V at 0.1 $mAcm^{-2}$ current density and the capacity retention after 25 cycles was 92%. Whereas, the cell fabricated with x = 0.3 sample showed continuous capacity fading due to the formation of spinel like structure during the subsequent cycling. The preparation of solid solutions based on $LiNiO_2-LiFeO_2-Li_2MnO_3$ has improved the properties of its end members.

Enzymatic Synthesis of Low Trans Fats Using Rice Bran Oil, Palm Stearin and High Oleic Sunflower Seed Oil (미강유, 팜스테아린 및 고올레인산 해바라기씨유를 이용한 저트랜스 유지의 효소적 합성)

  • Kim, Ji-Young;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.38 no.4
    • /
    • pp.470-478
    • /
    • 2009
  • Low trans fats were synthesized by interesterification of rice bran oil (RBO), palm stearin (PS) and high oleic sunflower seed oil (HO) using TLIM from Thermomyces lanuginosa. After 24-h reaction, physicochemical characteristics such as fatty acid and triacylglycerol composition, solid fat content, melting point, tocopherol, oryzanol and phytosterol contents were evaluated. Trans fatty acid contents of the produced low-trans fats showed less than 0.5 wt%. Mostly, triacylglycerol species in the products were palmitoyl-linoleoyl-oleoyl-glycerol (PLO), palmitoyl-oleoyl-oleoyl-glycerol (POO) and palmitoyl-oleoyl-palmitoyl-glycerol (POP). Total tocopherol contents ranged from 6.94 to 11.83 mg/100 g while $0.18{\sim}0.49$ mg/100 g of $\gamma$-oryzanol and $182.47{\sim}269.08$ mg/100 g of phytosterols were observed depending on the substrates ratios. When the content of PS in the reaction substrate was increased, solid fat content and slip melting points were increased.

Synthesis and Conductive Properties of Li1+xAlxTi2-x(PO4)3 (x = 0, 0.3, 0.5) by Sol-Gel Method (Sol-Gel법에 의한 Li1+xAlxTi2-x(PO4)3 (x = 0, 0.3, 0.5)의 합성 및 전도특성)

  • Moon, Jung-In;Cho, Hong-Chan;Song, Jeong-Hwan
    • Korean Journal of Materials Research
    • /
    • v.22 no.7
    • /
    • pp.346-351
    • /
    • 2012
  • $Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.

Synthesis and Optical Property of (GaN)1-x(ZnO)x Nanoparticles Using an Ultrasonic Spray Pyrolysis Process and Subsequent Chemical Transformation (초음파 분무 열분해와 화학적 변환 공정을 이용한 (GaN)1-x(ZnO)x 나노입자의 합성과 광학적 성질)

  • Kim, Jeong Hyun;Ryu, Cheol-Hui;Ji, Myungjun;Choi, Yomin;Lee, Young-In
    • Journal of Powder Materials
    • /
    • v.28 no.2
    • /
    • pp.143-149
    • /
    • 2021
  • In this study, (GaN)1-x(ZnO)x solid solution nanoparticles with a high zinc content are prepared by ultrasonic spray pyrolysis and subsequent nitridation. The structure and morphology of the samples are investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The characterization results show a phase transition from the Zn and Ga-based oxides (ZnO or ZnGa2O4) to a (GaN)1-x(ZnO)x solid solution under an NH3 atmosphere. The effect of the precursor solution concentration and nitridation temperature on the final products are systematically investigated to obtain (GaN)1-x(ZnO)x nanoparticles with a high Zn concentration. It is confirmed that the powder synthesized from the solution in which the ratio of Zn and Ga was set to 0.8:0.2, as the initial precursor composition was composed of about 0.8-mole fraction of Zn, similar to the initially set one, through nitriding treatment at 700℃. Besides, the synthesized nanoparticles exhibited the typical XRD pattern of (GaN)1-x(ZnO)x, and a strong absorption of visible light with a bandgap energy of approximately 2.78 eV, confirming their potential use as a hydrogen production photocatalyst.

Production of pediocin by Chemical Synthesis and Bactericidal Mode of Action

  • Koo, Min-Seon;Kim, Wang-June;Kwon, Dea-Young;Min, Kyung-Hee
    • Proceedings of the Korean Society for Applied Microbiology Conference
    • /
    • 2001.06a
    • /
    • pp.149-153
    • /
    • 2001
  • To investigate the mode of bactericidal action for antimicrobial peptide, pediocin, synthetic and mutant pediocins were prepared by direct chemical synthesis. Native pediocin was purified from Pedio-coccus acidilactici M and its conformational structure and bactericidal functions were analyzed and compared to synthetic pediocin. Schematic mode of pediocin actions, how pediocin binds on the target cell membrane, penetrates and makes tunnel are proposed. For these purposes, primary and secondary structures of pediocin was analyzed and disulfide bond assignment was also done. The pediocin purified from P. acidilactici M had high effective bactericidal ability against gram positive bacteria, especially Listeria monocytogenes and was very stable at extreme pHs and even at high temperatures such as autoclaving temperature (121$^{\circ}C$). Pediocin was consisted of 44 amino acids with four cysteines. Novel synthetic peptides were achieved by solid phase peptide synthesis(SPPS) method. To explain the function of cysteine in C-terminal region, mutant pediocin, Ped[C24A+C44A], was synthesized and their structural and biological functions were analyzed. Second mutant pediocin, Ped[KllE], was prepared to explain the function of lysine at 11 of N-terminal part of pediocin, especially loop of $\beta$-sheet, and to predict the initial binding site of pediocin. The native and synthetic pediocins was showed random coil conformation by spectropolarimetry in moderate conditions. This conformation was observed in extreme conditions such as high temperature and low and high pHs, also. Circular dichroism(CD) data also showed the existence of $\beta$-turn structure in N-terminal part both native and synthetic pediocins. A structural model for pediocin predicts that 18 amino acids in the N-terminal part of the peptide assume a three-strand $\beta$-sheet conformation. This random coil in C-terminal part of pediocin was converted to folding structure, helix structure, in nonpolar solvents such as alcohol and TFE. The disulfide bond between $^{9}$ Cys and $^{14}$ Cys was concrete and inevitable, however, evidences of disulfide bond between $^{24}$ Cys and $^{44}$ Cys was not. Data of Ped[C24A+C44A], pediocin mutant showed that $^{44}$ Cys was required during killing the target cells but not inevitable, since Ped[C24A+C44A] still have bactericidal activity but much less than native pediocin. Another pediocin mutant, Ped[KllE], had still bactericidal activity, was controversial to propose that positive charge like as $^{11}$ Lys in loop or hinge in bacteriocin bound or helped to binding to microorganism with electrostatic interaction between cell membrane especially teichoic acid and positive amino acid nonspecifically. The conformation of pediocin among native, synthetic and mutant pediocins did not show big difference. The conformations between oxidized and reduced pediocin were almost similar regardless of native or synthetic.

  • PDF

Synthesis of Borosilicate Zeotypes by Steam-assisted Conversion Method (수증기 쪼임법에 의한 제올라이트형 보로실리케이트 제조방법)

  • Mansour, R.;Lafjah, M.;Djafri, F.;Bengueddach, A.
    • Journal of the Korean Chemical Society
    • /
    • v.51 no.2
    • /
    • pp.178-185
    • /
    • 2007
  • Intermediate pentasil borosilicate zeolite-like materials have been crystallized by a novel method named steam-assisted conversion, which involves vapor-phase transport of water. Indeed, amorphous powders obtained by drying Na2O.SiO2.B2O3.TBA2O gels of various compositions using different boron sources are transformed into crystalline borosilicate zeolite belonging to pentasil family structure by contact with vapors of water under hydrothermal conditions. Using a variant of this method, a new material which has an intermediate structure of MFI/MEL in the ratio 90:10 was crystallized. The results show that steam and sufficiently high pH in the reacting hydrous solid are necessary for the crystallization to proceed. Characterization of the products shows some specific structural aspects which may have its unique catalytic properties. X-ray diffraction patterns of these microporous crystalline borosilicates are subjected to investigation, then, it is shown that the product structure has good crystallinity and is interpreted in terms of regular stacking of pentasil layers correlated by inversion centers (MFI structure) but interrupted by faults consisting of mirror-related layers (MEL structure). The products are also characterized by nitrogen adsorption at 77 K that shows higher microporous volume (0.160 cc/g) than that of pure MFI phase (0.119 cc/g). The obtained materials revealed high surface area (~600 m2/g). The infrared spectrum reveals the presence of an absorption band at 900.75 cm-1 indicating the incorporation of boron in tetrahedral sites in the silicate matrix of the crystalline phase.