• Title/Summary/Keyword: Hydrolysis-condensation reaction

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Interpretation of Hydrothermal Synthesis of BaTiO3 Powder (BaTiO3 분말의 수열합성 해석)

  • Oh, Jung Kang;Seo, Kyung Won
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.509-514
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    • 1999
  • In Preparing $BaTiO_3$ powder under hydrothermal conditions, effects of reaction period feedstock concentration and mixing rate on crystallinity, mean size and size distribution of particles were studied. Experimental results showed that the particle size became smaller with its narrow distribution as the reaction period and mixing rate increased, but feedstock concentration decreased in contrast with the results based on the classical nucleation-growth model. From these results, $BaTiO_3$ particles seem to be prepared hydrothermally through a multiple reaction procedure that includes dissolution, precipitation, hydrolysis-condensation, aggregation, diffusion and transformation.

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Control of Molecular Weight, Stereochemistry and Higher Order Structure of Siloxane-containing Polymers and Their Functional Design

  • Yusuke Kawakami;Yuning Li;Yang Liu;Makoto Seino;Chitsakon Pakjamsai;Motoi Oishi;Cho, Yeong-Bee;Ichiro Imae
    • Macromolecular Research
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    • v.12 no.2
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    • pp.156-171
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    • 2004
  • We describe the precision synthesis schemes of siloxane-containing polymers, i.e., the control of their molecular weight, stereoregularity, and higher-order structures. First, we found a new catalytic dehydrocoupling reaction of water with bis(dimethylsilyl)benzene to give poly(phenylene-disiloxane). Together with this reaction, we applied hetero-condensations to the synthesis of thermally stable poly(arylene-siloxane)s. The dehydrocoupling reaction was applied to the synthesis of syndiotactic poly(methylphenylsiloxane) and poly(silsesquioxane)s, which we also prepared by hydrolysis and deaminative condensation reactions. We discuss the tendency for loop formation to occur in the synthesis of poly(silsesquioxane) by hydrolysis, and provide comments on the design of functionality of the polymers produced. By taking advantage of the low energy barrier to rotation in the silicon-oxygen bond, we designed selective oxygen-permeable membrane materials and liquid crystalline materials. The low surface free energy of siloxane-containing systems allows surface modification of a blend film and the design of holographic grating materials.

Material and rheological properties of (glycidoxypropyl) trimethoxysilane modified colloidal silica coatings

  • Kang Hyun Uk;Park Jung Kook;Kim Sung Hyun
    • Korea-Australia Rheology Journal
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    • v.16 no.4
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    • pp.175-182
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    • 2004
  • Colloidal coating solution was prepared to enhance the hydrophilic property of the film surface. Water and ethanol were used as the dispersion media and (glycidoxypropyl) trimethoxysilane (GPS) as a binder in the colloidal silica coatings. Ethylene diamine was added to the colloidal silica solution as the curing agent. The colloidal silica solution was regarded as a hard-sphere suspension model with low volume fraction of the silica particles. Rheological properties of the silica suspensions modified with GPS have been investigated as a function of pH and concentration. The acidic solution showed high viscosity change by fast hydrolysis reaction and adsorption of the organic binders on the surface of silica particles. However, the hydrolysis was slow at the basic condition and the binders combined with themselves by condensation. The viscosity change was smallest at pH 7. The viscosity increased with the curing time after adding ethylenediamine, and the increase of viscosity at low pH was higher than that at high pH. The hydrophilic properties of the coating film were investigated by the contact angle of water and film surface. The smallest contact angle was shown under the strong acidic condition of pH 2.

The Synthesis of Vanadium-Doped Forsterite by the $H_2O_2$-Assisted Sol-Gel Method, and the Growth of Single Crystals of Vanadium-Doped Forsterite by the Floating Zone Method

  • 박동곤;Mikio Higuchi;Rudiger Dieckmann;James M. Burlitch
    • Bulletin of the Korean Chemical Society
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    • v.19 no.9
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    • pp.927-933
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    • 1998
  • Polycrystalline powder of vanadium-doped forsterite (Vδ $Mg_2SiO_4$) was synthesized by the $H_2O_2$-assisted sol-gel method. The vanadium dopant, which was added as VO$(OMe)_3$ in methanol, went through several redox reactions as the sol-gel reaction proceeded. Upon adding VO$(OMe)_3$ to a mixture of $Mg(OMe)_2$ and Si$(OEt)_4$ in methanol, V(V) reduced to V(IV). As hydrolysis reaction proceeded, the V(IV) oxidized all back to V(V). Apparently, some of the V(V) reduced to V(IV) during subsequent gelation by condensation reaction. The V(IV) remained even after heat treatment of the gel in highly oxidizing atmosphere. The crystallization of the xerogel around 880 ℃ readily produced single phase forsterite without any minor phase. Using the polycrystalline powder as feeding stock, single crystals of vanadium-doped forsterite were grown by the floating zone method in oxidizing or reducing atmosphere. The doping was limited in low level because of the high partitioning of the vanadium in liquid phase during melting. The greenish single crystal absorbed visible light of 700∼1100 nm. But, no emission was obtained in near infrared range.

Epoxidation of Styrene using Nanosized γ-Al2O3/NiO Heterogeneous Catalyst Derived from the P123 Surfactant

  • Son, Boyoung;Jung, Miewon
    • Journal of the Korean Ceramic Society
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    • v.49 no.5
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    • pp.423-426
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    • 2012
  • $Al_2O_3$/NiO powder was obtained through hydrolysis-condensation reactions and thermal treatments. An organic additive, triblock copolymer surfactant P123, was added to the starting materials to control the surface area and morphology. The synthesized powder was characterized by X-ray diffractometry (XRD), field-emission scanning electron microscopy (FE-SEM) and a Brunner-Emmett-Teller surface analysis (BET). The heterogeneous catalytic activity of this powder was applied to an epoxidation reaction of styrene and was monitored using a gas chromatograph with mass spectrophotometry (GC/MS).

Synthesis of $(\pm)-\alpha-Hydroxy-\alpha$-(p-Chlorobiphenyl)Acetic Acid and its Resolution ($(\pm)-\alpha-Hydroxy-\alpha$-(p-Chlorobiphenyl)acetic acid 합성과 분할)

  • 권순경
    • YAKHAK HOEJI
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    • v.39 no.4
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    • pp.433-437
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    • 1995
  • Optically pure(-)-and (+)-$\alpha$-hydroxy-$\alpha$-(p-chlorobiphenyl)acetic acids were prepared. The racemate was synthesized through three steps. By condensation of p-cnorobiphenyl with diethyl ketomalonate in the presence of SnCl$_{4}$, diethyl $\alpha$-hydroxy-$\alpha$-(p-chlorobiphenyl)malonate (1) was formed and subsequently ($\pm$)-$\alpha$-hydroxy-$\alpha$-(p-chlorobiphenyl)acetic acid (3) was obtained through hydrolysis and decarboxylation. For the separation of the racemate the classical resolution method, derivatization of a racemate by reaction with an optically pure compound was employed. In this case the optically pure compound were [R]-(+)-$\alpha$-methylbenzylamine and [S]-(-)-$\alpha$-methylbenzylamine. Diastereomeric salts between acids and bases could be easily separated by crystallization in absolute ethanol.

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Optical Characterization of Azo-dye Attached on Photonic Crystal: The Cause of Large Absorption Band Shift

  • Kim, Byoung-Ju;Kwon, Ki-Chul;Yu, A-Reum;Kang, Kwang-Sun
    • Current Photovoltaic Research
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    • v.5 no.2
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    • pp.43-46
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    • 2017
  • Large absorption band shift has been observed for the azo-dye (disperse red-13, DR-13) attached on the surface of silica spheres. Urethane linkage has been utilized to form covalent bond between azo-dye (-OH) and 3-isocyanatopropyltriethoxysilane (ICPTES, -N=C=O). The synthesized ICPTES-DR-13 (ICPDR) molecules were attached to the silica spheres by the hydrolysis and condensation reaction. Although the absorption peak of DR-13 in methanol is at 510 nm, the absorption peak of the ICPDR-silica spheres shifts to 788 nm. The large absorption peak shift is due to the formation of intramolecular charge-transfer band with large aggregated ICPDR.

Control of Pore Characteristics of Porous Glass in the $ZrO_2.SiO_2$ System Prepared by the Sol-Gel Method (졸-겔법으로 제조한 $ZrO_2.SiO_2$다공질유리의 세공제어)

  • 신대용;한상목
    • Journal of the Korean Ceramic Society
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    • v.30 no.6
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    • pp.485-491
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    • 1993
  • Porous glass in the ZrO2.SiO2 system containning up to 30mol% zirconia were prepared by the sol-gel method from metal alkoxides and their pore characteristics with reaction parameters were investigated. The gels were made by hydrolyzing and condensation of the mixed metla alkoxides and were converted into the porous glass by heating up to $700^{\circ}C$. As a results, the mean pore radius became larger with increasing contents of HCl, H2O and hydrolysis temperature, and an alcohol with a large molecular weight for making the porous glass. In the case of 20ZrO2.80SiO2 porous glass with heated at $700^{\circ}C$, HCl and H2O content was 0.3mol and 4mol, the specific surface area was 284$m^2$/g, average mean pore radius was about 19.4$\AA$, porosity was 22.55% and pore characteristics depended on heating temperature.

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Design and Synthesis of Novel 2'(β)-Fluoro-3'(α)-hydroxy-threose Nucleosides: Iso-FMAU Analogues as Potent Antiviral Agents

  • Kim, Seyeon;Jee, Jun-Pil;Hong, Joon Hee
    • Journal of Integrative Natural Science
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    • v.8 no.2
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    • pp.99-106
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    • 2015
  • Novel 2'(${\beta}$)-fluoro-3'(${\alpha}$)-hydroxy-threose nucleosides (iso-FMAU) as antiviral agents were designed and racemically synthesized from Solketal. Condensation successfully proceeded from a glycosyl donor 9 under $Vorbr{\ddot{u}}ggen$ conditions yielded the nucleoside analogues. Ammonolysis and hydrolysis of isopropylidene protection group gave the desired nucleoside analogues 12, 15, 18, and 19. The antiviral activities of the synthesized compounds were evaluated against the HIV-1, HSV-1, HSV-2 and HCMV. Compound 12 displayed some anti-HCMV activity ($EC_{50}=24.7{\mu}g/ml$) without exhibiting any cytotoxicity up to $100{\mu}M$.

Preparation and Physical Properties of Poly(lactic acid) Bio-Composites using Surface Modified Microfibriled Celluloses

  • Yeo, Jun-Seok;Seong, Dong-Wook;Hwang, Seok-Ho
    • Elastomers and Composites
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    • v.50 no.1
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    • pp.62-67
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    • 2015
  • The surface modification of microfibriled cellulose (MFC) was carried out through the hydrolysis-condensation reaction using (3-aminopropyl)triethoxysilane (APS) and 3-glycidyloxypropyltriethoxysilane (GPS) and then the modified cellulose was compounded with bio-degradable poly(lactic acid) (PLA). Also, pristine MFC was compounded with PLA as a control groups. The confirmation of surface modification for the pristine MFC was characterized by FT-IR and SEM/EDX. The thermal and mechanical properties of the PLA/MFC composites depended on the content of MFC and the type of silane coupling agents. From the thermal, morphological and mechanical behaviors of the PLA/MFC composites, it was found that GPS-MFC was more successful to improve the interface adhesion between PLA matrix and the surface of MFC than that of APS-MFC.