• Title/Summary/Keyword: Zirconium sulfate

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Characterization of Zirconium Sulfate Supported on Zirconia and Activity for Acid Catalysis

  • Son, Jong Rak;Gwon, Tae Dong;Kim, Sang Bok
    • Bulletin of the Korean Chemical Society
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    • v.22 no.12
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    • pp.1309-1315
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    • 2001
  • Zirconium sulfate supported on zirconia catalysts were prepared by impregnation of powdered $Zr(OH)_4$ with zirconium sulfate aqueous solution followed by calcining in air at high temperature. The characterization of prepared catalysts was performed using Fourier transform infrared (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and by the measurement of surface area. The addition of zirconium sulfate to zirconia increased the phase transition temperature of $ZrO_2$ from amorphous to tetragonal due to the interaction between zirconium sulfate and zirconia, and the specific surface area and acidity of catalysts increased in proportion to the zirconium sulfate content up to 10 wt% of $Zr(SO_4)_2$. Infrared spectra of ammonia adsorbed on $Zr(SO_4)2}ZrO_2$ showed the presence of Bronsted and Lewis acid sites on the surface. $10-Zr(SO_4)_2}ZrO_2$ calcined at $600^{\circ}C$ exhibited maximum catalytic activities for 2-propanol dehydration and cumene dealkylation. The catalytic activities for both reactions were correlated with the acidity of catalysts measured by ammonia chemisorption method.

The Preparation and Thermal Decomposition of the Basic Zirconium Sulfate (Basic Zirconium Sulfate의 제조와 그 열분해 거동)

  • 석상일;정하균;주명희;박도순
    • Journal of the Korean Ceramic Society
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    • v.27 no.6
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    • pp.707-712
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    • 1990
  • The basic zirconium sulfate was prepared from ZrOCl2.8H2O and H2SO4 in the 9$0^{\circ}C$ aqueous solution. The pH and amount of unreacted zirconium in the solution that reacton had completed was 0.2 and 10%. As the pH was increased to 1.4 by NH4OH theresulting precipitates were the mixtures of the basic zirconium sulfate and the zirconium hydroxide although the precipitates were recovered completely. The thermal decomposition behavior of this sample has been examined by thermal analysis(TG-DTA), X-ray diffraction study, infrared spectroscopy and sulfur analysis. As a result, it was found that the precipitates have perfectly been decomposed at 85$0^{\circ}C$ accompanying to the release of a molecule of water below 25$0^{\circ}C$ and 85% sulfate at about $600^{\circ}C$. The thermally decomlposed products were initially amorphous phase, which were become metastable tetragonal phase with increment of temperature and finally transformed to the stable monoclinic phase at 100$0^{\circ}C$.

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Removal Characteristics of Phosphorus at Synthetic Variation of Zirconium Mesoporous Structure (지르코늄 메조기공 구조체의 합성조건 변화에 따른 인 제거 특성)

  • Lee, Sang-hyup;Lee, Byoung-cheun;Lee, Kwan-yong;Choi, Yong-su;Park, Ki-young
    • Journal of Korean Society on Water Environment
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    • v.21 no.6
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    • pp.637-642
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    • 2005
  • The focus of this study was to examine the phosphorus removal characteristic by zirconium mesoporous structured material synthesized on various conditions. The zirconium sulfate-surfactant mesoporous structured material(ZS) was synthesized by hydro-thermal synthesis. The material has regular hexagonal array of surfactant micelles and sulfate ion ($HSO_4{^-}$). We confirmed that sulfate ion in zirconium mesoporous structured material can be ion-exchanged with phosphate ion ($H_2PO_4{^-}$) in phosphoric acid solution. On the X-ray diffraction (XRD) pattern of ZS, three peaks which shows the important characteristics of hexagonal crystal lattice were observed at (100), (110) and (200). The transmission electron micrograph (TEM) show high crystallization with pore size about $47{\AA}$. The maximum adsorption capacity of ZS was as great as 3.2 mmol-P/g-ZS. From the adsorption isotherm, correlation coefficients were higher for the Langmuir isotherm than the Freundlich isotherm. With the respect of chain length of surfactant, the adsorption capacity for phosphate synthesized with C12 was higher than C16 and C18. The highest amount of adsorbed phosphate on ZS was observed at the surfactant-to-zirconium molar ratio of 0.5 to 1.

The Phosphorus Removal from Water by Zirconium Mesoporous Structure (지르코늄 메조기공 구조체를 이용한 수중의 인 제거)

  • Lee, Byoung-cheun;Lee, Kwan-yong;Lee, Sang-hyup;Choi, Yong-su;Park, Ki-young
    • Journal of Korean Society of Water and Wastewater
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    • v.19 no.4
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    • pp.455-461
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    • 2005
  • This study was designed to investigate the fundamental aspects of a possible recovery of phosphorus strategy from wastewater by using the zirconium mesoporous structured materials as a new type of ion exchangers. Zirconium mesoporous structure material was synthesized by hydro-thermal synthesis. The synthesized zirconium mesoporous structure was examined by X-ray diffraction (XRD) and Transmission electron micrograph (TEM). From the results of XRD and TEM, it was found out that hexagonal mesoporous structure, pore size was about $47{\AA}$, was synthesized. Experimental results showed that the complex of zirconium sulfate tetrahydrate and surfactant micelles had very high ability for capture of phosphorus. The amount of phosphate ions exchanged into the solid was as great as 3.4mmol/g-ZS. And the ion exchange reaction was occurred between $PO_4{^{3-}}$ and $SO_4{^{2-}}$ and also between $PO_4{^{3-}}$ and $OH^-$. Therefore, it is possible to get the higher removal efficiency than other ion exchange media and adsorbent.

Synthesis and Phosphorus Adsorption Characteristics of Zirconium Magnetic Adsorbent Having Magnetic Separation Capability (자기분리가 가능한 지르코늄 자성 흡착제의 합성과 인 흡착 특성)

  • Lim, Dae-Seok;Kim, Yeon-Hyung;Kim, Dong-Rak;Lee, Tae-Gu;Lim, Hak-Sang
    • Journal of Korean Society of Water and Wastewater
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    • v.26 no.3
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    • pp.431-442
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    • 2012
  • The purpose of this study, is to separate magnetic separation devices using permanent magnets by using magnetization characteristics remaining in treated water after adsorption and synthesizing phosphorus adsorbent capable of magnetic separation for efficient removal of phosphorus. The synthesis of the adsorbent which set Zirconium(Zr) having high friendly features for phosphorus as an element, and by synthesizing Iron Oxide($Fe_3O_4$, another name of $Fe_3O_4$ is magnetite) being able to grant magnetism to Zirconium Sulfate($Zr(SO_4)_2$), zirconium magnetic adsorbent(ZM) were manufactured. In order to consider the phosphorus adsorption characteristics of adsorbent ZM, batch adsorption experiment was performed, and based on the results, pH effect, adsorption isotherm, adsorption kinetics, and magnetic separation have been explore. As the experiment result, adsorbent ZM showed a tendency that the adsorption number was decreased rapidly at pH 13; however, it was showed a high amount of phosphorus removal in other range and it showed the highest amount of phosphorus removal in pH 6 of neutral range. In addtion, the Langmuir adsorption isotherm model is matched well, and D-R adsorption isotherm model is ranged 14.43kJ/mol indicating ion exchange mechanism. The result shown adsorption kinetics match well to the Pseudo-second-order kinetic model. The adsorbent ZM's capablility of regenerating NaOH and $H_2SO_4$, was high selectivity on the phosphorus without impacts on the other anions. The results of applying the treated water after adsorption of phosphorus to the magnetic separation device by using permanent magnets, shows that capture of the adsorbent by the magnetization filter was perfect. And they show the possibility of utilization on the phosphorus removal in water.

CeO2-Promoted Highly Active Catalyst, NiSO4/CeO2-ZrO2 for Ethylene Dimerization

  • Pae, Young-Il;Shin, Dong-Cheol;Sohn, Jong-Rack
    • Bulletin of the Korean Chemical Society
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    • v.27 no.12
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    • pp.1989-1996
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    • 2006
  • The $NiSO_4/CeO_2-ZrO_2 $catalysts containing different nickel sulfate and $CeO_2$ contents were prepared by the impregnation method, where support, $CeO_2-ZrO_2$was prepared by the coprecipitation method using a mixed aqueous solution of zirconium oxychloride and cerium nitrate solution followed by adding an aqueous ammonia solution. No diffraction line of nickel sulfate was observed up to 20 wt %, indicating good dispersion of nickel sulfate on the surface of $CeO_2-ZrO_2$. The addition of nickel sulfate (or $CeO_2$) to $ZrO_2$ shifted the phase transition of $ZrO_2$ from amorphous to tetragonal to higher temperatures because of the interaction between nickel sulfate (or $CeO_2$) and $ZrO_2$. A catalyst (10-$NiSO_4/1-CeO_2-ZrO_2$) containing 10 wt % $NiSO_4$ and 1 mole % $CeO_2$, and calcined at $600{^{\circ}C}$ exhibited a maximum catalytic activity for ethylene dimerization. The catalytic activities were correlated with the acidity of catalysts measured by the ammonia chemisorption method. The role of $CeO_2$was to form a thermally stable solid solution with zirconia and consequently to give high surface area, thermal stability and acidity of the sample.

Zirconia Coating of SiC Whiskers Using the Aqueous Solutions of Zr(SO4)2 ($Zr(SO_4)_2$ 수용액을 이용한 SiC 휘스커의 지르코니아 코팅)

  • Kim, Duk-Jun;Kim, Hwan
    • Journal of the Korean Ceramic Society
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    • v.33 no.12
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    • pp.1380-1386
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    • 1996
  • The effects of urea addition and reaction conditions were examined in the prepareation of zirconia coated SiC whiskers through surface precipitation taking place during high-temperature aging of Zr(SO4)2 solutions containing the whiskers. More dense zirconia-hydrate was precipitated on the surfaces of the whiskers in the presence of urea. The ratio of the concentration of Zr(SO4)2 to the amount of added whiskers was the most important factor to confine the precipitation of zirconia-hydrate only at the surfaces of the whiskers The from of the coating layers was unchanged after heat-treatment leading to the dehydration and crystallization of the layers.

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The properties of glass ceramic of LAS system with Y2O3 and Fe2O3 (Y2O3와 Fe2O3가 포함된 LAS 계 결정화 유리 특성)

  • Lee, Ji-Sun;Lim, Tae-Young;Hwang, Jonghee;Lee, Youngjin;Jeon, Dae-Woo;Kim, Sun-Woog;Ra, Yong-Ho;Kim, Jin-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.29 no.4
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    • pp.154-159
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    • 2019
  • The glass-ceramic of $Li_2O-Al_2O_3-SiO_2$ system was fabricated by using yttrium oxide and iron oxide that it can reduce the melting temperature and affect the homogenization. Zirconium sulfate was used as a nucleation agent. Calcium phosphate was used to improve the flow the glass so as reduce the viscosity of the glass. The glass-ceramics met a thermal shock test of more than $750^{\circ}C$ and the temperature at which the coefficient of thermal expansion rapidly increased at over $800^{\circ}C$ was shifted by about the above $30^{\circ}C$. Therefore, it is concluded that the glass-ceramic of $Li_2O-Al_2O_3-SiO_2$ system with yttrium oxide and iron oxide was founded to have good melting conditions and excellent thermal expansion resistance at high temperature such as special field for kitchen utensils.

NiSO4 Supported on FeO-promoted ZrO2 Catalyst for Ethylene Dimerization

  • Sohn, Jong-Rack;Kim, Young-Tae;Shin, Dong-Cheol
    • Bulletin of the Korean Chemical Society
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    • v.26 no.11
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    • pp.1749-1756
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    • 2005
  • The $NiSO_4$ supported on FeO-promoted $ZrO_2$ catalysts were prepared by the impregnation method. FeOpromoted $ZrO_2$ was prepared by the coprecipitation method using a mixed aqueous solution of zirconium oxychloride and iron nitrate solution followed by adding an aqueous ammonia solution. The addition of nickel sulfate (or FeO) to $ZrO_2$ shifted the phase transition of $ZrO_2$ (from amorphous to tetragonal) to higher temperatures because of the interaction between nickel sulfate (or FeO) and $ZrO_2$. 10-$NiSO_4$/5-FeO-$ZrO_2$ containing 10 wt % $NiSO_4$ and 5 mol % FeO, and calcined at 500 ${^{\circ}C}$ exhibited a maximum catalytic activity for ethylene dimerization. $NiSO_4$/FeO-$ZrO_2$ catalysts was very effective for ethylene dimerization even at room temperature, but FeO-$ZrO_2$ without $NiSO_4$ did not exhibit any catalytic activity at all. The catalytic activities were correlated with the acidity of catalysts measured by the ammonia chemisorption method. The addition of FeO up to 5 mol % enhanced the acidity, surface area, thermal property, and catalytic activities of catalysts gradually, due to the interaction between FeO and $ZrO_2$ and due to consequent formation of Fe-O-Zr bond.

INTERGRANULAR CORROSION-RESISTANT STAINLESS STEEL BY GRAIN BOUNDARY ENGINEERING

  • Hiroyuki Kokawa;Masayuki Shimada;Wang, Zhan-Jie;Yutaka S. Sato
    • Proceedings of the KWS Conference
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    • 2002.10a
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    • pp.250-254
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    • 2002
  • Intergranular corrosion of austenitic stainless steels is a conventional and momentous problem during welding and high temperature use. One of the major reasons for such intergranular corrosion is so-called sensitization, i.e., chromium depletion due to chromium carbide precipitation at grain boundaries. Conventional methods for preventing sensitization of austenitic stainless steels include reduction of carbon content in the material, stabilization of carbon atoms as non-chromium carbides by the addition of titanium, niobium or zirconium, local solution-heat-treatment by laser beam, etc. These methods, however, are not without drawbacks. Recent grain boundary structure studies have demonstrated that grain boundary phenomena strongly depend on the crystallographic nature and atomic structure of the grain boundary, and that grain boundaries with coincidence site lattices are immune to intergranular corrosion. The concept of "grain boundary design and control", which involves a desirable grain boundary character distribution, has been developed as grain boundary engineering. The feasibility of grain boundary engineering has been demonstrated mainly by thermomechanical treatments. In the present study, a thermomechanical treatment was tried to improve the resistance to the sensitization by grain boundary engineering. A type 304 austenitic stainless steel was pre-strained and heat-treated, and then sensitized, varying the parameters (pre-strain, temperature, time, etc.) during the thermomechanical treatment. The grain boundary character distribution was examined by orientation imaging microscopy. The intergranular corrosion resistance was evaluated by electrochemical potentiokinetic reactivation and ferric sulfate-sulfuric acid tests. The sensitivity to intergranular corrosion was reduced by the thermomechanical treatment and indicated a minimum at a small roll-reduction. The frequency of coincidence-site-lattice boundaries indicated a maximum at a small strain. The ferric sulfate-sulfuric acid test showed much smaller corrosion rate in the thermomechanically-treated specimen than in the base material. An excellent intergranular corrosion resistance was obtained by a small strain annealing at a relatively low temperature for long time. The optimum parameters created a uniform distribution of a high frequency of coincidence site lattice boundaries in the specimen where corrosive random boundaries were isolated. The results suggest that the thermomechanical treatment can introduce low energy segments in the grain boundary network by annealing twins and can arrest the percolation of intergranular corrosion from the surface.

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