• Title/Summary/Keyword: Tungstosilicic acid

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Silica Supported Tungstosilicic Acid as an Efficient and Reusable Catalyst for the One-Pot Synthesis of β-Acetamido Ketones via a Four-Component Condensation Reaction

  • Nasr-Esfahani, Masoud;Montazerozohori, Morteza;Gholampour, Tahere
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3653-3657
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    • 2010
  • Silica supported tungstosilicic acid has been used as an effective catalyst for a modified Dakin-West one-pot, four-component condensation of an aryl aldehyde, an aryl ketone, acetyl chloride and acetonitrile for the synthesis of $\beta$-acetamido ketones. This catalytic system can act as an active, inexpensive, recoverable and recyclable catalyst. Some advantages of this system are short reaction times, good to excellent yields, easy work up and the ability to be carried out at the large scale reactions.

Removal of acetic acid from wastewater by esterification in the membrane reactor

  • Unlu, Derya;Hilmioglu, Nilufer Durmaz
    • Membrane and Water Treatment
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    • v.7 no.2
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    • pp.143-154
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    • 2016
  • Acetic acid can be removed from wastewater by esterification in a membrane reactor. Pervaporation membrane reactor (PVMR) is an alternative process to conventional separation processes. It is an environmentally friendly process. The main advantages of the PVMR are simultaneous water removal and production of an ester economically. In this study, the synthetic wastewater has been used. Esterification reaction of acetic acid with isopropanol has been studied in the presence of tungstosilicic acid hydrate as a catalyst in a batch reactor and in a PVMR. The effects of important operating parameters such as reaction temperature, initial molar ratio of isopropanol to acetic acid and catalyst concentration has been examined. Removal of acetic acid (conversion of acetic acid) was obtained as 85% using a PVMR by removal of water from the reaction mixture.

The Electrochemical Characteristics of MEA with Pt/Cross-Linked SPEEK-HPA Composite Membranes/Pt-Ru for Water Electrolysis (수전해용 Pt/공유가교 SPEEK-HPA 복합막/Pt-Ru MEA의 전기화학적 특성)

  • Hwang, Yong-Koo;Woo, Je-Young;Lee, Kwang-Mun;Chung, Jang-Hoon;Moon, Sang-Bong;Kang, An-Soo
    • Transactions of the Korean hydrogen and new energy society
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    • v.20 no.3
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    • pp.194-201
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    • 2009
  • The e1ectrocatalytic properties of heteropolyacids(HPAs) entrapped in covalently cross-linked sulfonated polyetheretherketone(CL-SPEEK/HPA) membranes have been studied for water electrolysis. The HPAs, including tungstophosphoric acid(TPA), molybdophosphoric acid(MoPA), and tungstosilicic acid(TSiA) were used as additives in the composite membranes. The MEA was prepared by a non-equilibrium impregnation-reduction(I-R) method, using reducing agent, sodium borohydride(NaBH4) and tetraamineplatinum(II) chloride(pt(NH$_3$)$_4$Cl$_2$). The electrocatalytic properties of composite membranes such as the cell voltage were in the order of magnitude CL-SPEEKlMoPA40 (wt%) > /TPA30 > /TSiA40. In the optimum cell applications for water electrolysis, the cell voltage of PtlPEM/Pt-Ru MEA with CL-SPEEKlTPA30 membrane was 1.75 V at 80$^{\circ}$C and I A/cm$^2$ and this voltage carried lower than that of 1.81 V of Nafion 117. Consequently, in regards of electrochemical and mechanical characteristics and oxidation durability, the newly developed CL-SPEEKITPA30 composite membrane exhibited a better performance than the others, but CLSPEEKlMoPA40 showed the best electrocatalytic activity (1.71 Vat 80$^{\circ}$C and 1 A/cm$^2$) among the composite membranes.

The Preparation and Physicochemical Characteristics of Covalently Cross-Linked SPEEK/HPA Composite Membranes for Water Electrolysis (수전해용 공유가교 SPEEK/HPA 복합막의 제조 및 물리화학적 특성)

  • Hwang, Yong-Koo;Lee, Kwang-Mun;Woo, Je-Young;Chung, Jang-Hoon;Moon, Sang-Bong;Kang, An-Soo
    • Transactions of the Korean hydrogen and new energy society
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    • v.20 no.2
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    • pp.95-103
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    • 2009
  • In order to improve the electrochemical, mechanical and electrocatalytic characteristics, engineering plastic of polyether ether ketone (PEEK) as polymer matrix was sulfonated (SPEEK) and the organic-inorganic blend composite membranes has been prepared by loading heteropoly acids (HPAs), including tungstophosphoric acid (TPA), molybdophosphoric acid (MoPA), and tungstosilicic acid (TSiA). And then these were covalently cross-linked (CL-SPEEK/HPA) as the electrolyte and MEA of polymer electrolyte membrane electrolysis (PEME). As a result, the optimum reaction conditions of CL-SPEEK/HPA was established and the electrochemical characteristics such as ion conductivity ($\sigma$) were in the order of magnitude: CL-SPEEK /TPA30 (${\sigma}=0.128\;S/cm^{-1}$) < /MoPA40 (${\sigma}=0.14\;S/cm^{-1})$ < /TSiA30 (${\sigma}=0.22\;S/cm^{-1}$) at $80^{\circ}C$, and mechanical characteristics such as tensile strength: CL-SPEEK /TSiA30 $\fallingdotseq$ /MoPA40 < /TPA30. Consequently, in regards of above characterisitics and oxidation durability, the CL-SPEEK/TPA30 exhibited a better performance in PEME than the others, but CL-SPEEK/MoPA40 showed the best electrocatalytic activity of cell voltage 1.71 V among the composite membranes. The dual effect of higher proton conductivity and electrocatalytic activity with the addition of HPAs, causes a synergy effect.

Study of Synthesis and Performance of Covalently Cross-Linked SPEEK/Cs-TSiA Composite Membranes with Ceria Contents for Water Electrolysis (수전해용 공유가교 SPEEK/Cs-TSiA 막의 Ceria의 함량에 따른 제조 및 성능 연구)

  • YOON, DAE-JIN;OH, YUN-SUN;SEO, HYEON;MOON, SANG-BONG;CHUNG, JANG-HOON
    • Transactions of the Korean hydrogen and new energy society
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    • v.26 no.3
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    • pp.212-220
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    • 2015
  • The engineering plastic of sulfonated polyether ether ketone (SPEEK) as a polymer matrix has been developed in this lab to replace Nafion, solid polymer electrolytes of perfluorosulfonic acid membrane which has several flaws such as high cost, and limited operational temperature above $80^{\circ}C$. The SPEEK was prepared in the sulfonation reaction of polyether ether ketone (PEEK). The organic-inorganic blended composite membranes were prepared by sol-gel casting method with loading the highly dispersed ceria and cesium-substituted tungstosilicic acid (Cs-TSiA) with cross-linking agent contents of 0.01 mL. In conclusion, CL-SPEEK/Cs-TSiA/ceria 1% membrane showed the optimum results such as 0.1882 S/cm of proton conductivity at $80^{\circ}C$, and 99.61 MPa of tensile strength which were better than Nafion 117 membrane.

Stabilization of Covalently Cross-Linked SPEEK/Cs-Substituted HPA Composite Membranes for Water Electrolysis ($Cs^+$치환에 따른 수전해용 공유가교 SPEEK/HPA 복합막의 안정화)

  • Jee, Bong-Chul;Ha, Sung-In;Song, Min-Ah;Chung, Jang-Hoon;Moon, Sang-Bong;Kang, An-Soo
    • Transactions of the Korean hydrogen and new energy society
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    • v.22 no.1
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    • pp.1-12
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    • 2011
  • To improve the mechanical properties, such as durabilities and antioxidative characteristics, the covalently cross-linked (CL-) SPEEK (sulfonated polyether ether ketone)/Cs-substituted HPA (heteropoly acid) organic-inorganic composite membranes (CL-SPEEK/Cs-HPAs), have been intensively investigated. The composite membrane were prepared by blending cesium-substituted HPAs (Cs-HPAs), including tungstophosphoric acid (TPA), molybdophosphoric acid (MoPA), and tungstosilicic acid (TSiA) with cross-linking agent content of 0.01 mL. And composite electrolytes composed of Cs-HPAs, prepared by immersion (imm.) and titration (titr.) methods to increase the stability of HPAs in water, were applied to polymer electrolyte membrane electrolysis (PEME). As a result, the proton conductivity of Cs-substituted composite membranes increased rapidly over $60^{\circ}C$ but mechanical properties, such as tensile strength, decreased in accordance with added Cs content. The bleeding-out of Cs-TPA membranes by titration method (50 vol.% Cs) decreased steadily to 2.15%. In the oxidative stability test by Fenton solution, the durability of membranes with Cs-HPA significantly increased. In case of CL-SPEEK/ Cs-TPA membrane, duration time increased more than 1200 hours. It is expected that even though CL-SPEEK/Cs-MoPA membrane shows the high proton conductivity, electrocatalytic activity and cell voltage of 1.80 V for water electrolysis, the CL-SPEEK/Cs-TPA (imm.) is more suitable as an alternative membrane in real system with the satisfactory proton conductivity, mechanical properties, anti-oxidative stability and cell voltage of 1.89 V.