The metal complex catalysis with participation of unsaturated hydrocarbons gains great interest because of ecological aspect and a possibility of re-using of the catalyst. It has a number of advantages in comparison with a heterogeneous catalysis, such as high activity and selectivity, low temperatures of reaction and pressure. A palladium-polyvinylpyrrolidone complex was synthesized and characterized by potentiometry, conductometry, mass-, and IR-spectroscopy. The complex was tested for catalytic activity in reaction of octene-1 oxidation by inorganic oxidizers (KIO4, NaBrO3, Na2S2O8, K2S2O8) in dimethylsulfoxide or dimethylformamide under mild conditions. The reaction product was octanone-2, obtained in good yield (80-98 %) and characterized by gas chromatography and mass spectrometry. The catalysts can be easily recycled five consecutive runs without significant loss of catalytic efficiency. The use of different surface analysis techniques, such as: Scanning Electron Microscopy (SEM) and Energy-Dispersive X-ray spectroscopy (EDX), led to a better understanding of the polymer promoting effect. Copyright © 2018 BCREC Group. All rights reservedReceived: 18th December 2017; Revised: 6th August 2018; Accepted: 9th August 2018How to Cite: Akbayeva, D.N., Bakirova, B.S., Seilkhanova, G.A., Sitzmann, H. (2018). Synthesis, Characterization, and Catalytic Activity of Palladium-polyvinylpyrrolidone Complex in Oxidation of Octene-1. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (3): 560- 572 (doi:10.9767/bcrec.13.3.1980.560-572)Permalink/DOI: https://doi.org/10.9767/bcrec.13.3.1980.560-572
In this article, the biocatalytic oxidation of ethanol into acetaldehyde was studied using a catalase entrapped within a monolithic polyampholyte cryogel, p(APTAC-co-AMPS), as catalyst. When an anionic monomer, 2-acrylamido-2-methyl-1-propanesulfonic acid sodium salt (AMPS), was mixed with a cationic monomer, (3-acrylamidopropyl) trimethylammonium chloride (APTAC), under cryo-polymerization conditions at a molar ratio of monomers [APTAC]:[AMPS] = 75:25 mol.% in the presence of 10 mol.% cross-linking agent, N,N-methylenebisacrylamide (MBAA), the macroporous polyampholyte cryogels containing various amounts of catalase were synthesized in situ. The conversion of ethanol into acetaldehyde in good-to-high yields was observed in flow-through and batch-type reactors under optimal conditions: at T = 10–20 °C, pH = 6.9–7.1, [C2H5OH]:[H2O2] = 50:50 vol.%. According to the SEM images, the pore sizes of the p(AMPS-co-APTAC) cryogel vary from 15 to 55 μm. The catalytic activity of catalase entrapped within a monolithic polyampholyte cryogel in the conversion of ethanol into acetaldehyde was evaluated through the determination of kinetic parameters such as the Michaelis constant (Km), maximum enzymatic rate (Vmax), activation energy (Ea), turnover number (TON) and turnover frequency (TOF). The catalase encapsulated within the monolithic polyampholyte cryogel exhibits a high conversion of ethanol into acetaldehyde. The key parameters of ethanol oxidation in flow and batch reactors in the presence of the cryogel monolith were calculated.
News of the Academy of sciences of the Republic of Kazakhstan 2 NAS RK is pleased to announce that News of NAS RK. Series of chemistry and technologies scientific journal has been accepted for indexing in the Emerging Sources Citation Index, a new edition of Web of Science. Content in this index is under consideration by Clarivate Analytics to be accepted in the Science Citation Index Expanded, the Social Sciences Citation Index, and the Arts & Humanities Citation Index. The quality and depth of content Web of Science offers to researchers, authors, publishers, and institutions sets it apart from other research databases. The inclusion of News of NAS RK. Series of chemistry and technologies in the Emerging Sources Citation Index demonstrates our dedication to providing the most relevant and influential content of chemical sciences to our community. Қазақстан Республикасы Ұлттық ғылым академиясы "ҚР ҰҒА Хабарлары. Химия және технология сериясы" ғылыми журналының Web of Science-тің жаңаланған нұсқасы Emerging Sources Citation Index-те индекстелуге қабылданғанын хабарлайды. Бұл индекстелу барысында Clarivate Analytics компаниясы журналды одан әрі the Science Citation Index Expanded, the Social Sciences Citation Index және the Arts & Humanities Citation Index-ке қабылдау мәселесін қарастыруда. Webof Science зерттеушілер, авторлар, баспашылар мен мекемелерге контент тереңдігі мен сапасын ұсынады. ҚР ҰҒА Хабарлары. Химия және технология сериясы Emerging Sources Citation Index-ке енуі біздің қоғамдастық үшін ең өзекті және беделді химиялық ғылымдар бойынша контентке адалдығымызды білдіреді. НАН РК сообщает, что научный журнал «Известия НАН РК. Серия химии и технологий» был принят для индексирования в Emerging Sources Citation Index, обновленной версии Web of Science. Содержание в этом индексировании находится в стадии рассмотрения компанией Clarivate Analytics для дальнейшего принятия журнала в the Science Citation Index Expanded, the Social Sciences Citation Index и the Arts & Humanities Citation Index. Web of Science предлагает качество и глубину контента для исследователей, авторов, издателей и учреждений. Включение Известия НАН РК в Emerging Sources Citation Index демонстрирует нашу приверженность к наиболее актуальному и влиятельному контенту по химическим наукам для нашего сообщества.
In this work we obtained a polymer-metal complex by mixing aqueous solution of copper(II) acetate with PVA at a certain ratio, pH of the solution and temperature. The composition of the complex compound was determined by potentiometric and conductometric titration. The possibility of a complex formation was proved by calculating thermodynamic characteristics. The stability constant of the polymer-metal complex was calculated on the basis of the modified Bjerrum’s method. The metal-polymer complex was synthesized in the ratio 1:2. IR spectroscopy and scanning electron microscopy (SEM) confirmed the coordination of polymeric PVA ligand to copper and allowed evaluating the morphology and features of the complex surface. The catalytic activity of the synthesized compound was evaluated in the oxidation reaction of elemental phosphorus (P4) by oxygen in aqueous-organic media under mild conditions. Quantitative analysis of phosphoric acid was made by photocolorimetric method. We found that the oxidation process of P4 in the presence of the complex Cu(PVA)2(OAc)2 in aqueous-organic media is characterized with the maximum absorption rate, in comparison with Cu(OAc)2·H2O oxidation process with P4, and yields up to 97% of the products. The process of oxidation of yellow phosphorus by oxygen in the presence of the copper(II)-PVA complex proceeds through key reactions of two-electron reduction of the catalyst P4 with the formation of intermediate phosphorus-containing products P3+ and the stages of catalyst regeneration by oxygen. Twenty-electron oxidation of P4 to the phosphorus-containing P5+ products involves 10 two-electron redox reactions and a number of complexation or hydrolysis stages.
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