• Title/Summary/Keyword: Palladium

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Addition Polymerization of 5-Norbornene-2-carboxylic Acid Esters Using Palladium Catalyst System: Synthesis of Monomers, Effect of Their Stereochemistry on Polymerization Behavior (Palladium 촉매를 이용한 5-Norbornene-2-carboxylic Acid Esters의 부가 중합: 단량체의 합성, 단량체의 Stereochemistry(Endo-, Exo-이성질체)가 고분자의 중합 거동에 미치는 영향)

  • Chung, Hae-Kang;Shim, Hyoug-Sub;Jeon, Seung-Ho;Kim, Ji-Heung;Nam, Sung Woo;Jeon, Boong Soo;Kim, Young Jun
    • Polymer(Korea)
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    • v.39 no.3
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    • pp.487-492
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    • 2015
  • The effects of chemical structure of alkyl groups of norbornene carboxylic alkyl esters(methyl, octyl, 4-chlorobenzyl) and endo/exo ratios of norbornene monomers on activity of palladium catalyst and polymerization behavior were investigated. Norbornene ester monomers were synthesized from the reaction of 5-norborene-2-carboxylic acid and various alcohols. Polymerization catalyst, di-${\mu}$-chloro-bis(-methoxybicyclo[2,2,1]-hept-2-ene)palladium(II) (DCBMP), was synthesized according to the literature procedure and silver hexafluoroantimonate ($AgSbF_6$) was used as a conjugate anion source. Gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) were the principal techniques for polymer characterization and $^1H$ NMR spectroscopy was used for chemical structures determination of monomers and polymers. For all of the norbonene alkyl esters GPC data showed that when the amounts of endo isomers exceeded those of exo isomers decreased molecular weight polymers were obtained probably due to the decreased catalyst activity. Polymerizations were conducted by varying the monomer/catalyst mole ratios (100:1, 200:1, 300:1). When 300:1 monomer/catalyst ratio was employed it was possible to synthesize high molecular weight ($M_n=27500g/mol$), film forming polymer from exo-norbornene carboxylic acid octyl ester.

Solvent Extraction of Platinum Group Metals from the leach Liquor of Spent Automotive Catalyst (자동차(自動車) 폐촉매(廢觸媒)의 침출액(浸出液)으로부터 백금족(白金族) 금속(金屬)의 용매추출(溶媒抽出))

  • Kim, Mi-Ae;Lee, Jae-Chun;Kim, Chi-Kwon;Kim, Min-Seuk;Kim, Byung-Su;Yoo, Kyoung-Keun
    • Resources Recycling
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    • v.15 no.5 s.73
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    • pp.3-10
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    • 2006
  • The solvent extraction for the separation of platinum group metals from the leach liquor of spent automotive catalysts has been studied. Tri-n-butyl phosphate (TBP), tri-n-octylamine (TOA) and di-n-hexyl sulfide (DHS) were used as extractants and kerosene as a diluent. The extraction behavior of platinum, palladium and rhodium has been investigated as functions of different kinds of extractants and their concentrations. In addition, the extraction behavior of the major metal impurities such as cerium, lead, iron, magnesium and aluminum has been investigated. Platinum and palladium were extracted with TBP. And platinum, palladium and rhodium were extracted with TOA. Platinum was co-extracted with palladium into the organic phase by solvent extraction using SFI-6 of DHS extractant, but only palladium was selectively extracted with SFI-6R. The selective extraction of palladium with SFI-6R was found better than that with SFI-6, but the kinetics of extraction with SFI-6R was found poor in comparison to SFI-6. The metal impurities extracted simultaneously during the extraction of platinum group metals should be removed in scrubbing and stripping processes. A suitable process has been proposed for the separation of platinum group metals from the leach liquor of spent automotive catalysts. Initially palladium was extracted with SFI-6R, followed by the separation of platinum with TBP or TOA leaving rhodium in the raffinate.

Highly Sensitive MEMS-Type Micro Sensor for Hydrogen Gas Detection by Modifying the Surface Morphology of Pd Catalytic Metal (Pd 촉매금속의 표면형상 변형에 의한 고감도 MEMS 형 마이크로 수소가스 센서 제조공정)

  • Kim, Jung-Sik;Kim, Bum-Joon
    • Korean Journal of Materials Research
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    • v.24 no.10
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    • pp.532-537
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    • 2014
  • In this study, highly sensitive hydrogen micro gas sensors of the multi-layer and micro-heater type were designed and fabricated using the micro electro mechanical system (MEMS) process and palladium catalytic metal. The dimensions of the fabricated hydrogen gas sensor were about $5mm{\times}4mm$ and the sensing layer of palladium metal was deposited in the middle of the device. The sensing palladium films were modified to be nano-honeycomb and nano-hemisphere structures using an anodic aluminum oxide (AAO) template and nano-sized polystyrene beads, respectively. The sensitivities (Rs), which are the ratio of the relative resistance were significantly improved and reached levels of 0.783% and 1.045 % with 2,000 ppm H2 at $70^{\circ}C$ for nano-honeycomb and nano-hemisphere structured Pd films, respectively, on the other hand, the sensitivity was 0.638% for the plain Pd thin film. The improvement of sensitivities for the nano-honeycomb and nano-hemisphere structured Pd films with respect to the plain Pd-thin film was thought to be due to the nanoporous surface topographies of AAO and nano-sized polystyrene beads.

Performance Enhancement by Adaptation of Long Term Chronoamperometry in Direct Formic Acid Fuel Cell using Palladium Anode Catalyst

  • Kwon, Yong-Chai;Baik, S.M.;Han, Jong-Hee;Kim, Jin-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2539-2545
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    • 2012
  • In the present study, we suggest a new way to reactivate performance of direct formic acid fuel cell (DFAFC) and explain its mechanism by employing electrochemical analyses like chronoamperometry (CA) and cyclic voltammogram (CV). For the evaluation of DFAFC performance, palladium (Pd) and platinum (Pt) are used as anode and cathode catalysts, respectively, and are applied to a Nafion membrane by catalyst-coated membrane spraying. After long DFAFC operation performed at 0.2 and 0.4 V and then CV test, DFAFC performance is better than its initial performance. It is attributed to dissolution of anode Pd into $Pd^{2+}$. By characterizations like TEM, Z-potential, CV and electrochemical impedance spectroscopy, it is evaluated that such dissolved $Pd^{2+}$ ions lead to (1) increase in the electrochemically active surface by reduction in Pd particle size and its improved redistribution and (2) increment in the total oxidation charge by fast reaction rate of the Pd dissolution reaction.

Development of Hexafluoropropylene Hydrogenation with Pd/C Particles Prepared with 1-Hexyl-3-methylimidazolium Tetrafluoroborate (1-Hexyl-3-methylimidazolium Tetrafluoroborate으로 제조된 팔라듐 탄소촉매를 이용한 Hexafluoropropylene 수소화 반응)

  • Jeong, Ji Baek;Yoo, Kye Sang
    • Applied Chemistry for Engineering
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    • v.24 no.4
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    • pp.412-415
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    • 2013
  • Palladium on carbon powder was prepared using 1-hexyl-3-methylimidazolium tetrafluoroborate, one of room temperature ionic liquids. The synthesized particles were tested as a hexafluoropropylene hydrogenation catalyst. Moreover, the hydrogenation was performed under various reaction conditions to develop an optimum reaction process. The catalyst prepared by more than 3 wt% of palladium and the unity mole ratio of ionic liquid to palladium precursor showed higher catalytic activity. For reaction conditions, the complete hexafluoropropylene (HFP) conversion was achieved at these conditions; the volume flow ratio of hydrogen to HFP was higher than 1.25 and $GHSV_{HFP}$ was lower than 50000 mL/g-h.

Fabrication of Highly Conductive Yarn using Electroless Nickel Plating (무전해 니켈 도금법을 이용한 고성능 도전사의 제조)

  • Hong, So-Ya;Lee, Chang-Hwan;Kim, Joo-Yong
    • Textile Coloration and Finishing
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    • v.22 no.1
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    • pp.77-82
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    • 2010
  • Highly conductive yarn was successfully obtained using electroless nickel plating method with palladium activation. In the presence of palladium seed on surface of fibers as a catalyst, continuos nickel layer produced on surface of fibers by reducing $Ni${2+}$ ion in the electroless plating bath to $Ni^0$. It was found that the Pd-activation using $SnCl_2$ and $PdCl_2$ to deposit palladium seeds on the surface of fibers plays a key role in the subsequent electroless plating of nickel. It also found that electroless nickel plating on the fibers can induce the nickel-plated $ELEX^{(R)}$ fibers to improve the electrical conductivity of the fibers. The thickness of nickel coating layer on the Pd-activated $ELEX^{(R)}$ fibers and specific conductivity of the fiber were increased through electroless plating time. The temperature of nickel plating bath was very effective to enhance the nickel deposition rate.

Synthesis of Palladium Nanocubes/Nanorods and Their Catalytic Activity for Heck Reaction of Iodobenzene

  • Ding, Hao;Dong, Jiling
    • Applied Microscopy
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    • v.46 no.2
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    • pp.105-109
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    • 2016
  • Palladium has been used as a catalyst not only in Suzuki and Heck cross coupling reaction in organic chemistry, but also in automobile industry for the reduction of vehicle exhausts. The catalytic activity of Pd nanoparticles depends strongly on their size and exposed crystalline facets. In this study, the single crystalline palladium nanocubes/nanorods were prepared in the presence of polyvinyl pyrrolidone (PVP) and potassium bromide (KBr) using the polyol method. Selected area diffraction pattern and high-resolution transmission electron microscopy (TEM) were performed by TEM. The result shows that the ratio of KBr/PVP is the key factor to determine whether the product is cubes or rods. The as-prepared Pd nanocubes were highly uniform in both size and shape. The ordered packing structures including monolayer and multilayer can be fabricated via the rate-controlled evaporation of solution solvent. The catalytic activity of these Pd nanocubes towards heck reaction of iodobenzene with acrylate or acrylic acid was found to be higher than that of Pd nanorods. We suspect it is caused by the difference of energy state while Pd nanocubes is {100} plane and nanorods is {111} plane.

Palladium-Catalyzed Carbonylative Coupling of Aryl Iodide and Diethylmalonate (팔라듐 촉매를 이용한 요오드화 방향족 화합물과 Diethylmalonate 와의 CO 첨가 커플링반응)

  • Jin Il Kim;Kwang Hyek Lee;Tae Soon Yoon
    • Journal of the Korean Chemical Society
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    • v.33 no.5
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    • pp.530-537
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    • 1989
  • Diethylbenzoylmalonates with various substituents were synthesized in moderately good yields through palladium-catalyzed carbonylative coupling of aryl iodide and diethylmalonate with carbon monoxide. Palladium-catalyzed carbonylative coupling reaction usually proceeded well in polar aprotic solvents in the presence of three equivalents of inorganic bases and palladium(II) catalyst. When the reaction was carried out under 10 atm pressure of carbon monoxide, the yield of diethylbenzoylmalonate derivatives was much better than that of reaction under atomspheric pressure of carbon monoxide.

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