- Preparation method of epoxy silane coupling agent
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The invention provides a preparation method of an epoxy silane coupling agent. The preparation method comprises the following steps: (1) synthesizing diallyl ether from chloropropene and allyl alcohol under the action of a catalyst and an alkali; (2) carrying out a hydrosilylation reaction on the diallyl ether and hydrogen-containing chlorosilane under the action of a platinum catalyst to obtain allyloxopropyl chlorosilane; (3) carrying out esterification reaction on the allyloxopropyl chlorosilane and saturated alcohol to obtain allyloxoalkoxy silane; and (4) carrying out epoxidation on the allyloxyalkoxy silane by using an oxidizing agent, so as to obtain gamma-(2, 3-epoxypropoxypropyl)alkoxy silane. The preparation method provided by the invention can be suitable for all gamma-(2, 3-epoxypropoxypropyl) epoxy silane, the used catalyst and raw materials are easy to obtain, the yield is high, and the industrial feasibility is high.
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Paragraph 0078-0079
(2021/05/05)
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- Platinum-Imidazolyl Schiff Base Complexes Immobilized in Periodic Mesoporous Organosilica Frameworks as Catalysts for Hydrosilylation
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An imidazolyl Schiff base-containing periodic mesoporous organosilica (PMO) was synthesized via co-condensation reactions between a newly prepared bis (imidazolyl)imine-bridged bis silane and tetraethyl orthosilicate in the presence of cetyltrimethyl ammonium bromide as a soft template. The resultant as-synthesized PMO was then employed as a solid support for platinum catalysts. This complex was fully characterized via various techniques including FTIR, solid-state13C NMR, and 29Si-NMR spectroscopy, as well as N2 adsorption/desorption analysis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) methods. In addition, the catalyst was proven to efficiently mediate hydrosilylation reactions between olefins and hydrosilanes, and it can be reused for at least five cycles without significant loss of activity.
- Huo, Yingpeng,Hu, Jiwen,Tu, Yuanyuan,Huang, Zhenzhu,Lin, Shudong,Hu, Yangfei,Feng, Chao
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- Platinum(II) complexes bearing bulky Schiff base ligands anchored onto mesoporous SBA-15 supports as efficient catalysts for hydrosilylation
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Reported herein is an easy-to-prepare novel heterogeneous catalyst of platinum complexes bearing binary ligands of bidentate naphthalenolimine and cyclo-1,5-octadiene that are anchored onto mesoporous silica SBA-15. The presence of the binary ligands not only stabilized the platinum, but also enabled the platinum atoms to form nanoclusters with diameters of ca 1?nm, and led to high platinum loading (8.69?wt%). Moreover, the platinum catalyst exhibited high catalytic activity towards hydrosilylation of terminal alkenes and styrene with silanes under mild and solvent-free conditions, with excellent regioselectivity.
- Huo, Yingpeng,Hu, Jiwen,Lin, Shudong,Ju, Xingming,Wei, Yanlong,Huang, Zhenzhu,Hu, Yangfei,Tu, Yuanyuan
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- Highly-active, graphene-supported platinum catalyst for the solventless hydrosilylation of olefins
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Herein we report the development of the first graphene-supported platinum catalyst that has demonstrated exceptional catalytic activity and stability for hydrosilylation reactions of olefins (TOF 4.8 × 106 h-1, TON = 9.4 × 106). The catalyst also exhibited functional group tolerance over a broad range of industrially relevant substrates with minimal metal leaching. In addition, the catalyst system was successfully translated into a packed bed platform for continuous hydrosilylation reactions.
- Kong, Caleb J.,Gilliland, Stanley E.,Clark, Brian R.,Gupton, B. Frank
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supporting information
p. 13343 - 13346
(2018/12/13)
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- Nano-dispersed platinum(0) in organically modified silicate matrices as sustainable catalysts for a regioselective hydrosilylation of alkenes and alkynes
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Nano-dispersed platinum(0) particles stabilized in a range of organically modified silicate (ORMOSIL) matrices are investigated as sustainable catalysts for the hydrosilylation of alkenes and alkynes. In this study, five different siloxane matrices including triethoxysilane (HTEOS), methyltriethoxysilane (MTES), ethyltriethoxysilane (ETES), triethoxyvinylsilane (TEVS) and propyltriethoxysilane (PTES) are investigated, and the distribution of the metal particles in these materials analyzed by transition electron microscopy (TEM). The particles appeared to be generally of a small size, with a diameter of ca. 2-5 nm in each of these catalysts, however the distribution is not equally uniform from one matrix to the other. HTEOS, MTES and ETES that respectively carry a hydrogen, a methyl and an ethyl group on the triethoxysilane moiety, displayed a more uniform distribution, while particles appeared to be more scattered in the remaining matrices. Catalysts with a uniform particles distribution produced higher and consistent yields, while those with poor particles distribution produced lower and almost random yields, suggesting that the uniformity in particle distribution, and by extension the nature of the siloxane matrix, are important for the catalytic properties of these materials. The scope of the reaction was broadened to a range of olefins, with a goal of investigating the tolerability of the reaction toward a number of reactive functional groups, resulting in the preparation of 28 compounds. This catalytic system also enabled the hydrosilylation of a limited number of alkynes under the optimized reaction conditions.
- Duke, Brett J.,Akeroyd, Evan N.,Bhatt, Shreeja V.,Onyeagusi, Chibueze I.,Bhatt, Shreya V.,Adolph, Brandy R.,Fotie, Jean
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p. 11782 - 11795
(2018/07/25)
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- Discovering Partially Charged Single-Atom Pt for Enhanced Anti-Markovnikov Alkene Hydrosilylation
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The hydrosilylation reaction is one of the largest-scale application of homogeneous catalysis and is widely used to enable the commercial manufacture of silicon products. However, considerable issues including disposable platinum consumption, undesired side reactions and unacceptable catalyst residues still remain. Here, we synthesize a heterogeneous partially charged single-atom platinum supported on anatase TiO2 (Pt1δ+/TiO2) catalyst via an electrostatic-induction ion exchange and two-dimensional confinement strategy, which can catalyze hydrosilylation reaction with almost complete conversion and produce exclusive adduct. Density functional theory calculations reveal that unexpected property of Pt1δ+/TiO2 originates from atomic dispersion of active species and unique partially positive charge Ptδ+ electronic structure that conventional nanocatalysts do not possess. The fabrication of single-atom Pt1δ+/TiO2 catalyst accomplishes a reasonable use of Pt through recycling and maximum atom-utilized efficiency, indicating the potential to achieve a green hydrosilylation industry.
- Chen, Yuanjun,Ji, Shufang,Sun, Wenming,Chen, Wenxing,Dong, Juncai,Wen, Junfeng,Zhang, Jian,Li, Zhi,Zheng, Lirong,Chen, Chen,Peng, Qing,Wang, Dingsheng,Li, Yadong
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supporting information
p. 7407 - 7410
(2018/06/11)
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- DEHYDROGENATIVE SILYLATION, HYDROSILYLATION AND CROSSLINKING USING PYRIDINEDIIMINE COBALT CARBOXYLATE CATALYSTS
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A process for producing a silylated product comprises reacting a mixture comprising (a) an unsaturated compound containing at least one unsaturated functional group, (b) a silyl hydride containing at least one silylhydride functional group, and (c) a catalyst, optionally in the presence of a solvent, to produce a dehydrogenative silylated product, a hydrosilylated product, or a combination of a dehydrogenative silylated product and a hydrosilylated product, wherein the catalyst is chosen from a pyridine diimine cobalt dicarboxylate complex or a cobalt carboxylate compound, and the process is conducted without pre-activating the catalyst via a reducing agent and/or without an initiator or promoter compound. The present catalysts have been found to be active in the presence of the silyl hydride employed in the silylation reaction.
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Page/Page column 42; 43
(2017/02/24)
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- Synthesis of a fumed silica-supported poly-3-(2-aminoethylamino)propylsiloxane platinum complex and its catalytic behavior in the hydrosilylation of olefins with triethoxysilane
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A novel fumed silica-supported bidentate nitrogen platinum complex was conveniently prepared from N-(2-aminoethyl)-3-aminopropyltriethoxysilane via immobilization on fumed silica followed by a reaction with hexachloroplatinic acid. The title complex was systematically characterized and analyzed by Fourier Transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and specific surface area analysis (BET). The resulting title complex was found to be efficient and stable in catalyzing the hydrosilylation reaction of olefins with triethoxysilane. Furthermore, the polymeric platinum complex could be separated by simple filtration and reused four times without any appreciable loss of catalytic activity.
- Li, Ji,Zhang, Lei,Li, Tingting,Yang, Chunhui
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p. 728 - 733
(2016/05/09)
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- Bench-Stable, Substrate-Activated Cobalt Carboxylate Pre-Catalysts for Alkene Hydrosilylation with Tertiary Silanes
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High-spin pyridine diimine cobalt(II) bis(carboxylate) complexes have been synthesized and exhibit high activity for the hydrosilylation of a range of commercially relevant alkenes and tertiary silanes. Previously observed dehydrogenative silylation is suppressed with the use of sterically unencumbered ligands, affording exclusive hydrosilylation with up to 4000 TON. The cobalt precatalysts were readily prepared and handled on the benchtop and underwent substrate activation, obviating the need for external reductants. The cobalt catalysts are tolerant of epoxide, amino, carbonyl, and alkyl halide functional groups, broadening the scope of alkene hydrosilylation with earth-abundant metal catalysts.
- Schuster, Christopher H.,Diao, Tianning,Pappas, Iraklis,Chirik, Paul J.
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p. 2632 - 2636
(2016/04/26)
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- Process for manufacturing polysiloxane microcapsules that are functionalized and are not very porous
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A method is provided for encapsulating products that can have lipophilic or hydrophilic, including volatile, properties in a polysiloxane membrane that is particularly impervious. A method is also provided for evaluating the imperviousness of capsules. The present method includes the following steps: a) formation of droplets by an emulsion between an oily phase containing the product to be encapsulated and an acidic aqueous phase heated to around 50° C. and in the presence of surfactants; b) addition and hydrolysis of at least one silane in order to obtain a silanol; c) increasing the pH in order to start condensation of the silanol to form a first membrane around the droplets of the product to be encapsulated; d) lowering the pH; e) increasing the pH, optionally preceded by adding a silane, in order to obtain a new condensation of silanol around the droplets of the product to be encapsulated.
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Page/Page column 4
(2016/09/26)
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- COSMETIC TREATMENT METHOD COMPRISING THE APPLICATION OF A COATING BASED ON AN AEROGEL COMPOSITION OF LOW BULK DENSITY
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The present invention relates to a cosmetic treatment method comprising the formation of a coating on keratin fibres characterized in that it comprises: 1) the preparation of an aerogel precursor composition comprising:—at least one organic solvent chosen from acetone, C1-C4 alcohols, C1-C6 alkanes, C1-C4 ethers, which may or may not be perfluorinated, and mixtures thereof and at least one precursor compound that contains:—at least one atom chosen from silicon, titanium, aluminium and zirconium,—at least one hydroxyl or alkoxy function directly attached to the atom chosen from silicon, titanium, aluminium and zirconium by an oxygen atom, and,—optionally an organic group directly attached to the atom chosen from silicon, titanium, aluminium and zirconium by a carbon atom, 2) the removal of the solvent or solvents resulting in the formation of an aerogel composition having a bulk density less than or equal to 0.35 g/cm3, 3) the application to the keratin fibres of the aerogel composition resulting from step 2) or of the aerogel precursor composition resulting from step 1). Advantageously, the molar ratio between the precursor compounds and the solvent is at most 1/20.
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Paragraph 0069
(2014/02/15)
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- FILM FORMING PERSONAL CARE COMPOSITIONS AND METHODS
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Compositions, kits and methods of preparing a biocompatible film for cosmetic or medical uses are disclosed. The compositions or kits contain polyvinyl acetal (PVA), siloxane and a solvent. The siloxane can have a hydrophilic group. Once the solvent content is reduced, for instance, by evaporation, the mixture of PVA and siloxane is solidified, forming a film. The compositions and kits, optionally, further include one or more of an antimicrobial agent, a pigment, an anti-inflammatory agent, an anesthetic agent or a hemostatic agent. Such a film can be used, for example, in the form of an antimicrobial sealant, a liquid bandage, body paints, scar camouflage, water-proof sun block, makeup sealer, or antimicrobial wipe or spray.
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- MCM-41-immobilised bidentate nitrogen platinum complex: A highly efficient and recyclable phosphine-free catalytic system for the hydrosilylation of olefins
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An MCM-41-immobilised bidentate nitrogen platinum complex (MCM-41-2N-Pt) was very conveniently synthesised from commercially available and cheap 3-(2-aminoethylamino)propyltrimethoxysilane by immobilisation on the mesoporous silica nanoparticles, MCM-41, followed by reaction with potassium chloroplatinite. It was found that the MCM-41-2N-Pt complex is a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane and can be easily recovered and reused several times without significant loss of activity.
- Zhang, Hean,Liu, Jiaqin,Cheng, Shaojuan,Cai, Mingzhong
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experimental part
p. 241 - 243
(2012/09/08)
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- A novel fumed silica-supported nitrogenous platinum complex as a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane
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A novel fumed silica-supported nitrogenous platinum complex was conveniently prepared from cheap γ-aminopropyltriethoxysilane via immobilization on fumed silica in toluene, followed by a reaction with hexachloroplatinic acid. The title complex was characterized by fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). It was found that the complex is an efficient and stable catalyst for the hydrosilylation of olefins with triethoxysilane. The title platinum complex could be separated by simple filtration and reused several times without any appreciable loss in the catalytic activity. Crown Copyright
- Li, Ji,Yang, Chunhui,Zhang, Lei,Ma, Tianlong
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experimental part
p. 1845 - 1849
(2011/06/19)
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- MCM-41-supported bidentate phosphine rhodium complex: An efficient and recyclable heterogeneous catalyst for the hydrosilylation of olefins
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MCM-41-supported bidentate phosphine rhodium complex (MCM-41-2P-RhCl 3) was conveniently synthesized from commercially available and cheapγ-aminopropyltriethoxysilane via immobilization on MCM-41, followed by reacting with diphenylphosphinomethanol and rhodium chloride. It was found that the title complex is a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane and can be recovered and recycled by a simple filtration of the reaction solution and used for at least 10 consecutive trials without any decreases in activity.
- Hu, Ronghua,Hao, Wenyan,Cai, Mingzhong
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experimental part
p. 1629 - 1634
(2012/01/13)
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- New Heterogenized Rhodium Complexes, Methods of their Synthesis and Application as Hydrosilylation Catalysts
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The subjects of the invention are new heterogenized rhodium complexes, the methods of their synthesis and their application as catalysts for synthesis of organosilicon compounds by hydrosilylation. The subject of the invention are new siloxide rhodium(I) complexes immobilised on the silica surface, of the general formula 1. [(≡SiO)(L)Rh(diene)] The second subject of the invention is the method of synthesis of the new rhodium complexes of the general formula 1. The third subject of the invention is the method of obtaining the organosilicon compounds in the reaction of hydrosilylation between the selected alkenes or functionalised alkenes containing the terminal C═C bond and the appropriate compounds containing the Si═H bond selected from silanes, (poly)siloxanes and (poly)carbosiloxanes, in the presence of heterogenized rhodium catalysts, of the general formula 1.
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Page/Page column 4-5
(2010/03/31)
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- A diphosphino-functionalised MCM-41-anchored platinum complex: An efficient and reusable catalyst for the hydrosilylation of olefins
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A diphosphino-functionalised MCM-41 anchored platinum complex (MCM-41-2P-Pt) was conveniently synthesised from commercially available and cheap γ-aminopropyltriethoxysilane via immobilisation on MCM-41, followed by reactiopn with diphenylphosphinomethanol and potassium chloroplatinite. It was found that the title complex is a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane and can be recovered and recycled by a simple filtration of the reaction solution and used for at least 10 consecutive reactionss without any decrease in activity.
- Zha, Lingfang,Hao, Wenyan,Cai, Mingzhong
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experimental part
p. 648 - 652
(2011/03/18)
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- MCM-41-supported mercapto platinum complex as a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane
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A novel MCM-41-supported mercapto platinum complex was conveniently synthesized from commercially available and cheap γ-mercaptopropyltriethoxysilane via immobilization on MCM-41, followed by reacting with potassium chloroplatinite. The powder X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were employed to characterize the title platinum complex. It was found that the title complex is an efficient catalyst for hydrosilylation of olefins with triethoxysilane and can be reused several times without noticeable loss of activity.
- Hu, Ronghua,Zha, Lingfang,Cai, Mingzhong
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scheme or table
p. 563 - 566
(2010/08/05)
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- Hydrosilylation of olefins over rhodium complex anchored over thioether-functionalized MCM-41
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The hydrosilylation of alkenes with triethoxysilane has been achieved at 120 °C in the presence of 0.01. mol% of thioether-functionalized MCM-41 anchored rhodium complex, affording the corresponding addition products in 68-91% yields. This supported rhodium complex can be reused several times without noticeable loss of activity. Our system not only solves the basic problems of catalyst separation and recovery, but also avoids the use of phosphine ligands.
- Zha, Lig Fang,Yang, Wei Sen,Hao, Wen Yan,Cai, Ming Zhong
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experimental part
p. 1310 - 1313
(2011/10/09)
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- Hydrosilylation of allyl glycidyl ether with triethoxysilane
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Hydrosilylation of allyl glycidyl ether with triethoxysilane in presence of Speier's catalyst leads to triethoxy(3-glycidoxypropyl)silane and triethoxy(2-glycidoxy-1-methylethyl)silane and is accompanied by isomerization of allyl glycidyl ether and cleavage of the oxirane ring and the ether bond. An effect of admixtures in allyl glycidyl ether on the process is revealed. Some other hydrosilylation catalysts and additives to Speier's catalyst are studied.
- Chernyshev,Belyakova,Knyazeva,Khromykh
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- Synthesis, first structures, and catalytic activity of the monomeric rhodium(I)-siloxide phosphine complexes
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Four new square-plane rhodium siloxide complexes of the general formula [Rh(cod)(PR3′)(OSiR3)] (where R = Me, i-Pr, O-t-Bu, R′ = Cy, Ph) were synthesized and the structures of three of them were resolved by the X-ray method. [Rh(cod)(PCy3)(OSiMe3)] (1) appeared to be a very efficient catalyst for hydrosilylation of allyl glycidyl ether to yield, selectively, 3-glycidoxypropyltriethoxysilane, a commercially important silane coupling agent. Catalytic measurements and stoichiometric experiments of 1 with triethoxysilane suggest a mechanism where an unsaturated Rh-H species is responsible for the catalysis.
- Marciniec, Bogdan,Blazejewska-Chadyniak, Paulina,Kubicki, Maciej
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p. 1292 - 1298
(2007/10/03)
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