Liquid phase reduction method

Among various methods to synthesize nanometer-sized particles [1-3], the liquid-phase reduction method as the novel synthesis method of metallic nanoparticles is one of the easiest procedures, since nanoparticles can be directly obtained from various precursor compounds soluble in a solvent [4], It has been reported that the synthesis of Ni nanoparticles with a diameter from 5 to lOnm and an amorphous-like structure by using this method and the promotion effect of Zn addition to Ni nanoparticles on the catalytic activity for 1-octene hydrogenation [4]. However, unsupported particles were found rather unstable because of its high surface activity to cause tremendous aggregation [5]. In order to solve this problem, their selective deposition onto support particles, such as metal oxides, has been investigated, and also their catalytic activities have been studied. 

The liquid-phase reduction method was applied to the preparation of the supported catalyst [27]. Virtually, Muramatsu et al. reported the controlled formation of ultrafine Ni particles on hematite particles with different shapes. The Ni particles were selectively deposited on these hematite particles by the liquid-phase reduction with NaBFl4. For the concrete manner, see the following process. Nickel acetylacetonate (Ni(AA)2) and zinc acetylacetonate (Zn(AA)2) were codissolved in 40 ml of 2-propanol with a Zn/Ni ratio of 0-1.0, where the concentration of Ni was 5.0 X lO mol/dm. 0.125 g of Ti02... 

Highly dispersed Rh nanoparticles were successfully loaded on GaN ZnO without aggregation by adsorbing Rh nanoparticles that were stabilized by 3-mercapto-1-propanesulfuric acid (prepared by a liquid-phase reduction method) onto GaN ... 

Liquid phase reduction method. Liquid-reduction method uses hydrazine hydrate as reductant. Hydrazine hydrate is a kind of alkaline, corrosion and poisonous hquid which is miscible with water and has the good stability. It is mainly used in medicine and vesicant and reductant and antioxidant because of its strong reductivity. RUCI3 can be reduced completely by hydrazine hydrate in thermodynamics. 

In the past years, chemiluminescence (CL) analysis of inorganic compounds has been extensively developed in both gas and liquid phases. These methods typically rely on the oxidation or reduction of a chemically reactive agent and the subsequent emission of a photon from an electronically excited-state intermediate. 

Liquid-phase chemical reduction is suitable for the formation of metal and metal oxide NPs on nanocarbons. Careful consideration is required in designing the nanocarbon-precursor interaction and choosing the reduction/oxidation method. The synthetic process is often quite time consuming and a number of filtering/washing steps are often required. As discussed, the concurrent liquid phase reduction of GO and precursor is a simple, efficient way to produce a hybrid but the lack of control of GO reduction may affect further applications. 

In a method proposed by Booth et al. (141) for the determination of phylloquinone in various food types, extracted samples are subjected to silica solid-phase extraction followed, in the case of meat or milk samples, by further purification using reversed-phase solid-phase extraction or liquid-phase reduction extraction, respectively. The final test solution is analyzed by NARP-HPLC, and the fluorescent hydroquinone reduction products of phylloquinone and the internal standard are produced online using a postcolumn chemical reactor packed with zinc metal. 2, 3 -Dihydrophylloquinone, a synthetic analog of phylloquinone, is a suitable internal standard for the analysis of vegetable juice, whole milk, and spinach. Another synthetic analog, Ku23), is used for the analysis of bread and beef, because a contaminant in the test solution coelutes with dihydro-phylloquinone. 

Precipitation or coprecipitation methods are also often used. Suh et al. [40] analyzed the effect of the oxygen surface functionalities of carbon supports on the properties of Pd/C catalysts prepared by the alkali-assisted precipitation of palladium chloride on carbon supports, followed by liquid-phase reduction of the hydrolyzed salt with a saturated solution of formaldehyde. They observed that the metal dispersion increased with increasing amount of oxygen surface groups. Nitta et al. [41] also used a deposition-precipitation method, with sodium carbonate and cobalt chloride or nitrate, to prepare carbon-supported Co catalysts for the selective hydrogenation of acrolein. 

Recently, Soria et al. [109] also investigated the effect of synthesis method on the WGS activity of Au/Fc203 catalysts. They prepared catalysts by deposition-precipitation method, liquid phase reductive depositions and double impregnation method. Among the various catalysts, the catalyst synthesized by deposition-precipitation method exhibits higher CO conversion. 

Liquid-phase reductive deposition as a novel nanoparticle synthesis method and its application to supported noble metal catalyst preparation, Y. Sunagawa, K. Yamamoto, H. Takahashi, and A. Muramatsu, Catal Today, 2008,132, 81. 

Unfortunately, many commonly used methods for parameter estimation give only estimates for the parameters and no measures of their uncertainty. This is usually accomplished by calculation of the dependent variable at each experimental point, summation of the squared differences between the calculated and measured values, and adjustment of parameters to minimize this sum. Such methods routinely ignore errors in the measured independent variables. For example, in vapor-liquid equilibrium data reduction, errors in the liquid-phase mole fraction and temperature measurements are often assumed to be absent. The total pressure is calculated as a function of the estimated parameters, the measured temperature, and the measured liquid-phase mole fraction. 

Note that filter aid selection must be based on planned laboratory tests. Guidelines for selection may only be applied in the broadest sense, since there is almost an infinite number of combinations of filter media, filter aids, and suspensions that will produce varying degrees of separation. The hydrodynamics of any filtration process are highly complex filtration is essentially a multiphase system in which interaction takes place between solids from the suspension, filter aid, and filter medium, and a liquid phase. Experiments are mandatory in most operations not only in proper filter aid selection but in defining the method of application. Some general guidelines can be applied to such studies the filter aid must have the minimum hydraulic resistance and provide the desired rate of separation an insufficient amount of filter aid leads to a reduction in filtrate quality — excess amounts result in losses is filtration rate and it is necessary to account for the method of application and characteristics of filter aids. 

The main advantage of the salt reduction method in the liquid phase is that it is reproducible and allows colloidal nanoparticles with narrow size distribution to be prepared. 

Gomez-Sainero et al. (11) reported X-ray photoelectron spectroscopy results on their Pd/C catalysts prepared by an incipient wetness method. XPS showed that Pd° (metallic) and Pdn+ (electron-deficient) species are present on the catalyst surface and the properties depend on the reduction temperature and nature of the palladium precursor. With this understanding of the dual sites nature of Pd, it is believed that organic species S and A are chemisorbed on to Pdn+ (SI) and H2 is chemisorbed dissociatively on to Pd°(S2) in a noncompetitive manner. In the catalytic cycle, quasi-equilibrium ( ) was assumed for adsorption of reactants, SM and hydrogen in liquid phase and the product A (12). Applying Horiuti s concept of rate determining step (13,14), the surface reaction between the adsorbed SM on site SI and adsorbed hydrogen on S2 is the key step in the rate equation. 

The second processing step consisted of salt decomposition with the subsequent reduction to pure metal. The method of chemical deposition of metal salts from the water salt solution with the subsequent reduction to pure metal by liquid phase reducer has been applied to prepare graphite-tin CMs. In this case tin chloride was used for impregnation and potassium tetrahydroborate was used as liquid phase reducer. 

In a closely related study, Tung and Sun discussed the microwave-assisted liquid-phase synthesis of chiral quinoxalines [80], Various L-a-amino acid methyl ester hydrochlorides were coupled to MeOPEG-bound ortho-fluoronitrobenzene by the aforementioned ipso-fluoro displacement method. Reduction under microwave irradiation resulted in spontaneous synchronous intramolecular cyclization to the corresponding l,2,3,4-tetrahydroquinoxalin-2-ones (Scheme 7.71). Retention of the chiral moiety could not be monitored during the reaction, but after release of the desired products it was found that about 10% of the product had undergone racemization. 

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