Solution combustion synthesis of calcium zirconate, CaZrO3, powders

Single-phase CaZrO₃ powder was prepared by heating at 300 °C an aqueous solution of Ca(NO₃)₂, ZrO(NO₃)₂ and β-C₃H₇NO₂ (molar ratio=3:3:4). TG-DTA analysis indicated that an intense exothermic reaction occurred at 255 °C, which lead to the formation of a voluminous white powder. No additional annealing was required, as pure crystalline CaZrO₃ resulted directly from the combustion reaction. Although no advanced milling was performed, the specific surface area of the powder was 21.5 m²/g. The average crystallite size of CaZrO₃ was 23.9 nm. After sintering in air at 1400 °C for 2 h, the pellets - shaped by uniaxial pressing at 200 MPa - reached 95% of the theoretical density, had no open pores and were slightly translucent.     

Catalyst preparation by combustion synthesis for electrochemical hydrocarbon devices

Metals and ceramics can behave as active electrocatalyst materials, particularly in hydrocarbon oxidation in anodic reaction fuel cells. Combustion synthesis is a very reliable, fruitful and rapid synthesis method to produce metals, ceramics and cermets with low particle size and high specific surface area. This work describes the preparation of nanoparticle Pt/Ru alloys, ceramic perovskites such as Sm_0.95CoO_3–, and Sm_0.95CoO_3–/Pt cermets, and shows how promising these materials can be in the role of electrochemically active materials.Presented at the OSSEP Workshop Ionic and Mixed Conductors: Methods and Processes, Aveiro, Portugal, 10–12 April 2003     

The 4-nitrobenzenesulfonyl group as a convenient N-protecting group for iminosugars—synthesis of oligosaccharide inhibitors of heparanase

The 4-nitrobenzenesulfonyl (nosyl) group can be used advantageously for the protection of the ring nitrogen atom of iminosugars. This group is conveniently introduced, is stable to most of the standard carbohydrate transformations and can be removed under mild conditions. The applicability of the nosyl group is demonstrated by the synthesis of sulfated oligosaccharides which are inhibitors of the enzyme, heparanase. The N-(4-nitrobenzenesulfonyl) group is orthogonal with the azido function.     

Facile electrochemical synthesis of nano iron porous coordination polymer using scrap iron for simultaneous and cost-effective removal of organic and inorganic arsenic

An eco-economic and facile electrochemical method was developed to synthesize iron porous coordination polymers (Fe-PCPs) for the simultaneous removal of inorganic and organic arsenic from natural water.     

Optimization and ecofriendly synthesis of iron oxide nanoparticles as potential antioxidant

The present study involves the use of Box-Behnken design for optimization of the energy-efficient process variables, eco-friendly synthesis of nanoparticles of iron oxide using Coriandrum sativum L. (cilantro) leaf extract. The factors, which significantly influenced mean nanoparticle size, surface charge, and size distribution, were the volume of leaf extract, agitation speed, and temperature. The developed model using Box-Behnken design was validated by synthesizing the iron nanoparticles using optimized operational conditions i.e. 10 ml volume of leaf extract, 1500 rpm agitation speed and 30 °C temperature. This resulted in the formation of highly stable iron oxide nanoparticles with mean particle size 161.5 nm and polydispersity index 0.132 with a zeta potential of −19.5 mV. The free radical inhibitory activity of prepared iron oxide nanoparticles was found comparable to ascorbic acid. These results reveal that iron nanoparticles for a biomedical application can be prepared at ambient temperature in an eco-friendly manner.     

Efficient and practical synthesis of N-acetyl enamides from ketoximes by unique iron catalytic system

A new procedure for the iron-catalyzed synthesis of enamides from ketoximes was developed, and its mechanism was proposed. A unique reduction system, with the concerted use of KI and Na₂S₂O₄, was involved. The reaction exhibited a wide substrate scope and gave good yields in a short reaction time. The procedure is operationally simple and also applicable for the large-scale synthesis.     

Phenol-formaldehyde resin route to the synthesis of several iron group transition metal phosphides

Abstract

A series of iron, cobalt and nickel metal phosphides of chemical formula Fe_xP, Co₂P and Ni₂P with high specific surface areas of 331.1, 294.2 and 228.0 m² g^?1, respectively, was firstly synthesized by phenol-formaldehyde resin route. It was found that the as-prepared Co₂P and Ni₂P samples synthesized using phenol-formaldehyde resin as a carbon source showed much higher BET surface areas than those prepared using other carbon sources reported before, including cinnamic strong alkali anion exchange resin, p-phenylenediamine and hexamethylenetetramine. This phenol-formaldehyde resin route was proved to be as universal as traditional H₂ reduction method.     

燃烧合成法制备纳米氧化锌

采用燃烧合成法制备氧化锌纳米粉体，DTA结果表明用柠檬酸作为燃烧剂比用尿素为燃烧剂时进行燃烧反应放出的热量少，更易制得纳米级氧化物．利用XRD和TEM表征样品，确定了生产纳米氧化锌粉体的最佳条件：硝酸锌与柠檬酸按9：1．5(物质的量比)形成前驱体，600℃进行反应．得到球形粉体粒径为16．4nm。     

Facile solid-state synthesis of oxidation-resistant metal nanoparticles at ambient conditions

A simple and scalable method for the synthesis of metal nanoparticles in the solid-state was developed, which can produce nanoparticles in the absence of solvents. Nanoparticles of coinage metals were synthesized by grinding solid hydrazine and the metal precursors in their acetates and oxides at 25 °C. The silver and gold acetates converted completely within 6 min into Ag and Au nanoparticles, respectively, while complete conversion of the copper acetate to the Cu sub-micrometer particles took about 2 h. Metal oxide precursors were also converted into metal nanoparticles by grinding alone. The resulting particles exhibit distinctive crystalline lattice fringes, indicating the formation of highly crystalline phases. The Cu sub-micrometer particles are better resistant to oxidation and exhibit higher conductivity compared to conventional Cu nanoparticles. This solid-state method was also applied for the synthesis of platinum group metals and intermetallic Cu₃Au, which can be further extended to synthesize other metal nanoparticles.     

金属蒸气合成在金属有机合成中的应用

本文简要地介绍了金属蒸气合成法的基本原理、仪器和实验技术, 并按金属原子分别与炔、单烯、多烯、环烯、芳烃体系、卤代烃、有机混和物的反应及有机金属硼化合物的合成, 对金属蒸气合成法在金属有机合成中的应用进行了讨论。     

The surface properties of iron catalyst for ammonia synthesis

The reduction process and the surface properties of industrial prereduced triply and doubly promoted iron catalyst for ammonia synthesis have been studied using thermogravimetry, thermal desorption of N₂ and X-ray diffraction. The properties of both catalysts have been discussed on the basis of the double layer model of iron catalyst. A concept of facet formation on the active surface of the catalysts has been proposed. This revised version was published online in June 2006 with corrections to the Cover Date.     

模板法合成含中心功能基Schiff型大环化合物的研究

报道了一种利用Ba^2+,Sr^2+作为模板离子直接合成含中心功能基Schiff型大 环化合物的方法。并通过元素分析，IR，^1H NMR及MS确定其新化合物的结构。     

Synthesis and properties of sol-gel submicron silica powders doped with partly oxidized iron particles

Magnetic powders based on metallic iron crystallites encapsulated in submicron-sized spherical silica particles have been obtained and investigated. The metallic iron clusters have been produced by the exploding wire method. The silica shells have been prepared via the modified sol-gel Stöber method and the metallic particles have been entrapped by occlusion during the silica powder formation. The entrapped iron particles are partially oxidized due to the nature of the synthetic methods employed. The obtained hybrid materials have been investigated by electron microscopy, X-ray diffraction, magnetic and ζ-potential techniques. Such materials can be employed in such applications as e.g. magnetically-controlled drug vectors or electromagnetic field-shielding.     

含二茂铁基的硫代碳酰腙和缩氨基硫脲的合成

硫代碳酰腙和氨基硫脲衍生物具有一定的生理活性,可作为某些金属离子的特效试剂,本文报道在乙醇-醋酸介质中通过取代氨基硫脲,硫代碳酰腙与不同的二茂铁衍生物缩合,合成了新的缩氨基硫脲和硫代碳酰腙衍生物.     

Combustion synthesis and luminescent properties of metal yttrium borates M3Y2 (BO3)4:Eu3+ (M = Ba,Sr) for PDPs applications

The polycrystalline powder samples of Eu³⁺ activated; mixed metal yttrium borate phosphors M₃Y₂(BO₃)₄ (M = Ba, Sr) with improved color purity of red emission for plasma display panels (PDPs) were prepared by solution combustion technique. The synthesis is based up on the exothermic reaction between the fuel (Urea) and oxidizer (Ammonium nitrate) .The heat generated in the reaction is utilized for auto combustion of ingredients. The formation of desired product and crystal structure was confirmed by powder XRD technique; while particle morphology was studied using FE-SEM. Samples under 254 and 147 nm excitation showed intense and pure red emission around 613 nm corresponding to the electric dipole ⁵D₀ → ⁷F₂ transition of Eu³⁺, CIE chromaticity coordinates of synthesized phosphors was found to be (x = 0.67, y = 0.32) close to National Television Standard Committee (NTSC) for red color; found suitable to employ in plasma display panels (PDPs) applications.     

Counter-flow liquid injection plasma synthesis of spinel powders

A novel counter-flow liquid injection plasma synthesis (CF-LIPS) reactor has been developed to produce ceramic powders. By using a counter-flow plasma configuration, entrainment of reactant particles into the plasma is improved compared to conventional injection methods. The counter-flow process also creates large recirculation zones which increase the residence time to more than 100 ms as predicted by modeling results [1]. The long residence time ensures complete evaporation and decomposition of precursor particles and complete reactions to the desirable products. Also, the process employs liquid precursors rather than solids, resulting in less contamination of products from unevaporated reactants. Results show that CF LIPS is an excellent method for producing single-phase and spherical spinel powders with a narrow particle size distribution. Particle size increases with increasing precursor concentration based on the synthesis of magnesium aluminate powders. Characterization techniques include X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDXS), X-ray mapping, centrifugal sedimentation particle size distribution analysis, and vibrating sample magnetometer (VSM) measurements. In addition, crystallographic studies are conducted to determine the bond lengths, bond angles, and stoichiometries of the as-produced spinels.     

Flow fine synthesis with heterogeneous catalysts

In the past few decades, organic reactions under flow conditions have attracted increasing attention. Flow reactions have a number of advantages over batch reactions in terms of environmental compatibility, efficiency, and safety. In particular, flow reactions with heterogeneous catalysts that yield desired products without significant levels of by-product formation can enable purification processes to be avoided. This feature can allow flow reactions to be assembled in a multi-step and continuous manner for the synthesis of complex molecules. These new techniques have opened up new approaches to the synthesis of fine chemicals and are expected to play a prominent role in future chemical manufacturing processes. In this context, this review aims to summarize recent developments in continuous-flow reactions with heterogeneous catalysts for synthesis of fine chemicals.     

Oligoribonucleotide synthesis by the use of 1-(2-cyanoethoxy)ethyl (CEE) as a 2′-hydroxy protecting group

A novel method for the synthesis of oligoribonucleotides using 1-(2-cyanoethoxy)ethyl (CEE) as a 2′-hydroxy protecting group has been developed. A CEE group was introduced to the 2′-position of N-acyl-3′,5′-O-silyl-protected ribonucleosides under acidic conditions in good yields. The 2′-O-CEE group was found to be stable in an aqueous or ethanolic ammonia and was quickly removed by treatment with anhydrous tetrabutylammonium fluoride (TBAF). A combination of the use of N-acyl and 2′-O-CEE protecting groups enabled a reliable and complete two-step deprotection, first with NH₃–EtOH, then with TBAF in THF, without cleavage of internucleotidic linkages.     

Magnetic properties of lanthanum orthoferrite fine powders prepared by different chemical routes

Fine powders of lanthanum iron oxide, LaFeO₃, have been prepared by solid state reaction as well as sol-gel synthesis and nebulized spray pyrolysis. Structures, morphologies and magnetic susceptibility measurements of these powders have been examined. The powders prepared by all the three low-temperature routes contain nearly spherical particles with an average diameter of 40 nm. These samples show a lower Neel temperature than the powder prepared by solid state reaction besides showing much lower magnetic susceptibility at low temperatures. Dedicated to Professor C N R Rao on his 70th birthday     

Magnesium tetraorganyl derivatives of group 13 metals as intermediate products in the synthesis of group 13 metal alkyls and aryls

Reactions of organomagnesium halides with group 13 metal halides lead to the formation of R₃M type compounds (R = alkyl, aryl; M = Al, Ga, In) and are considered as the simplest methods of R₃M compound syntheses. These seemingly simple reactions reveal a much more complex chemistry involving mixed magnesium-group 13 metal compounds. To elucidate the reaction course of reactions of organomagnesium halides with group 13 metal halides, we have studied reactions of R₃M with organomagnesium halides. The interaction of Et₃M with R¹MgX led to the formation of following products being mixtures of crystalline ionic complexes with the general composition of [Et_4-nR¹_nM]⁻[XMg (thf)₅]⁺·(thf): [Et_2.2Al(CH=CH₂)_1.8]⁻[BrMg (thf)₅]⁺·(thf) ( 1 ), [Et₃Ga(CH=CH₂)]⁻[BrMg (thf)₅]⁺·(thf) ( 2 ), [Et₄Al]⁻[BrMg (thf)₅]⁺·(thf) ( 3 ), [Et₄Ga]⁻[BrMg (thf)₅]⁺·(thf) ( 4 ), [Et_2.9Al(C₆H₅)_1.1]⁻[BrMg (thf)₅]⁺·(thf) ( 5 ), [Et_2.9Ga(C₆H₅)_1.1]⁻[BrMg (thf)₅]⁺·(thf) ( 6 ), [Et_3.4GaMe_0.6]⁻[IMg (thf)₅]⁺·(thf) ( 7 ) and [Et₄In]⁻[BrMg (thf)₅]⁺·(thf) ( 8 ). A comparison of the production course of group 13 metal trialkyls R₃M with a thermal decomposition of 1–8 products showed that reactions of MX₃ with RMgX (X = Br, I; R = alkyl, aryl) yield initially intermediate ionic compounds, which must then be thermally decomposed to obtain pure R₃M compounds. If group 13 metal bromides and iodides, and alkyl (aryl)magnesium bromides and iodides in thf are used, only intermediate products with the [R₄M]⁻[XMg (thf)₅]⁺·(thf) structure are formed.