Room temperature synthesis of glycerol carbonate catalyzed by N-heterocyclic carbenes

N-Heterocyclic carbenes were used as efficient organocatalysts for the synthesis of glycerol carbonate from glycerol and dimethyl carbonate. The reaction takes place in a liquid mixture of reactants without solvent at room temperature. It provides glycerol carbonate in high yield using 2.6–4 mol % of catalyst in a reaction period of 20–30 min.     

Room temperature solution synthesis of alkyl-capped tetrahedral shaped silicon nanocrystals

We report the room temperature solution synthesis of alkyl protected silicon nanocrystals. The nanocrystals are of unusually uniform tetrahedral morphology and of a limited size distribution. The nanocrystals were characterized by transmission and scanning electron microscopy as well as atomic force microscopy.     

The efficient synthesis of carbodiimides using a titanium imido complex

An efficient rt synthesis of carbodiimides or ureas from the combination of a titanium imido complex 2 and a range of 12 aryl and aliphatic isocyanates is described. Control experiments suggest that carbodimide formation is via heterocumulene metathesis through a transient intermediate η²-ureato-N,O metallacycle 8.     

Room temperature solution synthesis of monodispersed single-crystalline ZnO nanorods and derived hierarchical nanostructures

In this work, we report a room temperature wet-chemical approach to synthesize highly regulated, monodispersed ZnO nanorods and derived hierarchical nanostructures. In particular, ZnO has been prepared into single-crystalline conical or prismatic nanorods, and various hierarchical structures such as hexagonally branched, reversed umbrella-type, and cactus-like ZnO nanostructures comprising individual c-oriented nanorods. Depending on the synthetic conditions used, the diameter of nanorods can be controlled with a size down to 10-30 nm, while the aspect ratio can be controlled up to 50-100. Various preparative parameters, such as initial reactant concentrations, solvents, ligands, surfactants, precursor salts, and reaction time, have been systematically examined. Due to slow reactions at room temperature, excellent crystallinity and high morphological yield (100% in most cases) have been achieved via tuning the synthetic parameters. Our photoluminescence and UV measurements also confirm the attained crystal perfection and size uniformity.     

Room temperature synthesis of HgTe nanocrystals

We report a new method to synthesize monodisperse zinc blende HgTe nanocrystals at room temperature in noncoordinating solvent-octadecene. Thiol was needed to control the reaction at a suitable nucleation and growth speed. In the early stage of the reaction, HgTe nanocrystals formed aggregates, and then the aggregates were dispersed and individual dot-shaped nanocrystals were formed with stronger photoluminescence emitting. UV-vis, photoluminescence, and TEM have been used to study the properties of as-prepared HgTe nanocrystals.     

Room temperature, high-yield synthesis of multiple shapes of gold nanoparticles in aqueous solution

A seed-mediated growth method was used to control the morphology and dimensions of Au nanocrystals by the manipulation of the experimental parameters in aqueous solution at room temperature. This chemical route produces various structural architectures with rod-, rectangle-, hexagon-, cube-, triangle-, and starlike profiles and branched (such as bi-, tri-, tetra-, and multipod) Au nanocrystals of various dimensions in high yield in the presence of a single surfactant, cetyltrimethylammonium bromide.     

Synthesis of uniform layered protonated titanate hierarchical spheres and their transformation to anatase TiO2 for lithium-ion batteries

Layered protonated titanates (LPTs), a class of interesting inorganic layered materials, have been widely studied because of their many unique properties and their use as precursors to many important TiO(2)-based functional materials. In this work, we have developed a facile solvothermal method to synthesize hierarchical spheres (HSs) assembled from ultrathin LPT nanosheets. These LPT hierarchical spheres possess a porous structure with a large specific surface area and high stability. Importantly, the size and morphology of the LPT hierarchical spheres are easily tunable by varying the synthesis conditions. These LPT HSs can be easily converted to anatase TiO(2) HSs without significant structural alteration. Depending on the calcination atmosphere of air or N(2), pure anatase TiO(2) HSs or carbon-supported TiO(2) HSs, respectively, can be obtained. Remarkably, both types of TiO(2) HSs manifest excellent cyclability and rate capability when evaluated as anode materials for high-power lithium-ion batteries.     

Enzymatic synthesis of layered titanium phosphates at low temperature and neutral pH by cell-surface display of silicatein-alpha

We introduce a novel method of inorganic synthesis using the catalytic and structure-directing properties of the demosponge enzyme silicatein-alpha. Recombinant silicatein-alpha was displayed at the surface of Escherichia coli cells by fusion to outer membrane protein A and used to biocatalytically direct the formation of layered and amorphous titanium phosphates from a small water-soluble precursor at near-neutral pH at 16 degrees C. Synthesis of titanium phosphates, with potential applications in catalysis and separation technology, previously has required prolonged reactions with phosphoric acid at elevated temperatures. Additionally, we use library screening to isolate a 15-mer with affinity toward the silicatein active site (Kd ca. 50 nM) and introduce this new approach to demonstrate the success of our display strategy. Considering our previous findings with native silicatein filaments, we suggest that this scalable, efficient, cell-based system may have a broad utility for the synthesis of a range of structured metallophosphates and other inorganic materials.     

Room temperature synthesis of upconversion fluorescent nanocrystals

Synthesis of nanocrystals that exhibit strong upconversion (UC) luminescence upon infrared excitation has been challenging due to the stringent control needed over experimental variables. Herein, we report a method to synthesize nanocrystals demonstrating high UC at room temperature in aqueous solution on graphene.     

Room temperature synthesis of surface-functionalised boron nanoparticles

Capped boron nanoparticles have been synthesized at room temperature by a simple route that does not involve the use of flammable boranes.     

Room temperature synthesis of hollow CdMoO(4) microspheres by a surfactant-free aqueous solution route

Hollow cadmium molybdate microspheres have been successfully prepared via a template-free aqueous solution method with the assistance of NaCl at room temperature. The structure and morphology of the CdMoO(4) hollow microspheres were characterized by X-ray diffraction, field-emission scanning electron microscopy, and transmission electron microscopy. The microspheres have diameters of 3-6 microm and hollow interiors of 2-3 microm. The shell is composed of numerous single-crystalline nanorods with diameters of 30-120 nm and lengths of 1-2 microm which are radially oriented to the center. A certain concentration of NaCl plays a key important role in the formation process of hollow microspheres, which might provide a suitable chemical environment to favor the formation of hollow CdMoO(4) microspheres. A possible NaCl-induced Ostwald ripening process is proposed for the formation of hollow CdMoO(4) microspheres on the basis of scanning electron microscopy observation of intermediate products at different precipitation stages.     

Room temperature luminescence of a retinal complex of cyclodextrin

Retinal, which is normally insoluble in an aqueous medium and not fluorescent in solution at room temperature, emits a luminescence in the region of 450 nm, even in air-saturated aqueous solutions, when complexed to β or γ-cyclodextrin. The intensity decreases in the order β> γ and the quantum yields of luminescence are in the range 10^?3–10^?4. Further, retinal molecules in the inclusion complexes are subject to a bleaching process. Solubilization in micellar sodium dodecyl sulphate solutions also allows emission, albeit in smaller yield.     

Low temperature synthesis and characterization of rosette-like nanostructures of ZnO using solution process

Rosette-like structures of ZnO were synthesized at low temperature (60 °C) using solution process over 20 min of time. Hydroxylamine hydrochloride was used as capping agent with zinc nitrate hexahydrate and sodium hydroxide. Transition from triangular shaped plate like particles to rosette-like structure and to individual nanorods is observed with increasing refluxing temperature. Single-crystalline nature with wurtzite hexagonal phase is confirmed from transmission electron microscopic observations. Photoelectron spectroscopic measurement presented spectra close to the standard bulk ZnO, with an O 1s peak composed of surface adsorbed O–H group, O^2? in the oxygen vacancies on ZnO structure and ZnO.     

Single-step synthesis of pyrazoles using titanium catalysis

A simple titanium complex catalyzes the coupling of alkynes, isonitriles, and monosubstituted hydrazines to generate substituted pyrazoles in a single step.     

Room temperature crystallization of amorphous polysiloxane using photodimerization

Bulk crystallization in flexible polymeric systems is difficult to control due to the random orientation of the chains. Here we report a photo cross-linking strategy that results in simultaneous cross-linking and crystallization of polysiloxane chains into millimeter sized leaf-like polycrystalline structures. Polymers containing pendant anthracene groups are prepared and undergo [4+4] photocycloaddition under 365 nm irradiation at room temperature. The growth and morphology of the crystalline structures is studied using polarized optical microscopy (POM) and atomic force microscopy and is found to progress through three unique stages of nucleation, growth, and constriction. The mobility of the individual chains is probed using pulsed-field gradient (PFG) NMR to provide insights into the diffusion processes that may govern chain transport to the growing crystal fronts. The room temperature crystallization of this conventionally amorphous polymer system may allow for a new level of morphological control for silicone materials.

Millimeter sized polymer crystallites grow rapidly when anthracene-containing siloxanes are photocrosslinked using UV light.     

CaCO3超细粉末的低温水热合成与表征

超细碳酸钙有颗粒尺寸小、比表面积大和表面活性高等优良特性,在橡胶、塑料、纸张、涂料、日用化学品等领域有广泛的应用。因此,研究CaCO3超细粉末的制备方法,开发CaCO3超细微粉的用途,具有十分重要的意义。目前其制备方法主要是碳化法,本文利用水热法制备单一相超细CaCO3粉末,通过不同的反应前驱物在120℃和150℃下进行水热反应直接合成出超细CaCO3粉末,并对产品的结构和形貌进行了表征。     

高分子基质作用下多孔碳酸钙的仿生合成

依据生物矿化的基本原理,通过仿生合成的方法,以聚丙烯酰胺作为基质合成了一种有机、无机复合的多孔碳酸钙材料.用X射线粉末衍射(XRD)分析、扫描电子显微镜(SEM)、傅里叶变换红外吸收光谱(FT-IR)和电导率测定等手段对所得复合碳酸钙进行了表征,结果发现该多孔CaCO3晶体为方解石型,并且在结晶过程中,聚丙烯酰胺与CaCO3之间存在着相互作用,本文讨论了这种作用的可能机理.     

三草酸合铁(Ⅲ)酸钾的室温固相合成与晶体结构表征

以草酸钾和氯化铁为原料,通过室温固固反应合成了三草酸合铁(Ⅲ)酸钾配合物,用ICP、元素分析、X-射线单晶衍射、X-射线粉末衍射、红外光谱及热分析等方法对其组成和结构进行了表征.实验结果表明:三草酸合铁(Ⅲ)酸钾K3[Fe(C2O4)3]·3H2O的晶体结构属于单斜晶系,P2(1)/n空间群,晶胞参数a=0.774 52(4) nm,b=1.990 39(10) nm,c=1.034 31(5) nm,β=107.704(2)°,Z=4,Dc=2.148 g/cm~3.草酸根中的O原子与Fe原子形成了配位数为6的变形八面体配合物,在N2气氛中的热分解过程分4步,最后的残余物为FeO和K_2CO_3.     

Room temperature facile synthesis of quinoxalines catalyzed by amidosulfonic acid

Amidosulfonic acid NH₂–SO₃H catalyzed direct condensations of o‐phenylenediamines with α‐diketones at room temperature in organic solvents to afford quinoxalines in excellent yields. The amidosulfonic acid as a solid acid catalyst in this preparation was efficient and recoverable.     

An efficient procedure for the synthesis of Esomeprazole using a titanium complex with two chiral ligands

A procedure has been proposed for the selective preparation of Esomeprazole via asymmetric oxidation of the corresponding prochiral sulfide in the presence of a catalytic complex derived from titanium(IV) isopropoxide and two different chiral ligands, diethyl d-tartrate and (R)-N,N-dimethyl-1-phenyl-ethanamine.