In-situ synthesis of nanoparticles via supersolubilizing micelle self-assembly

In-situ synthesis of nano-particles using the self-assembly of molten salt and super soluble micellae was proposed based on a phenomenon of super solubilization of molten salt in reverse micellae and its self-assembly when the concentration reached up to 95% (w/w). The mechanism of the self-assembly indicates that the self-assembly of molten salt occurs in a reverse micelle where a homogenous phase is established between 5% (w/w) of a surfactant with a VB value of less than 1 and a hydrocarbon species. This synthesis has some unique features, such as being free of water, highly effective deposition and narrow distribution of particle size.     

In-situ synthesis of nanoparticles via supersolubilizing micelle self-assembly

In-situ synthesis of nano-particles using the self-assembly of molten salt and super soluble micellae was proposed based on a phenomenon of super solubilization of molten salt in reverse micellae and its self-assembly when the concentration reached up to 95%(w/w).The mechanism of the self-assembly indicates that the self-assembly of molten salt occurs in a reverse micelle where a homogenous phase is established between 5%(w/w)of a surfactant with a VB value of less than 1 and a hydrocarbon spe- cies.This synthesis has some unique features,such as being free of water,highly effective deposition and narrow distribution of particle size.     

Novel synthesis and characterization of CuO nanomaterials:Biological applications

CuO nanoparticles were synthesized at a relatively low temperature(80 ℃) for 2 h using polyethylene glycol-glycerol mixture which acts as a capping agent.A detailed characterization of the synthesized nanomaterials were performed utilizing X-ray diffraction(XRD),infra-red spectroscopy(IR),thermogravimetric analysis(TGA-DTA),transmission electron microscopy(TEM),photoluminescence(PL) by studying its crystalline phase,vibrational mode,thermal analysis,morphology and photoluminescence properties.The effect of annealing on the as-prepared nanoparticles were studied and compared with their corresponding bulk counterpart.The synthesized nanoparticles have been screened for in vitro cytotoxicity(1C_(50)) studies against the human cervical adenocarcinoma cell line(HeLa) using WITT assay methods.The as-prepared nanoparticle inhibits the proliferation of this HeLa cell.The standard disc diffusion method has been used to study the antibacterial activity of the samples against the human pathogenic bacteria Escherichia coli(MTCC 729),Proteus mirabilis(MTCC 425) and Klebsiella pneumoniae subsp.pneumoniae(MTCC 432).The results have been compared with the positive control antibiotic gentamycin.The synthesized nanoparticles would provide a potential alternative to antibiotics for controlling some of the microorganisms causing urolithiasis.     

Direct synthesis of silver/polymer/carbon nanocables via a simple hydrothermal route

High-yield silver/polymer/carbon nanocables were synthesized via a one-step simple hydrothermal route by using silver chloride and glucose as precursors. High-resolution TEM and element mapping proved that as-prepared nanocables consist of a silver nanowire core, a polymer inner shell, and a graphitic carbon outer shell. A three-step growth mechanism was proposed to explain the growth of such three-layer nanocables, i.e. the formation of silver nanowires, the glycosidation of glucose molecules on silver nanowire surface and the carbonization of the outmost glycosidation layer. We believe that reaction temperature plays the key role in the polymerization of glucose and sequent surface-carbonization.     

超增溶胶团自组装合成纳米氧化铝

应用超增溶胶团纳米自组装原理,以硝酸铝和尿素为熔盐,聚异丁烯马来酸三乙醇胺为表面活性剂制备超增溶氢氧化铝胶团,然后以氢氧化铝为前躯体合成纳米氧化铝.采用BET、压汞法、SEM、TEM和XRD方法对合成的氧化铝进行表征.结果表明,纳米氧化铝粒子形状为球形体或棒状体,孔道在几十纳米到几百纳米,粒度分布均匀且纯度较高.     

Preparation of AgCl-polyacrylamide composite microspheres via combination of a polymer microgel template method and a reverse micelle technique

A new route was created for the preparation of AgCl-polyacrylamide (AgCl-PAM) composite microspheres with patterned surface structures. The route is a combination of a polymer microgel template method and a reverse micelle technique. The size of the AgCl nanoparticles existing on the surfaces of the composite microspheres and the clearness of the surface patterns of the composite microspheres can be altered by simply adjusting the amount of precipitated AgCl and the rate of the deposition reaction. The route can be also used for the preparation of other water-insoluble salt-polymer composite microspheres, such as BaSO(4)-PAM. It is expected that the composite microspheres with patterned surface structures may not only combine the advantages of polymers and those of inorganic compounds, but also combine the advantages of microspheres in the micrometer size range and those in the nanometer size range.     

Synthesis of alpha-chymotrypsin/polymer composites by a reverse micelle/gas antisolvent method

Alpha-chymotrypsin (CT)/polyvinylpyrrolidone (PVP) composites was synthesized by combination of reverse micelles and CO(2). In this method, the two reverse micellar solutions containing CT and PVP, respectively, were first mixed, then compressed CO(2) was used as an antisolvent to precipitate the CT and PVP simultaneously and CT/PVP composites were successfully prepared. The morphology of the obtained CT/PVP composites was characterized by transmission electron microscopy (TEM). The FTIR spectra of the composites showed that there was interaction between CT and PVP. The storage activity of the enzyme immobilized on the polymer by this method was higher than that of the pure enzyme. This method has some advantages and can be easily applied to the synthesis of some other enzyme/polymer composites.     

Novel enzyme/DNA/inorganic nanomaterials: a new generation of biocatalysts

The design, synthesis and properties of a new class of enzyme/DNA/inorganic nanobiomaterials are described here. DNA has been used to stabilize the enzymes intercalated in the galleries of the inorganic solid, alpha-Zr(iv) phosphate (alpha-Zr(HPO(4))(2).H(2)O, abbreviated as alpha-ZrP). Interestingly, the presence of DNA improved the activity and stability of the bound enzymes. Key studies leading to the current strategy are presented initially, and these are followed by more recent developments. Several enzymes and proteins, including horseradish peroxidase, lysozyme, glucose oxidase, chymotrypsin, bovine serum albumin, cytochrome c, met-hemoglobin and met-myoglobin are successfully intercalated in the galleries of alpha-ZrP, under benign ambient conditions (aqueous buffered solutions, at room temperature and neutral pH). These novel materials are characterized by XRD, SEM and TEM as well as by biochemical, calorimetric and spectroscopic methods. Spectroscopic studies (circular dichroism, CD), for example, indicated that co-intercalation of DNA improved the retention of bound enzyme structure. The activity was enhanced markedly (five-fold) when DNA is co-intercalated, when compared to the activity in the absence of DNA. Addition of DNA to the sample, after enzyme intercalation, did not make any improvements. Our hypothesis is that enzyme-DNA supramolecular complex binds to the solid and the unfavorable interactions between the enzyme and the solid are minimized. These novel nanobiocomposite materials provide a simple method for packaging DNA and aid in engineering more effective synthetic materials for gene/RNA-delivery and drug delivery applications.     

Morphology-controlled synthesis of nanostructured zinc hydroxide fluoride via a microwave-assisted ionic liquid route

Zinc hydroxide fluoride (Zn(OH)F) with multiform morphologies such as flower-like particles, pumpkin-like aggregates, and hollow orange-like aggregates are prepared by a microwave-assisted ionic liquid method. During synthesis, microwave irradiation accelerates the reaction rate and shortens the reaction time. 1-Butyl-3-methylimidazolium tetrafluoroborate ([Bmim][BF₄]) or 1-2-hydroxylethyl-3-methylimidazolium tetrafluoroborate ([C₂OHmim][BF₄]) is used as both reactant and template. Experimental results indicate that the morphology evolution of Zn(OH)F is mainly controlled by the concentration of zinc acetate solution. A possible mechanism underlying the formation of nanostructured Zn(OH)F with diverse morphologies is proposed. Furthermore, nanoporous ZnO is obtained by the thermal decomposition of as-prepared Zn(OH)F in air, and the morphology is well retained.     

Facile synthesis of microporous carbonaceous materials derived from a covalent triazine polymer for CO_2 capture

Highly porous nitrogen-doped carbon materials were synthesized by the carbonization of a low-cost porous covalent triazine polymer, PCTP-3, which had been synthesized by the AlCl_3 catalyzed FriedelCrafts reaction of readily available monomers. The nature of the bond and structure of the resulting materials were confirmed using various spectroscopic methods, and the effects of KOH activation on the textural properties of the porous carbon materials were also examined. The KOH-activated porous carbon(aPCTP-3c) materials possessed a high surface area of 2271 m~2 g~(-1) and large micro/total pore volumes of 0.87/0.95 cm~3 g~(-1), respectively, with narrower micropore size distributions than the porous carbon prepared without activation(PCTP-3c). The aPCTP-3c exhibited the best CO_2 uptakes of 284.5 and 162.3 mg g~(-1) and CH_4 uptakes of 39.6 and 25.9 mg g~(-1) at 273 and 298 K/1 bar, respectively, which are comparable to the performance of some benchmark carbon materials under the same conditions. The prepared materials exhibited high CO_2/N_2 selectivity and could be regenerated easily.     

CdS/有机复合纳米材料的可控合成与表征

本文在室温下,以正丁胺为模板剂,二硫化碳为硫源,制得了CdS/有机复合纳米材料.采用XRD、FTIR、SEM、TEM、元素分析以及热重分析(TG)等测试手段对产物进行了表征.实验结果表明产物的结构是CdS(CH3CH2CH2CH2NHCSNHCH2CH2CH2CH3) (CS2).随着正丁胺与二硫化碳的摩尔比、陈化时间...     

Novel synthesis of o-naphthothiophenequinone derivatives via regioselective Diels-Alder reaction

A novel procedure to construct o-naphthothiophenequinones has been achieved from readily available o-benzothiophenquinones and N-dienes via Diels-Alder reaction-aromatization sequence as key steps. The absolute regioselectivity was established via Diels-Alder reaction of o-benzothiophenquinones with rich electron N-dienes.     

Structural characterization of amorphous and nanostructured bismuth silicate xerogels

Bismuth silicate xBi₂O₃·(1 − x)SiO₂ xerogels, 0 ≤ x ≤ 0.5, doped with gadolinium have been synthesized by sol–gel method. The study aims to evidence by X-ray diffraction (XRD), electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) the structural changes in amorphous Bi₂O₃–SiO₂ xerogels, function of Bi₂O₃ content and heat treatment. As was proved by XRD, nanostructured samples were obtained after 30 min heat treatment at 400 °C of the as-prepared samples with x > 0, in the mainly amorphous matrices nanocrystals of Bi_5.6Si_0.5O_9.4 phase being developed. The dimension of the nanocrystallites are function of the bismuth content, and vary from few nanometers to 25 nm for samples with x = 0.14 and x = 0.5 respectively. The local order around silicon, reflected by 29Si MAS NMR spectra, is less dependent on both composition and thermal history of the samples, showing that an amorphous silicon rich phase is present in all samples. The changes in the local order around Gd³⁺ ions, as reflected by the EPR spectra dependence on composition and especially on the heat treatment, support the assumption that a part of these paramagnetic ions is incorporated in the bismuth rich phase.     

Novel formal synthesis of cephalotaxine via a facile Friedel-Crafts cyclization

[structure: see text]. A novel formal synthesis of cephalotaxine (CET), the parent structure of the antileukemia Cephalotaxus alkaloids, was achieved via a facile Friedel-Crafts cyclization of the amino (or amido) spiro-cyclopentenone precursor (A) mediated by a protic acid leading to tetracyclic ketone B. A remarkable stereoelectronic effect of the methylenedioxy substituent (R) and an interesting skeletal isomerization of the CET core ring system (B, X = H2) were observed.     

Novel synthesis of the glycosidase inhibitor deoxymannojirimycin and of a synthetic precursor D-lyxo-hexos-5-ulose

[reaction: see text]. The synthesis of D-lyxo-hexos-5-ulose (5-ketomannose, 1,5-dicarbonyl sugar), a synthetic precursor to the glycoprocessing inhibitor deoxymannojirimycin, was carried out by an in situ epoxidation and hydrolysis of a trimethylsilyl-protected 6-deoxyhex-5-enopyranoside followed by facile removal of the protecting groups. A novel nine-step synthesis of deoxymannojirimycin has also been achieved from methyl alpha-D-mannopyranoside; this involved methanolysis of epoxides derived from an acetylated 1-azido-6-deoxyhex-5-enopyranoside followed by deprotection and catalytic hydrogenation.     

Novel synthesis of photochromic polymers via ROMP

[reaction: see text] Ring-opening metathesis polymerization (ROMP) of a photochromic 1, 2-bis(3-thienyl)cyclopentene monomer generated a series of novel polymers. All polymers exhibit reversible light-activated interconversion between their colorless-open and their colored-closed forms.     

Mechanochemical synthesis of a nitrogen-containing amorphous carbonaceous material

The results of mechanochemical treatment of an amorphous carbonaceous material (ACM) together with urea in a planetary ball mill with ball accelerations up to 60 g are discussed. The common mechanochemical treatment of an AMC and urea is helpful to add up to 2.6 wt % urea to the AMC. X-ray photoelectron spectroscopy indicates that nitrogen can enter the AMC structure in the form of three-coordinated and quaternary nitrogen. The mechanochemical treatment of an AMC together with urea considerably increases the micropore proportion on account of the destruction of larger pores.     

Predictive modeling of creep in polymer/layered silicate nanocomposites

A predictive creep model is developed which uses the properties of matrix and reinforcement to predict the creep of polymer/layered silicate nanocomposites. Up to this point, primarily empirical creep models such as Findley and Burgers models have been used for creep of polymer/clay nanocomposites. The proposed creep model is based on the elastic-viscoelastic correspondence principle and a stiffness model of these nanocomposites. Also, the added stiffness of polymeric matrix due to the constraining effect of layered silicates on polymer chains in the nanocomposite is considered by a parameter termed constraint factor. The results of the proposed model show good agreement with experimental creep data for different clay contents, stresses and temperatures. Comparing the model predictions with experimental data, a logical relationship between the method of processing and the constraint factor is discovered which shows that in-situ polymerization can be more efficient for improving creep resistance of polymer/layered silicate nanocomposites relative to melt processing.