Synthesis of nanometer-sized sodalite without adding organic additives

Aggregates (80 nm) of sodalite nanocrystals with crystallite sizes ranging from 20 to 40 nm have been synthesized from a sodium aluminosilicate solution at low temperature, without adding any organic additives, while paying attention to the key factors for the synthesis of nanosized zeolite crystals. The physical properties of nanosized sodalite crystals were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, 29Si solid-state magic-angle spinning (MAS) NMR, and N2 adsorption. As expected, the external surface area of nanosized sodalite crystals is significantly increased compared with that of microsized sodalite crystals. The size of synthesized sodalite crystals can be controlled from 20 nm to 10 microm. It is found that the preparation of a homogeneous aluminosilicate solution followed by the formation of an aluminosilicate hard gel by adjusting the initial composition, for example, SiO2/Al2O3 and Na2O/H2O ratios, is critical for synthesis.     

Silica gel-mediated self-aldol reactions of highly volatile aldehydes under organic solvent-free conditions without reflux condenser

Silica gel-mediated self-aldol reactions were catalyzed by piperidine to give the corresponding α,β-conjugated aldehydes in good yields. The aldol reactions of 4-nitro-, 4-trifluoromethyl-, and 4-chlorobenzaldehydes with acetone afforded the corresponding aldol products. Highly volatile aldehydes and acetone could be employed even without a reflux condenser for these reactions. Silica gel could be recycled five times without any significant decrease of the yields of the products.     

Direct crystallisation of a hydroxy sodalite membrane without seeding using a conventional oven

A double layered hydroxy sodalite membrane was synthesised directly onto a tubular -alumina support without seeding using a conventional hot-air oven. The effect of different synthesis parameters including the water content, ageing period, synthesis time and temperature, on the purity and continuity of the membrane was investigated. The water content was an important factor in controlling the presence of contaminating zeolite phases in the membrane. The optimised membrane which was contaminant free was characterised by XRD, SEM and single gas permeation using He, N₂ and SF₆. The permeance of the three gases through the membrane ranged from 0.8 to 8 × 10⁻⁸ mol m⁻² s⁻¹ Pa⁻¹. The selectivity ( = 2.5–2.7) compared well to the Knudsen diffusion ratio for He/N₂.     

Spectroscopic characterization of the conversion of poly(p-phenylene-vinylene) precursor by ion irradiation

Different spectroscopic techniques show that poly(p-phenylene vinylene) films can be derived from a sulphonium precursor by irradiation with ion beams at energies of the order of 100 keV. The comparison with the pyrolysis conversion shows less chlorine and sulfur residues in the irradiated thickness, whereas some ketone structures are evidenced. The formation of nanometric scale carbon clusters induced by the irradiation degradation of PPV is however indicated by UV spectrophotometry, leading to bandgap narrowing and increase of the conductivity. The irradiation with doping species allows the conversion and doping of PPV films in a single stage. The induced conductivity is limited by the formation of complexes with chlorine residues through a gettering process.     

Using a precursor in lamellar structure for the synthesis of uniform ZnS nanocrystals

Uniform ZnS nanocrystals of about 15?nm were prepared through a low temperature hydrothermal approach by treating Zn-PhPO nanosheets with Na₂S aqueous solution. Both the precursor and the final product were studied by the means of X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The photo-luminescent spectrum of the synthesized ZnS nanocrystals showed their good crystalline nature. Based on this study, the precursor structure-controlling effect was discussed, and in addition, the relevant factors possibly affecting the particle formation and the growth possessed were applied in the discussion to interpret the transformation mechanism. Further research showed that both the structure characters of the precursors and the mass transportation which occurred during the synthesis greatly affected the morphology and organization state of the final products. This research may provide some facts on the structure-controlling approaches along with a general method for the preparation of uniform sulfide nanocrystals.     

桦甸油页岩有机岩相特征及其富集特性

为了研究油页岩中有机组分结合特性对有机质分离富集的影响,利用薄片透射光、反射单偏光、反射荧光等煤岩学研究手段研究桦甸油页岩中有机组分的种类、含量及赋存状态,并利用两种密度分离手段研究油页岩中有机质的解离特性.结果表明,桦甸油页岩有机质的变质程度较低,有机显微组分以沥青质体为主,占85.8%,镜质组和惰质组含量较低;有机质与矿物结合紧密,形成有机-矿物复合体,密度分离方法对有机质与矿物质分离效果有限;浮沉实验小于1.40g/cm³密度级样品的热解失重量及失重速率均低于较高密度级产物,这与颗粒状镜质组、惰质组与矿物质结合程度相对较差,在较低密度级产物中富集有关.     

Vibrations of a single adsorbed organic molecule: anharmonicity matters!

Vibrational spectroscopy is a powerful tool to identify molecules and to characterise their chemical state. Inelastic electron tunnelling spectroscopy (IETS) combined with scanning tunnelling microscopy (STM) allows the application of vibrational analysis to a single molecule. Up to now, IETS was restricted to small species due to the complexity of vibration spectra for larger molecules. We extend the horizon of IETS for both experiment and theory by measuring the STM-IETS spectra of mercaptopyridine adsorbed on the (111) surface of gold and comparing it to theoretical spectra. Such complex spectra with more than 20 lines can be reliably determined and computed leading to completely new insights. Experimentally, the vibrational spectra exhibit a dependence on the specific adsorption site of the molecules. Theoretically, this dependence is only accessible if anharmonic contributions to the interaction potentials are included. These joint experimental and theoretical advances open new perspectives for structure determination of organic adlayers.     

Enhancement of the conversion of toluene by Pseudomonas putida F-1 using organic cosolvents

Pseudomonas putida F-1 (ATCC700007) was used as a model organism in stirred tank reactors, to study conversion enhancement of poorly soluble substrates by organic cosolvents. After a literature study, silicone oil was used as a solvent system to enhance the mass transfer rate. To study the benefits of the organic solvent addition, batch experiments were conducted in two side-by-side fermentation vessels (experimental and control) at three different levels of silicone oil (10, 30, and 50%). Results showed that the presence of silicone oil resulted in a 100% increase in the toluene mass transfer compared to the control. Experiments in continuous stirred-tank reactors showed that improved conversion could beobtained, at higher agitation rates.     

不同催化剂上有机质加氢热解行为及催化作用机理研究

对不同类型催化剂如Zn Cl2、Ni Cl2、Fe2O3、Y型沸石(Na Y)及Mo S2上有机质的催化加氢热解行为及反应机理进行了研究。结果表明,有机质加氢液态产物收率和组成受控于催化剂类型,但不同催化剂上加氢热解所得到的产物生标参数差异不大;同时,对于不同成熟度和类型的有机质样品,各催化剂所体现的催化效果也不尽相同。基于固体残渣元素组成、红外光谱和X射线衍射分析结果发现,不同类型催化剂上的加氢作用机制也存在明显差异。与Ni Cl2相比,Zn Cl2体系中除存在催化裂解和催化加氢作用外,还存在质量传递效应;Fe2O3催化剂主要是通过其表面的活性O吸收H2中的H形成H自由基而加速有机质的加氢反应;Mo S2体系存在过渡金属Mo的催化加氢和中间产物H2S的自由基引发作用两种催化机制。     

Synthesis and ceramic conversion of a new oligomeric precursor to boron nitride

A new polyaminoborazine with good solubility was synthesized by ammonolysis reaction of a mixture of B‐chloroborazine, B‐bischloroborazine, and B‐trichloroborazine under mild condition. The oligomer was easily cured at 250°C. The pyrolytic residue of the cured oligomer was investigated with X‐ray photoelectron spectroscopy (XPS), powder X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermal gravimetric analysis (TGA). The results indicated that crystalline h‐BN with B/N ratio of 1:1.01 is main in the residue pyrolyzed at 1500°C. Copyright © 2010 John Wiley & Sons, Ltd.     

Aging effects on sorption-desorption behaviors of PAHs in different natural organic matters

Ag(2)S is an important direct semiconductor material that receives considerable research interest because of its low toxicity and high chemical stability. This work reports an easy and novel route for the synthesis of hollow Ag(2)S particles by a sacrificial core method in surfactant containing aqueous media. Sulfur is used as a sacrificial core in this method and removed by dissolving in carbon disulfide. Core sulfur particles were synthesized in situ by acid catalyzed reaction of sodium thiosulphate in aqueous surfactant media. The particles were characterized by using different instrumental techniques, showing 67% improved light emission capacity in terms of quantum yield compared to solid Ag(2)S particles. The same route is also suggested to prepare other nanoparticles.     

Electron beam conversion of cellulose into liquid organic products

Cotton and pine cellulose was distilled under the heating with a beam of accelerated electrons (∼2 kGy/s) in a flow of gaseous alkanes. An organic liquid (∼60 wt %), gas (13–18 wt %), and charcoal were the products. Carbonyl compounds and furans dominate in the composition of the liquid. It is supposed that electron beam processing has a combined effect including preliminary radiolytic modification of cellulose, the initiation of its radical-chain destruction, and strong rapid warming-up within tracks.     

Imidazole derivatives as the organic precursor of ZnO nano particle

N₁-Hydroxy-2,4,5-trisubstituted imidazoles were synthesized starting from 1,2-diketones. The crystal structure of 4,5-dimethyl-2-(3-nitrophenyl)-1H-imidazol-1-ol has been determined. An unusual intermolecular hydrogen bonding through the association of water molecule has been reported. These imidazole derivatives can be thought of as the organic precursor for the synthesis of zinc oxide nano particles.     

Effective photocatalytic degradation of organic pollutant by ZnS nanocrystals synthesized via thermal decomposition of single-source precursor

2-Aminocyclopentene-1-dithiocarboxylate complex of zinc(II) has been synthesized and found to be an effective single-source precursor for the preparation of ZnS NCs (rod and sphere) by the use of ethylenediamine and hexadecylamine as structure directing solvents. Structural characterizations were carried out using XRD, TEM and BET measurements and the optical properties by UV-Vis and PL spectroscopic techniques. The prepared ZnS NCs show effective photocatalytic activity towards the degradation of Rose Bengal dye (RB) under light irradiation for their probable application in waste water treatment. The degradation mechanism of RB dye under light irradiation is established by terephthalic acid photoluminescence probing technique.     

由硅溶胶生长单分散颗粒的研究

针对现行单分散二氧化硅颗粒制备方法的粒径预见性差、步骤繁琐、收率低等问题，研究了一种用硅溶胶作为种子，在氨、水和乙醇的混合溶液中通过水解正硅酸乙酯（ＴＥＯＳ）生长出单分散颗粒的简便方法。该方法仅在初始的悬浮液中滴加ＴＥＯＳ即可使种子正常生长，无须补充氨水以修正体系浓度的变化。最终的分散相浓度可达１０％（质量分数）。可选择生长的粒径范围在１微米以内并可精确控制。所得颗粒粒径分布偏差于Ｓｔｏｂｅｒ方法