Magnetic properties,phase evolution,hollow structure and biomedical application of hematite (α-Fe2O3) and QUAIPH

We investigate synthesis, phase evolution, hollow and porous structure and magnetic properties of quasi-amorphous intermediate phase (QUAIPH) and hematite (α-Fe₂O₃) nanostructure synthesized by annealing of akaganeite (β-FeOOH) nanorods. It is found that the annealing temperature determines the phase composition of the products, the crystal structure/size dictates the magnetic properties whereas the final nanorod morphology is determined by the starting material. Annealing of β-FeOOH at ～300 °C resulted in the formation of hollow QUAIPH nanorods. The synthesized material shows low-cytotoxicity, superparamagnetism and good transverse relaxivity, which is rarely reported for QUAIPH. The QUAIPH nanorods started to transform to porous hematite nanostructures at ～350 °C and phase transformation was completed at 600 °C. During the annealing, the crystal structure changed from monoclinic (akaganeite) to quasi-amorphous and rhombohedral (hematite). Unusually, the crystallite size first decreased (akaganeite → QUAIPH) and then increased (QUAIPH → hematite) during annealing whereas the nanorods retained particle shape. The magnetic properties of the samples changed from antiferromagnetic (akaganeite) to superparamagnetic with blocking temperature T_B = 84 K (QUAIPH) and finally to weak-ferromagnetic with the Morin transition at T_M = 244 K and high coercivity H_C = 1652 Oe (hematite). The low-cytotoxicity and MRI relaxivity (r₂ = 5.80 mM^?1 s^?1 (akaganeite), r₂ = 4.31 mM^?1 s^?1 (QUAIPH) and r₂ = 5.17 mM^?1 s^?1 (hematite)) reveal potential for biomedical applications.     

Synthesis of manganese titanate and its precursors from xerogel

An overview of research on the synthesis of manganese titanates is presented. The xerogel of Mn–Ti–O–C–H composition was synthesized from manganese acetate and titanium tetrabutylate via liquid-phase method using organic solvents. The calcination of xerogel in air at 450 °C and 700 °C yielded manganese titanate precursors in the form of a nanostructured mixture of Mn₂O₃ and TiO₂. Annealing at 1000 °C, manganese metatitanate MnTiO₃ was obtained. Reference experiments with initial reagents included, separately, thermal decomposition of Mn(CH₃COO)₂×4H₂O and the product of Ti(OC₄H₉)₄ hydrolysis. The composition, structure, and properties of the products were studied using X-ray diffraction, scanning electron microscopy, elemental analysis, diffuse reflectance IR Fourier spectroscopy, thermogravimetry, and by measuring specific surface area. The data presented by these different techniques are basically consistent with each other (with an increase in the annealing temperature, an increase in globule size and decrease in specific surface area are observed; structuring occurs within the long- and short-range order; the size of the crystallites does not exceed that of the globules; elemental composition correlates with phase composition; the endothermic character of the reaction of MnTiO₃ formation at 900 °C is confirmed by a thermodynamic calculation). Nevertheless, some unexpected effects were revealed (based on the FTIR diffuse reflection spectra, mixed oxide Mn–Ti–O is formed in the surface layer of particles already at 450 °C and 700 °C; etc.). Application of the proposed technique for modifying Al₂O₃ powders, with the aim of implementing low-temperature sintering of corundum ceramics, is discussed.     

Fluoride-mediately solvothermal synthesis and tunable photocatalytic selectivity of urchin-like ZrO2 hollow microspheres

Photocatalysts often show excellent performances on the basis of their surface state of exposed faces with high reactivity, but unfortunately surfaces of this type are usually concealed into the interior of crystals for their high surface energy. We report here a possibility that for fluorine-terminated surfaces of monoclinic ZrO₂, these higher-energy surfaces could be retained and exposed. Urchin-like ZrO₂ hollow microspheres (UZHS) composed of nanoribbons with exposed (010) facets are obtained through a fluoride mediately solvothermal method. We prove the stabilization effect of fluorine adsorption on (010) facets by density functional theory calculations. More interestingly, UZHS exhibit tunable photocatalytic selectivity in dye degradation. The fluorinated UZHS exhibit good performances both on decomposing Congo red (CR) and methylene blue, while the surface-modified UZHS by calcination only favor decomposition of CR.     

Synthesis,characterization and ion exchange properties of zirconium(IV) tungstoiodophosphate,a new cation exchanger

Zirconium(IV) tungstoiodophosphate has been synthesized under a variety of conditions. The most chemically and thermally stable sample is prepared by adding a mixture of aqueous solutions of 0·5 mol L⁻¹ sodium tungstate, potassium iodate and 1 mol L⁻¹ orthophosphoric acid to aqueous solution of 0·1 mol L⁻¹ zirconium(IV) oxychloride. Its ion exchange capacity for Na⁺ and K⁺ was found to be 2·20 and 2·35 meq g⁻¹ dry exchanger, respectively. The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the exchange capacity of drying the exchanger at different temperatures has been studied. The analytical importance of the material has been established by quantitative separation of Pb²⁺ from other metal ions.     

Interval based MINLP superstructure synthesis of mass exchange networks

A new simultaneous synthesis approach for mass exchange networks (MENs) is presented. The technique is adapted from the interval based mixed integer non-linear program (MINLP) superstructure (IBMS) synthesis of heat exchanger networks (HENs). The superstructure interval boundary compositions are defined by the supply and target compositions of either the rich or lean set of streams. Each rich and lean stream in the superstructure has the potential of exchanging mass with streams of opposite kind in each interval based on mass transfer feasibility. The model harnesses the strengths of the stagewise superstructure and the pinch technology methods for mass exchange network synthesis (MENS). The IBMS approach simultaneously trades-off the capital and operating costs for MENs. The superstructure composition interval defining approach introduced in this paper enforces the mixing of split streams at equal compositions, hence there is no need to include mixing equations in the model. Fixing the interval boundaries helps to eliminate the complexities involved in initialisations, thus the region of search for the optimum solution is reduced. The IBMS model is applied to MENS problems involving continuous contact and staged columns. It is also extended to problems involving multiple mass separating agents (MSAs) and regeneration. The results obtained compare well with those in the literature.     

聚碳硅烷的分子量分布与可纺性研究

阐述了聚碳烷的合成及其分子量分布，讨论了高低分子含量对聚碳硅烷熔点及可纺性的影响，而且提出了分子量分布的控制标准与方法。     

Synthesis, characteristics and oxygen-sensitive properties of SrMgxTi 1 − xO3 nanocrystals

SrMg_xTi_{1 - x}O₃ nanocrystals (x = 0.1–0.6) were synthesized by the stearic acid gel method. Powder samples were characterized by X-ray diffraction and X-ray photoelectron (XP) spectroscopy. The results showed that the lattice parameter a and the O 1s XP spectrum changed not only with the Mg content x but also with the grain size d of the samples. The conductivity of a thick film specimen fabricated on an aluminium oxide wafer was investigated in a nitrogen—oxygen atmosphere.     

Autothermal two-stage gasification of low-density waste-derived fuels

In order to increase the efficiency of waste utilization in thermal conversion processes, pre-treatment is advantageous. With the Herhof Stabilat^® process, residual domestic waste is upgraded to waste-derived fuel by means of biological drying and mechanical separation of inerts and metals. The dried and homogenized waste-derived Stabilat^® fuel has a relatively high calorific value and contains high volatile matter which makes it suitable for gasification. As a result of extensive mechanical treatment, the Stabilat^® produced is of a fluffy appearance with a low density. A two-stage gasifier, based on a parallel-arranged bubbling fluidized bed and a fixed bed reactor, has been developed to convert Stabilat^® into hydrogen-rich product gas. This paper focuses on the design and construction of the configured laboratory-scale gasifier and experience with its operation. The processing of low-density fluffy waste-derived fuel using small-scale equipment demands special technical solutions for the core components as well as for the peripheral equipment. These are discussed here. The operating results of Stabilat^® gasification are also presented.     

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天然气制合成油得到的柴油燃料基本不含硫和芳烃 ,费—托法合成技术的进步已使天然气制合成油(GTL)的生产成本可与 18～ 2 2美元 /桶的原油价格相竞争 ,因而GTL已成为天然气 ,尤其是偏远地区天然气高效利用的一个有前景的途径。GTL技术由合成气生产、费—托合成和产品精制三部分组成。GTL的工艺方案有埃克森公司AGC - 2 1工艺、壳牌公司SMDS工艺、萨索尔公司Synthol工艺、合成油公司工艺等。GTL技术在合成气生产和费托合成方面还出现了一些新的进展。 2 1世纪将迎来GTL装置新的发展期 ,在未来 15年内 ,预计GTL装置生产能力将增加 (45 0 0～ 6 75 0 )× 10 4 t/a。 2 0 0 5年前将有 7套GTL装置投运 ,总能力 880× 10 4 t/a。     

Polymerization Kinetics of Fischer‐Tropsch Reaction on Iron Based Catalysts and Product Grade Optimization

The polymerization kinetics of Fischer‐Tropsch reactions on a K‐promoted Fe catalyst was studied. To represent the product distribution, a kinetic model was developed based on alkyl and alkenyl mechanisms for hydrocarbon chain propagation, which were assumed to occur simultaneously in the Fischer‐Tropsch synthesis. The conclusion was drawn that superimposed Anderson‐Schulz‐Flory (ASF) distributions with different chain growth probabilities, on iron catalysts, can be the result of different chain growth mechanisms. The polymerization mechanism was used to obtain the product distribution for several conditions, and the optimum conditions for the production of transportation fuels were found.