Thermo-analytical study on stainless steelmaking dust

1　INTRODUCTIONStainlesssteelmakingdustisaby productwastegeneratedfromsteelmakingindustry .Itcontainssig nificantamountsofiron ,lead ,nickel,chromium ,etc .Heavymetalmaybeleachedintotheenviron mentbyrainorundergroundwater ,soitisclassifiedashazardouswastesandbannedbeingdisposedinreg ularlandfill[1] .Thevaluablemetalsinthedustcanberecoveredinthewayofdirectrecycling[2 6 ] andtheworthlessdustshouldbetreatedinthewayofvitrifi cation[7] .But,itisnecessarytocommandthether malbehaviorofthedustbe…     

Synthesis and optophysical properties of blue-emitting iridium （Ⅲ） complex bearing oxadiazole-based picolinic acid derivative

An iridium (III) bis[(4,6-difluorophenyl)pyridinato-N, C²][6-(6′-(4″-(5‴-phenyl-1‴, 3‴, 4‴-oxadiazole- 2‴-yl) phenoxy) hexyloxy picolinate) was synthesized and characterized by ¹H NMR and elementary analysis in order to study the effect of ancillary ligand of the oxadiazole-based picolinic acid derivative on optophysical properties of its iridium complex, and further to obtain an iridium complex with highly-efficient blue emission. The thermal stability, UV absorption and photoluminescent properties of this iridium complex were investigated. Compared with iridium (III) bis[(4,6-difluorophenyl)pyridinato-N, C²](picolinate) reported as a highly-efficient blue electroluminescent material, this iridium complex bearing an oxadiazole-based picolinic acid derivative presents higher thermal stability, more intense UV absorption at 291 nm and similar photoluminescent spectrum peaked at 469 nm. This indicates that tuning ancillary ligand of picolinic acid with an oxadiazole unit can improve the optophysical properties of its iridium complex. Foundation item: Projects(20772101, 50473046) supported by the National Natural Science Foundation of China; Project(2007FJ3017) supported by the Hunan Provincial Science Foundation, China; Project(07C764) supported by the Science Foundation of the Education Department of Hunan Province, China     

High temperature cyclic oxidation behavior of Y2O3-ZrO2 thermal barrier coatings irradiated by high-intensity pulsed ion beam

The high-temperature oxidation resistance behavior of 7% (mass fraction) Y₂O₃-ZrO₂ thermal barrier coatings (TBCs) irradiated by high-intensity pulsed ion beam (HIPIB) was investigated under the cyclic oxidation condition of 1 050 °C and 1 h. The columnar grains in the TBCs disappear after the HIPIB irradiation at ion current densities of 100–200 A/cm² and the irradiated surface becomes smooth and densified after remelting and ablation due to the HIPIB irradiation. The thermally grown oxide (TGO) layer thickness of the irradiated TBCs is smaller than that of the original TBCs. After 15 cycles, the mass gains of the original TBCs and those irradiated by ion current densities of 100 and 200 A/cm² due to the oxidation are found to be 0.8–0.9, 0.6–0.7, and 0.3–0.4 mg/cm², respectively. The inward diffusion of oxygen through the irradiated TBCs is significantly impeded by the densified top layer formed due to irradiation, which is the main reason for the improved overall oxidation resistance of the irradiated TBCs. Foundation item: Projects supported by The 2nd Stage of Brain Korea and Korea Research Foundation     

Synthesis and photophysical and electrochemical properties of new cyclometalated platinum complex containing oxadiazole ligand

A new cyclometalated platinum complex containing 2, 5-bis（naphthalene-1-yl）-1,3,4-oxadiazole ligand was synthesized and characterized. The UV-Vis absorptions and photoluminescent properties of the ligand and its platinum complex were investigated A characteristic metal-ligand charge transfer absorption peak at 439 nm in the UV spectrum and a strong emission peak at 625 nm in the photoluminescence spectrum were observed for this complex in dichloromethane. Cyclic voltammtry （CV） analysis shows that the EHOMO （energy level of the highest occupied molecular orbital） and ELUMO （energy level of the lowest unoccupied molecular orbital） of the platinum complex are about -5.69 and -3.25 eV, respectively, indicating that the oxadiazole-based platinum complex has a potential application in electrophosphorescent devices used as a red-emitting material.     

频率响应法研究苯在N a Y分子筛上的吸附和扩散行为

利用频率响应技术考察了苯在N a Y分子筛上的吸附、 扩散行为, 并与TG / DTG曲线和吡啶红外等技 术相结合来分析苯在分子筛上的吸附扩散机理。结果表明, N a Y分子筛中存在两种酸性中心, 即弱B酸中心和弱L 酸中心, 且以L酸中心为主; 在3 3 3、 4 2 3K时, 苯在N a Y分子筛上有两个吸附作用力, 分别是孔填充物理吸附和π电 子相互作用两种吸附形式。逐渐接近加氢催化裂化反应的温度( 5 7 3K) 时, 苯在 N a Y分子筛上的传质仍以吸附过程 为主。但是6 2 3K时, 在 N a Y分子筛上的传质以扩散过程为主, 吸附作用力弱, 易脱附, 更易于芳烃分子在其上的扩 散, 从而提高加氢裂化反应性能。     

Manufacture of high-dispersed W-Cu composite powder by mechano-thermal process

In order to improve the process of co-reduction of oxide powder, a new mechano-thermal process was designed to produce high-dispersed W-Cu composite powder by high temperature oxidation, short time high-energy milling and reduction at lower temperature. The particle size, oxygen content and their sintering abilities of W-Cu composite powder in different conditions were analyzed. The results show that after a quick milling of the oxide powder for about 3-10 h, the reduction temperature of the W-Cu oxide powder can be lowered to about 650 ℃ from 700-750 ℃ owning to the lowering of particle size of the oxide powder. The average particle size of W-Cu powder after reduction at 650 ℃ is about 0. 5μm smaller than that reduced at 750 ℃. After sintering at 1 200℃ for 1 h in hydrogen atmosphere, the relative density and thermal conductivity of final products (W-20Cu) can attain 99. 5% and 210 W ·m-1· K-1 respectively.     

Electrochemical behavior of diverse vanadium ions at modified graphite felt electrode in sulphuric solution

PAN-based graphite felt (PGF) treated in 98% sulphuric acid for 5 h and then kept at 450 ℃ for 2 h was evaluated for their electrochemical performance as electrodes of vanadium redox battery (VRB). Structure and characteristic of treated PAN-based graphite felt (TPGF) were determined by means of Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, Brunauer-Emmett-Teller surface area analysis and VRB test system. The results show that the acid and heat synergistic effect increase the number of —COOH functional groups on the PGF surface, and the PGF is eroded by sulphuric acid oxidation, resulting in the surface area increases from 0.31 m2/g to 0.45 m2/g. The V(Ⅱ)/V(Ⅲ) redox reaction is electrochemically reversible on the TPGF electrode, while the V(Ⅳ)/V(Ⅴ) couple is a quasi reversible process. The diffusion coefficients of the oxidation for V(Ⅳ)/V(Ⅴ) obtained from the scope of peak current Ip vs scan rate v1/2 is 4.4×10-5 cm2/s. The improvement of electrochemical activity for the electrode is mainly ascribed to the increase of the number of —COOH groups on the TPGF, which behaves as active sites catalyzing the vanadium species reactions and accelerating electron transfer reaction and oxygen transfer.     

Synthesis of lanthanum tris (mono- i -octyl phthalate) and its thermal stability for polyvinyl chloride

A novel type of thermal stabilizer—lanthanum tris (mono-i-octyl phthalate) (LTMP) was synthesized by double-decomposition reaction of sodium mono-i-octyl phthalate with lanthanum chloride at 60 °C. Sodium mono-i-octyl phthalate was prepared by sodium hydrate and mono-i-octyl phthalate prepared by reaction of isooctyl alcohol and phthalic anhydride in the presence of sulfuric acid catalyst at 110 °C. The yield of lanthanum tris (mono-i-octyl phthalate) is about 84.5%. Its thermal stabilities were measured by heat-ageing oven test when incorporated into PVC. The experimental results show that the heat stability time is about 40min at 190 °C when adding 3phr (per hundred resin) to PVC. The thermal stability of this product is better than that of Ca-Zn complex and basic lead salt stabilizers, and equal to that of dibutyltin diaurate. Foundation item: The Key Program of 9^th Five-Year Plan of China(No. 96-119-04-03-05) Biography of the first author: LIU You-nian, associate professor, born in Oct. 1964, majoring in fine chemical engineering & separation processes.     

Synthesis, oxygenation and catalytic performance of manganese complex with p-aminomethyl benzoic acid Schiffbase

The amino acid Schiff base complex (Sal-AMBA-Mn) was prepared with p-amino-methylbenzoic acid, salicylaldehyde and Mn(OAc)2·4H2O. Its structures was characterized with IR and UV spectra. Oxygenation mechanism of the complex in N, N-dimethylformamide solution was investigated. The results show that lower temperature is in favor of the oxygenation, and energy, enthalpy and entropy are -3.8 kJ/mol, -4.2 J/mol and -161.44 J/(mol·K), respectively. In the presence of the manganese complex, dehydroepiandrosterone acetate is effectively oxidized by molecular oxygen and the corresponding enone 7-ketodehydroepiandrosterone acetate is obtained. The yield is 62.1% when the oxidation is carried out under the reaction conditions of 60 ℃, 2 MPa of O2 pressure, C5H5N as a solvent and molar ratio of the substrate to the complex of 1:10.     

Identification and analysis based on genetic algorithm for proton exchange membrane fuel cell stack

The temperature of proton exchange membrane fuel cell stack and the stoichiometric oxygen in cathode have relationship with the performance and life span of fuel cells closely. The thermal coefficients were taken as important factors affecting the temperature distribution of fuel cells and components. According to the experimental analysis, when the stoichiometric oxygen in cathode is greater than or equal to 1.8, the stack voltage loss is the least. A novel genetic algorithm was developed to identify and optimize the variables in dynamic thermal model of proton exchange membrane fuel cell stack, making the outputs of temperature model approximate to the actual temperature, and ensuring that the maximal error is less than 1℃. At the same time, the optimum region of stoichiometric oxygen is obtained, which is in the range of 1.8 -2.2 and accords with the experimental analysis results. The simulation and experimental results show the effectiveness of the proposed algorithm.     

Behavior of oxygen in DG? invar-Cu alloys and its effects on mechanical and physical properties

The invar alloy powder, mixed with different Cu powder contained different content of oxygen, was compacted and sintered into four sorts of DG™ invar-Cu low expansion and high conductivity alloy specimens. The mechanical and physical properties of the alloys were tested and analyzed. The behavior of oxygen and its effect mechanism were discussed. The results show that the ultimate strength decreases with the increase of oxygen content, so does the coefficient of thermal expansion (α) whereas the α platform is shortened. Project supported by the Natural Science Foundation of Hunan Province Synopsis of the first author Wang Zhifa, Senior Engineer, born in 1946, specializing in electronic packing materials. His studied group developed the first W disc and the first invar-Cu plate of the country for power semiconductor devices.     

Aerobic oxidation behavior of α-ionone catalyzed by N-hydroxyphthalimide combined with acetylacetone cobalt(II)

A practical catalytic method to oxidize α-ionone with molecular oxygen using N-hydroxyphthalimide(NHPI) combined with acetylacetone cobatt(II) (Co(acac)₂) was developed, and the probable catalytic mechanism was proposed. The influences of the reaction conditions on conversion of α-ionone and the selectivity of the major product (5-keto-α-ionone) were investigated, and the technical parameters for 5-keto-α-ionone were optimized. The results show that the primary product is 5-keto-α-ionone, and by-products include epoxy-α-ionone, as well as rearrangement products 4-keto-β-ionone and epoxy-β-ionone, which are characterized by infrared spectra, proton nuclear magnetic resonance spectra, mass spectra and elemental analysis. The selectivity of 5-keto-α-ionone and the conversion of α-ionone are 55.0% and 97.0%, respectively, when 30%(molar fraction) NHPI, 1.0%(molar fraction) Co(acac)₂ and no solvent are employed under O₂ pressure of 1.0 MPa and the reaction temperature of 65 °C for 11 h. The procedure shows good reproducibility in the parallel experiments. Foundation item: Project(50573019) supported by the National Natural Science Foundation of China     

Preparation of ferromagnetic metal fine fibers by organic gel-thermal reduction process

The organic gel-thermal reduction process was used for the preparation of ferromagnetic metal Ni, Co and Fe fine fibers from the raw materials of citric acid, lactic acid and metal salts. The structure, thermal decomposition process and morphologies of the gel precursors and fibers derived from thermal reduction of these gel precursors were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, thermo-gravimetric/differential scanning calorimetry and scanning electron microscopy. The results show that spinnability of gel largely depends on molecular structure of metal-carboxylate complex that is a linear-type structure formed in the gel. As a result, the gels exhibit a good spinnability. Metal Ni, Co and Fe fine fibers are featured with diameters of around 1 μm and a high aspect ratio up to 1×106.     

Determination of thermal conductivity of magnesium-alloys

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Potential control flotation of galena in strong alkaline media

The electrochemical oxidation of galena in collectorless and collector flotation systems, particularly in strong alkaline media, was studied. The results show that, with pH value higher than 12.5 and potentials below 0.17 V, the oxidation products of galena are elemental sulfur and HPbO2^- . Elemental sulfur was present on the mineral surface in excess of oxidized lead species due to dissolution of HPbO2^- , which is beneficial to the flotation of galena. Under the same conditions, sphalerite and pyrite were depressed as a result of significant surface oxidation. Diethyldithioearbamate (DDTC) was found to be the most suitable collector for galena flotation in strongly alkaline media. The very potential produced hydrophobic PbD2-the surface reaction produet of DDTC with galena, is 0 to 0.2 V. Meantime DDTC can depress the surface over-oxidation of galena.Investigations also indicate that, in the range of - 0.9 V to 0.6 V, hydrophobic PbD2 can be firmly adsorbed on galena.     

Kinetics of Fe3O4 formation by air oxidation

The kinetics of Fe₃O₄ formation by air oxidation of slightly acidic suspension of Fe(OH)₂ was studied. The effects of initial concentration of Fe(II), temperature, partial pressure of oxygen, air flow rate and stirring rate on the oxidation rate were investigated. The results show that Fe₃O₄ formation is composed of two-step reaction, the first step is the formation of Fe(OH) ₂ ⁺ by oxidation of Fe(OH)⁺ complex ions, the second step is the formation of magnetite by dehydration and deprotonation of Fe(OH)⁺ and Fe(OH) ₂ ⁺ . The oxidation reaction is zero-order with respect to the concentration of Fe(II) and around 0.5-order with respect to partial pressure of oxygen, and oxygen transfer process is rate-limiting step of oxidation reaction with apparent activation energy of 2.74 kJ · mol⁻¹.     

Preparation and antimicrobial ability of natural proous antibacterial materials

The liquid ion exchange method, solid salt melt method and dry-wet circulation method were used to prepare natural porous antimicrobial materials with natural minerals, such as zeolite, spilite, palygorskite and montmorillonite, respectively. Atomic absorption spectrum and X-ray diffraction analysis were carried out to investigate the effects of Ag⁺, Cu²⁺ and Zn²⁺ on antimicrobial abilities of natural porous minerals, and the effect of preparation method on ion exchange capacity of antimicrobial material, respectively. The results show that for the ion exchange capacity, clay mineral is higher than fibrous mineral, i. e. both zeolite and montmorillonite are higher; the antimicrobial ability of material with Ag⁺ is the best; the exchange capacities of materials with Cu²⁺ or Zn²⁺ are all higher, but the antimicrobial ability of Cu²⁺ is better than that of Zn²⁺. Foundation item: Project (40072020) supported by the National Natural Science Foundation of China; project (2001AA322070) supported by the National High Technology Research and Development Program of China     

液相导向剂法合成高硅NaY型沸石

研制了液相导向剂 ,利用它合成了NaY型沸石 ,其产品结晶度高 ,Si/Al高 .目前有实际应用价值的合成方法是水热合成法 ,应用廉价水玻璃合成高硅NaY型沸石 ,并就合成条件进行了讨论 .     

Alteration of diaspore by thermal treatment

Diaspore (α-AlOOH) was heated at various temperatures from 300 to 1000 ℃ for 2 h. The alteration of diaspore by thermal treatment was investigated by differential thermal analysis, thermogravimetric analysis and X-ray diffraction. The mechanism of thermal decomposition of diaspore was discussed according to the Coats-Redfern equation. It is found that after thermal treatment at 500 ℃, diaspore is transformed entirely to corundum (α-Al2O3). Combined with the mass loss ratio obtained from the thermogravimetric analysis data, the activation energies for the thermal treatment of diaspore are calculated as Ea=10.4 kJ/mol below 400 ℃ and Eb=47.5 kJ/mol above 400 ℃, respectively, which is directly related to the structural alteration of diaspore during the thermal treatment. The results indicate that the thermal decomposition of diaspore is conducted primarily by means of an interfacial reaction.     

Cyclic oxidation behavior of Fe-9Cr-1Mo steel in water vapor atmosphere

The cyclic oxidation behavior of Fe-9Cr-1Mo steel (9Cr-1Mo) in 10%H₂O+90%Ar (volume fraction) atmosphere at 600, 650 and 700 for °C various time was studied. The oxidation mechanism of 9Cr-1Mo steel in 10%H₂O+90%Ar atmosphere was discussed. The thermal stress was evaluated in two oxide layers to illustrate the spallation of the oxide layer. The experimental results indicate that there exists a duplex oxide scale with an outer layer of Fe₂O₃ and an inner layer of mixed (Fe, Cr)₃O₄ formed on 9Cr-1Mo steel during cyclic oxidation. Some cracks generated in both inner and outer oxide layers. Parts of oxide scales spalled from substrate during the cyclic oxidation. A higher tensile stress in the oxide layer is formed at the early oxidation stage than at the later oxidation stage during heating. This tensile stress results in the formation of cracks in the oxide layer. Foundation item: Project(2006–8) supported by the Huadian International Corporation Limited