Preparation of high selectivity silicalite-1 membranes by two-step <Emphasis Type="Italic">in situ</Emphasis> hydrothermal synthesis

High selectivity silicalite-1 membranes were synthesized on silica tubes by in situ hydrothermal synthesis. Using a two-step synthesis, a membrane with a separation factor of 99 was prepared for separating an ethanol/water mixture at 60°C. The average (n = 4) flux and separation factor of the membranes were 0.47 kg m-2 h-1 and 89, respectively. The membranes exhibited high reproducibility, and the relative standard deviation of the average (n = 4) flux and separation factor were only 5.3% and 9.2%, respectively. These results suggest that silica is a suitable support for synthesis of high-performance silicalite-1 membranes.     

A novel Pd/silicalite-1 composite membrane for hydrogen separation

A novel Pd/silicalite-1 composite membrane supported on the macroporous tubular stainless steel substrate was successfully fabricated by electroless plating at 303 K. The structure, morphology and gaseous permeability of the membrane were detected by X-ray diffractiometry （XRD）, scanning electron microscopy （SEM） and single-gas permeation test, respectively. Results confirm the formation of a thin, smooth, and continuous Pd/silicalite-1 composite membrane. The obtained composite membrane shows a high H2 permeance of 1.15×10^-6 mol. m^-2. s^-1. Pa^-1 with moderate H2 selectivity of 250 for H2/N2 at 773 K, at 0.1 MPa pressure drop, suggesting the potential application for H2 separation.     

Styrene polymerization catalyzed by nickel complexes bearing hydroxyindanone-iminate ligands

Activated by methylaluminoxane, mononuclear bis（hydroxyindanone-iminate）nickel complexes Ni[ArN=CC2H3（CH3）C6H2（R）O]2 （Ar = 2,6-i-Pr2C6H3, R=Me（1）, R=CI（2）, and R=H（3）） showed good activity for the styrene polymerization. The effect of many reaction parameters including the AI/Ni ratio, temperature, and reaction time on catalytic activities of catalytic systems and the molecular weights of the obrained polystyrene was ascertained. The highest activity of 1.34×10^5g（PS）·mol^-1（Ni）·h^-1 was obtained under the optimum reaction condition. The ^13C NMR spectra of the polymers revealed that the polymer was isotactic-rich atactic polystyrene. And the coordination mechanism was confirmed by the analyses of the polymer chain end-groups.     

Investigation on the coordinate structures of the rare earth metal complexes with edta and cydta ligands

0　IntroductionThegreatattentionhasbeenpaidtorareearthorradioactiverareearthmetalcomplexesfortheirvariousbiologicactivi ties[1 3] .Forexamples,theradioactiverareearthmetal1 53SmⅢ com plexeswerewidelyusedfortumourtherapyofbrain ,liver,lung ,heartandbonetissues[4 5] ;forrareearthmetalEuⅢandTbⅢemitinguniquefluorescence ,theircompoundswereappliedfordiagnosesofvariousdiseases[6 ,7] ;forrareearthmetalGdⅢcontainingthemosthigh spinsingleelectrons,itscomplexeswereusuallyusedforcontrastagentsofmag…     

Coordination behavior between zinc salts and L-α-methionine

The solubility properties of ZnCl\-2/ZnAc\-2/ZnSO\-4_Met_H\-2O systems at 25℃ in the whole cocentration range have been investigated by phase equilibrium method. The results indicate that ZnAc\-2 and ZnSO\-4 systems are both simple systems, which do not exist any compound; there are 2 complexes formed in ZnCl\-2 system: Zn(Met)Cl\-2 and Zn(Met)\-2Cl\-2·2H\-2O. Under the direction of phase equilibrium result, 2 solid complexes have been prepared in water and characterized by chemical analysis, IR, X_ray diffraction. Their combustion energies have also been determined by means of a RBC_type_1 rotating_bomb calorimeter, and their standard enthalpies of formation, Δ f, coor(s)H O-, have been calculated which are (-828.32±3.00) kJ·mol -1 and (-1 117.08±6.15) kJ·mol -1, respectively.     

Preparation and performance of LiNi0. 8Co0.2O2 cathode material based on Co-substituted α-Ni（OH）2 precursor

Co-substituted α-Ni（OH）2 was synthesized by a novel microwave homogeneous precipitation method in the presence of urea. LiNi0.8Co0.2O2 cathode material was synthesized by calcining Co-substituted α-Ni（OH）2 precursor and LiOH·H2O at 900℃for 10 h in flowing oxygen. XRD, FTIR, FESEM and electrochemical tests were used to study the physical and the electrochemical performances of the materials. The results show that the prepared LiNi0.8Co0.2O2 compound has a good layered hexagonal structure. Moreover, the LiNi0.8Co0.2O2cathode material demonstrates stable cyclability with a high initial specific discharge capacity of 183.9 mAh/g. The good electrochemical performance could be attributed to the uniform distribution of Ni^2＋ and Co^2＋ ions in the crystal structure and a minimal cation mixing in LiNi0.8Co0.2O2 host structure.     

A new type of longitudinally driven GMI effect of FeCo-based alloy

On investigating the longitudinally driven GMI effect of the DC annealed Fe36Co36Nb4Si4.8B19.2 alloy ribbon, the current density was 3.2×10^7 A/m^2, the GMI effect responds sensitively （the sensitivity is as high as 2440.2%/（A-m^-1）） to weak magnetic field after a 600-second annealing. The experimental result shows that the sensitivity is closely related to annealing current density, driven current frequency and eroded thickness. GMI effect, current annealing, sensitivity, magnetic domain structure     

The v-v energy transfer of highly vibrationally excited states (II)

The vibrational energy transfer from highly vibrationally excited CO to H₂O molecules is studied by time-resolved Fourier transform infrared emission spectroscopy (TR FTIR). Following the 193 nm laser photolysis of CHBr₃ and O₂ the secondary reactions generate CO(v). The infrared emission of CO(v → v−1) is detected by TR FTIR. The excitation of H₂O molecules is not observed. By the method of the spectral simulation and the differential technique, 8 rate constants for CO(v)/H₂O system are obtained: (1.7 ±0.1), (3.4 ±0.2), (6.2 ±0.4), (8.0 ±1.0), (9.0 ±2.0), (12 ±3), (16 ±4) and (18 ±7) (10¹³cm³ · molecule^-1· s^-1). At least two reasons lead to the efficient energy transfer. One is the contributions of the rotational energy to the vibational energy defect and the other is the result of the complex collision. With the SSH andab initio calculations, the quenching mechanism of CO(v) by H₂O is suggested.     

Direct electrochemistry and electrocatalysis of horseradish peroxidase in MnO2 nanosheet film

A novel material MnO2 nanosheet has been used as the support matrix for the immobilization of horseradish peroxidase （HRP）. HRP entrapped in MnO2 nanosheet film exhibits facile direct electron transfer with the electron transfer rate constant of 6.86 s^-1. The HRP/MnO2 nanosheet film gives a reversible redox couple with the apparent formal peak potential （E^0＇） of -0.315 V （vs. Ag/AgCl） in pH 6.5 phosphate buffer solution （PBS）. The formal potential E^0＇ of HRP shifts linearly with pH with a slope of -53.75 mV.pH^-1, denoting that an electron transfer accompanies single-proton transportation. The immobilized HRP shows an electrocatslytic activity to the reduction of H2O2. The response time of the biosensor for H2O2 is less than 3 s, and the detection limit is 0.21 μmol · L^-1 based on signal/noise = 3.     

新的糖/茂钛化合物的合成及其生物活性研究

用4种含糖基团取代二氯化二茂钛中的氯,合成了4种新的糖/茂钛化合物:乳糖酸根一氯化二茂钛C12H21O12.C10H10TiCl,质酸根一氯化二茂钛C14H20NO11.C10H10TiCl.8H2O,乳糖酸根一质酸根二茂钛C12H21O12.C14H20NO11.C10H10Ti.26H2O和乳糖酸酰胺乙酸根一氯化二茂钛C14H24NO13C10H10TiCl.化合物都经过红外光谱、核磁共振、元素分析表征,并用MTT法研究了化合物对人体子宫颈癌细胞增殖体外实验.研究表明新合成的化合物都溶于水,对癌细胞有很好的抑制作用,糖结构的引入有明显的肝靶向效应.     

制药废水膜法深度处理通量变化研究

为了深度处理制药废水,达到工业用水水质标准,对纳滤、反渗透深度处理综合性制药废水的膜通量变化进行了研究。在连续式与循环式处理模式下,研究了膜操作条件、膜通量和水回收率等因素,根据膜通量变化,确定了适合膜分离工业化应用的处理和清洗方案。结果表明：纳滤膜日常清洗中物理清洗时间为7 min、强化清洗酸洗—碱洗时间各为90 min,平均膜通量连续式为16.1 L/(m²·h)、循环式为7.7 L/(m²·h),水回收率约为73%;反渗透膜日常清洗中物理清洗时间12 min、强化清洗酸洗—碱洗时间各90 min,平均膜通量连续式为12.8 L/(m²·h)、循环式为7.2 L/(m²·h),水回收率约为74%。研究制药废水深度处理中膜通量的变化,可对制定适合膜分离工业化应用的废水处理和清洗方案提供借鉴和参考。     

Preparation of three-dimensionally ordered macroporous perovskite materials

In this paper,we use La0.8Sr0.2MnO3 and La0.7Ca0.2Sr0.1MnO3 as examples to demonstrate a preparation method for threedimensionally ordered macroporous(3DOM) perovskite thermochromic materials.Polystyrene spheres with an average diameter of 220 nm were self-assembled into a three-dimensionally ordered colloidal crystal template.A mixed metal nitrate solution prepared using La(NO3) 3·6H2O,Ca(NO3) 2·4H2O,Sr(NO3) 2,Mn(CH3COO) 2·4H2O and an ethanol precursor was used to fill the interstitial voids of the polystyrene colloidal crystal templates.3DOM La0.8Sr0.2MnO3 and La0.7Ca0.2Sr0.1MnO3 materials were then obtained after the sphere templates were removed via drying and calcination.The results show that the framework of the 3DOM materials can have different thicknesses and pore shrinkage rates by varying the filling times.In addition,the Curie temperatures of the 3DOM and bulk La0.8Sr0.2MnO3 materials can be varied by altering the preparation method.     

Standard molar enthalpy of formation of morin studied by rotating-bomb combustion calorimetry

Flavonols are plant pigments that are ubiquitous in nature. Morin and other related plant flavonols have come into recent prominence because of their usefulness as anticancer, anti-tumor, anti-AIDS, and other important therapeutic activities of significant potency and low systemic toxicity. The heat of combustion of morin (molecular formula, C₁₅H₁₀O₇·H₂O) in oxygen was measured by a rotating-bomb type combustion calorimeter, the standard molar enthalpy of combustion of morin at T = 298.15 K was determined to be Δ_c H _m^⦵ (C₁₅H₁₀O₇·H₂O, s) = −(5 937.99 ± 2.99) kJ · mol⁻¹. The derived standard molar enthalpy of the formation of morin in solid powder state at T = 298.15 K, Δ_f H _m^⦵ (C₁₅H₁₀O₇·H₂O, s), was −(1 682.12 ± 3.58) kJ · mol⁻¹, which provide an accurate data of the stability of morin to the pharmacy and pharmacology. Biography: HOU Hanna(1956–), female, Visiting researcher, Associate professor of Hubei University of Education, research direction: thermochemistry.     

Icariin suppresses bone resorption activity of rabbit osteoclasts in vitro

The effect of icariin on the bone resorption activity of rabbit osteoclasts is assessed in vitro. Osteoclasts were isolated from Japanese white rabbits and cultured on plates with a sterilized bone slice in each well. After treatment with icariin at various concentrations, the bone resorption activity of osteoclasts was evaluated by examining pit areas, superoxide anion (·O2-) generation, size and number of actin rings and intracellular calcium concentration [Ca2 ]i. As revealed by these data, icariin elicited continuous decline of [Ca2 ]i, making actin ring constricted and ·O2- generation decreased. These events resulted in smaller and fewer pits which indicate suppressed bone resorption activity of rabbit osteoclasts by icariin.     

C-H···Pd(II) interaction-driven homochiral M helix formation of neutral (R,R)-bis(pyrrol-2-ylmethyl- eneamino) cyclohexane palladium(II) complex

A chiral complex of (R,R)-Pd was prepared by reaction of optically pure (R,R)-bis(pyrrol-2-ylmethyl-eneamino) cyclohexane ligand with Pd(OAc)2·2H2O under the base condition at room temperature. The weak intermolecular C-H···Pd interaction was found to be responsible for the homochiral M helix for-mation of the neutral,chiral,mononuclear (R,R)-Pd in the crystal packing.     

Modification of TiO2 nanotubes arrays by CdS and their photoelectrocatalytic hydrogen generation properties

In order to realize hydrogen generation under visible light, novel CdS/TiO2 nanotubes arrays are developed by electrochemical anodizaUon of Ti in 0.15 mol/L NHTF ＋ 0.08 mol/L H2C2O4 electrolyte. The diameter of the nanotube is 80-100 nm and the length is approximately 550 nm. The CdS nano-particles are deposited on the TiO2 nanotubes arrays by chemical bath deposition （CBD） in the ammonia-thiourea system. A 300 W Xe lamp is used as the light source, CdS/TiO2 nanotube arrays are used as the photoanode with the application of 1.0 V bath voltage, and 0.1 mol/L Na2S ＋ 0.04 mol/L Na2SO3 solution is used as the electrolyte, then the rate of photoelectrocatalytic hydrogen generation is 245.4 μL/（h·cm^2）. This opens new perspectives for photoelectrocatalytic hydrogen generation by using CdS/TiO2 nanotubes arrays.     

Crystallization kinetics of sea-salt aerosols studied by high-speed photography

Morphological changes with decreasing relative humidity(RH) of supersaturated sea-salt aerosol droplets on a quartz substrate were observed using a high-speed video-camera.Stable gypsum(CaSO4·2H2O) or the metastable hemihydrate(CaSO4·0.5H2O) were precipitated as the RH decreased.The dynamic process of crystal growth under steady-state humidity was studied by controlling the RH;the metastable hemihydrate was precipitated at 70.5%-77.1% RH,and the apparent crystal growth rate was between 1.42 and 2.33 μm3/s.Stable gypsum was formed at 80.7%-82.2% RH,and the apparent crystal growth rate was between 0.70 and 0.81 μm3/s.     

Solvothermal synthesis of CdS nanorods and photovoltaic characteristics of CdS/PVK composite system

Large quantities of CdS nanorods are successfully synthesized through Cd（CH3COO）2·2H2o reacting with Na2S·9H2O and EDA in aqueous solution. XRD result shows that the sample is of hexagonal structure. And TEM result shows that the morphologies of the resulting CdS are mainly in three-armed rod-like structure with a diameter of 10--15 nm and a length of 100 nm. The nanocomposites of CdS/PVK with different molar ratios are prepared by spin coating method on tin-doped indium oxide （ITO） substrate. A notable decrease of photoluminescence （PL） efficiency and a significant enhancement of surface photovoltage signal have been observed in CdS/PVK composites when the molar fraction of CdS increases. We interpret these results as the energy level matching between CdS and PVK in nanocomposites. This energy level matching facilitates fast interfacial charge transfer then increases the separation efficiency of electron-hole pairs and the carrier generation efficiency. The detailed charge transfer process has also been demonstrated.     

冷凝液硫含量对SUS444铁素体不锈钢腐蚀行为的影响

利用冷凝液浸蚀-高温氧化循环腐蚀法模拟汽车排气系统内部服役环境,借助失重分析、腐蚀形貌观察及腐蚀产物分析,研究了SUS444不锈钢在不同硫含量的冷凝液中的腐蚀行为。结果表明,随着腐蚀循环次数的增加,不锈钢表面不断沉积的FeSO_4·7H_2O、Fe(NH_4)(SO_4)_2及Fe_4(SO_4)_5(OH)_2·18H_2O等硫酸盐物质加速了不锈钢的腐蚀进程,其点蚀深度及腐蚀速率均随冷凝液中硫含量的升高而增加。     

Measurement of the Newtonian gravitational constant based on the principle of free fall

The Newtonian gravitational constant (G) is one of the fundamental physical constants. This paper introduces a method to determine the Newtonian gravitational constant based on the principle of free fall, through measuring the change of gravity from the disturbed mass with an FG5/112 absolute gravimeter. This method has good repeatability. The measurement precision can be improved by error control and a large number of experiments. The constant G is obtained by two experiments, and the measured value is (6.6665±0.0554)×10⁻¹¹ m³/(kg·s²). Supported by the National Basic Research Program of China (Grant No. 2003CB716300) and Key Project of the Knowledge Innovation Program of the Chinese Academy of Sciences (Grant No. KZCX2-YW-125)