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01 June 2015, Volume 31 Issue 3

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Chemical Research in Chinese Universities Vol.31 No.3 February 2015

2015, 31(3):  0-0. 

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Letter

2-Hydroxymalonitrile-A Useful Reagent for One-step Synthesis of α-Hydroxy Esters

YANG Jianxin, YIN Yunxing, HE Zhenmin, MA Li, LI Xin, ZHANG Zhiliu, LIN Xiaojuan, MA Rujian

2015, 31(3):  321-324.  doi:10.1007/s40242-015-4495-6

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An efficient one-pot synthesis of α-hydroxy esters by employing the useful reagent 2-hydroxymalononitrile reacting with an aldehyde or ketone in just one step has been reported.



Articles

Synthesis of Zn-containing Aluminophosphate with ERI Topology

DUAN Fangzheng, LIU Lingzhi, QIAO Chunyu, YANG Huimin, CHEN Peng

2015, 31(3):  325-327.  doi:10.1007/s40242-015-5013-6

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A Zn-containing aluminophosphate with ERI-zeotype structure was hydrothermally synthsized with 1,2-diaminocyclohexane(DACH) as the template. The result of the structural analysis indicates that the Zn-containing aluminosphate crystallized in the hexagonal space group of P6₃/m was constituted up by the alternating Al(Zn)O₄ and PO₄ tetrahedra. The organic amine DACH located in the ERI cages was used to balance the negative charge of the framework.



Structure and Fluorescence Property of a Two-fold Interpenetrated Three-dimensional Zn(II) Complex Constructed by Terephthalate and 1,3-Dipyridyl Benzene

XU Jingyao, ZHANG Lei, SHAO Xueman, PAN Chengling, XU Jiqing

2015, 31(3):  328-331.  doi:10.1007/s40242-015-4433-7

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A new coordination polymer {[Zn₂(dpb)₂(bdc)₂]·1.3H₂O}_n(1) was prepared under solvothermal condition using terephthalate(1,4-H₂bdc) as well as 1,3-dipyridyl benzene(1,3-dpb) as initiators. The complex was characterized by means of infrared spectroscopy(IR), thermogravimetric analysis(TGA), powder X^-ray diffraction(XRD) and X^-ray single-crystal diffraction. The results indicate that complex 1 crystallizes in the monoclinic system with space group of P2₁/c. The neighboring Zn(II) ions are linked by ligand dpb to form infinitely meso-helical or zigzag chains, which are further connected to form a two-fold interpenetrated 3D framework, in which there exists strong hydrogen bonds(O-H…O) between the interpenetrated frameworks. In addition, the solid-state fluorescence behavior of complex 1 was also discussed.



Preparation of TiO₂ Nanoflakes and Their Influence on Lithium Ion Battery Storage Performance

LI Yi, HAN Xiangbo, LIANG Jicai, LENG Xuning, YE Kaiqi, HOU Changmin, YU Kaifeng

2015, 31(3):  332-336.  doi:10.1007/s40242-015-4421-y

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TiO₂ nanoflakes were prepared by hydrothermal precipitation method using Ti(SO₄)₂ as titanium source and NaOH solution as alkaline medium. Their surface morphology, grain size measured after high temperature calcination and effect on the electrochemical performance of Li ion battery were discussed. TiO₂ nanoflakes were characterizated by means of transmission electron microscopy(TEM), X^-ray powder diffraction(XRD), N₂ adsorption-desorption isothermal assay, cyclic voltammetry(CV) and cycle performance test. The result of electrochemical performance test shows that the prepared TiO₂ nanoflakes have high discharge specific capacity and good cycle performance. Discharge specific capacity for the first circle at the discharge rate of 0.1 C is 261.5 mA·h·g^-1. After 90 cycles, the discharge capacity reduces to 172.2 mA·h·g^-1.



Two New Inorganic-organic Hybrid Compounds Constructed from Different Polymolybdates and Transition Metal-amine Subunits

WANG Xiuli, LIU Danna, HAN Na, LIN Hongyan, LUAN Jian, TIAN Aixiang

2015, 31(3):  337-341.  doi:10.1007/s40242-015-4386-x

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Two new polyoxometalate(POM)-based hybrid compounds, [Cu(en)][H₄Mo₄O₁₆]_0.5(1)(en=ethylene- diamine) and [Ag(3-C₅H₆N₂)₂][H₂PMo₁₂O₄₀](2)(3-C₅H₆N₂=3-aminopyridine), containing different transition metal-amine subunits were hydrothermally synthesized and characterized by elemental analyses, infrared spectroscopy and single-crystal X^-ray diffraction. For compound 1, each [H₄Mo₄O₁₆]^4-(Mo₄O₁₆) cluster was linked to four neighboring Mo₄O₁₆ clusters through four [Cu(en)]²⁺ subunits to yield a (2,4)-connected 2D layer, which was further extended to a 3D supramolecular network via hydrogen bonding interactions. For compound 2, the adjacent [H₂PMo₁₂O₄₀]^- clusters were bridged by [Ag(3-C₅H₆N₂)₂]⁺ subunits to generate a 1D chain. The electrochemical behaviors and the photocatalytic activities of compounds 1 and 2 were studied in detail.



Low Temperature Molten Salt Synthesis of Perovskite-type ACeO₃(A=Sr, Ba) in Eutectic NaCl-KCl

LIU Ming, HU Lei, XU Pengfei, ZHAO Kun, ZONG Lingbo, YU Ranbo, CHEN Jun, XING Xianran

2015, 31(3):  342-346.  doi:10.1007/s40242-015-4330-0

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A molten salt method was developed for the synthesis of ACeO₃(A=Sr, Ba) with perovskite structure at 750 ℃(SrCeO₃) and 850 ℃(BaCeO₃) in the eutectic NaCl-KCl. The synthetic temperature was much lower than that of the conventional method(generally>1000 ℃). The structure and morphology of the product were characterized by means of X^-ray diffraction(XRD), field emission scanning electron microscopy(FESEM) and transmission electron microscopy(TEM). The results show that the synthesized octahedral SrCeO₃ crystallizes in the orthorhombic system with the unit cell parameters of a=0.85855 nm, b=0.61523 nm, c=0.60059 nm, and the synthesized cuboid BaCeO₃ crystallizes in the cubic system with the unit cell parameter of a=0.43962 nm. The result of X^-ray photoelectron spectroscopy(XPS) analysis indicates that both Ce⁴⁺ and Ce³⁺ exist in the two structures, and the Ce⁴⁺/Ce³⁺ peak area ratios for SrCeO₃ and BaCeO₃ are 1.93 and 2.12, respectively. Meanwhile, the adsorbed/lattice oxygen ratios(1.87 for SrCeO₃ and 3.04 for BaCeO₃) indicate the existence of a lot of oxygen vacancies in the structures of SrCeO₃ and BaCeO₃, which indicates a far-reaching significance to study the corresponding physicochemistry performance.



A Highly Selective Fluorescent Chemosensor for Cu²⁺

GUAN Jie, ZHANG Peng, WEI Taibao, LIN Qi, YAO Hong, ZHANG Youming

2015, 31(3):  347-351.  doi:10.1007/s40242-015-4403-0

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A new Zn²⁺ probe L2-Zn(L2=naphthofuran carbonylhydrazone derivant) was synthesized as a fluorescence chemosensor for Cu²⁺, by which Cu²⁺ ion could be detected with high selectivity and sensitivity in a wide pH range via a displacement “turn-off” signaling strategy. Whereas the coordination between Zn²⁺ and L2 resulted in a considerable enhancement of typical luminescence of a naphthalofuran group in complex L2-Zn, the addition of Cu²⁺ ion led to a dramatic decrease in the emission intensity of probe L2-Zn at about 503 nm(excitation at 423 nm). The competitive fluorescent experiments showed that other metal ions, such as Hg²⁺, Fe³⁺, Ag⁺, Ca²⁺, Co²⁺, Ni²⁺, Cd²⁺, Pb²⁺, Zn²⁺, Cr³⁺ and Mg²⁺ could not impact the detection of Cu²⁺. The detection limit of the novel probe L2-Zn for Cu²⁺ ion was as low as 2.3×10^-7 mol/L, which is far lower than the guideline value of 1.6×10^-5 mol/L of the United States Environmental Protection Agency.



Evaluation of Oil Yield of Oil Shale by Infrared Spectrometry Coupled with Ultrasound-assisted Extraction

ZHAO Zhenying, LIN Jun, YU Yong, HOU Chuanbin, SUN Yuyang

2015, 31(3):  352-356.  doi:10.1007/s40242-015-4364-3

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The oil yield of oil shale was evaluated by Fourier transform infrared(FTIR) spectrometry coupled with ultrasound-assisted extraction. The extraction conditions, including the amount of sample, extraction time and extraction temperature, were examined and optimized. Twenty-four oil shale samples were collected and divided into calibration set and prediction set randomly with a ratio of 2:1. The oil yields of all the samples were determined by the routine method(low-temperature retorting) for reference. The linear regression(LR) equations of oil yield vs. the total area of the spectrum peaks in a wavenumber range of 3100-2800 cm^-1 as well as the sum of absorbance of three absorption peaks(2855, 2927 and 2955 cm^-1), and the multiple linear regression(MLR) model of oil yield vs. the absorbances of the three absorption peaks were constructed with the samples in calibration set and applied to the evaluation of the oil yields of the samples in prediction set, respectively. The results show that the MLR model provides more accurate predictions than the other LR two equations. The determination coefficient(R_p²), the root-mean-square error of prediction(RMSEP) and the residual prediction deviation(RPD) of the MLR model are 0.9616, 0.6458 and 3.6, respectively. The present method is a rapid and effective alternative to the routine low-temperature retorting method.



Synthesis and Photochromism of Novel Spiro(indoline-2,3'-naphtho[2,1-b][1,4]oxazine)

LI Hong, PANG Meili, GUO Xinfu, MENG Jiben

2015, 31(3):  357-361.  doi:10.1007/s40242-015-4482-y

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A series of novel spirooxazine(SPO) derivatives containing nitrogen heterocycles was synthesized and characterized by ¹H NMR spectra, Fourier transform infrared(FTIR) spectra, mass spectra(MS) and elemental analysis, and their photochromic behaviors were fully investigated in solvents and polymer media. In solvents, they displayed excellent photochromism properties such as high photochromic response and fast thermal bleaching rate. Especially, compounds 1 and 4 exhibited strong fluorescence intensities in dichloromethane solution. It was additionally found that compound 4 showed high fatigue resistence in poly(methyl methacrylate)(PMMA) film, and the thermal decay curves were fitted with biexponential function in PMMA film.



Difluoromethylation of 2-Hydroxychalcones Using Sodium 2-Chloro-2,2-difluoroacetate as Difluoromethylating Agent

WANG Wei, HUA Mingqing, HUANG Yan, ZHANG Qi, ZHANG Xiaoyan, WU Jingbo

2015, 31(3):  362-366.  doi:10.1007/s40242-015-4456-0

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Difluoromethylation of 2-hydroxychalcones using sodium 2-chloro-2,2-difluoroacetate as the difluoro-methylating agent was developed. Under facile conditions, a wide range of aryl difluoromethyl ethers were obtained in yields of 36%-80%. It is noteworthy that the new addition products, 2,2-difluoro-2H-benzofuran derivatives, were also synthesized in the reactions. The yield of 2,2-difluoro-2H-benzofuran derivative could be up to 35% when 3-methyl-2-hydroxychalcone was used as the reactant. A plausible reaction mechanism was proposed.



Synthesis and Biological Evaluation of Novel Uracil and 5-Fluorouracil-1-yl Acetic Acid-Colchicine Conjugate

SHEN Lihong, HU Junping, WANG Haixian, WANG Aibing, LAI Yisheng, KANG Yanhui

2015, 31(3):  367-371.  doi:10.1007/s40242-015-4445-3

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A series of novel uracil and 5-fluorouracil-1-yl-acetic acid-colchicine derivatives(6a-6n) was synthesized via coupling uracil and 5-fluorouracil(5-FU) with C-10 analogues of colchicine. The antitumor activities of the target compounds against human hepatocellular carcinoma(BEL7402) cells, human ovary carcinoma(A2780) cells, human lung adenocarcinoma(A549) cells and human breast carcinoma(MCF7) cells were tested in vitro, and the structure-activity relationship(SAR) of the compounds was also studied. The bioassay results demonstrate that most of the tested compounds display significant activity and particularly, compounds 6a, 6e, 6h and 6l show more potent cytotoxic activities than 5-fluorouracil and colchicine. The results show that the new derivatives of colchicine are potential suppressors on human cancer.



Discovery of Novel Tricyclic 5H-Pyridazino[4,5-b]indoles as Potent Antitumor Agents: Design, Synthesis and Biological Evaluation

ZHAI Xin, WANG Limei, SHI Jiyue, GONG Ping

2015, 31(3):  372-380.  doi:10.1007/s40242-015-4435-5

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A novel series of 5H-pyridazino[4,5-b]indoles(L-01-L-32) was synthesized and characterized by means of ¹H NMR, MS and elemental analysis. The cytotoxicity of the target compounds against Bel-7402 and HT-1080 cell lines were evaluated by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide(MTT) assay. Most of them exhibited moderate to excellent cytotoxicity, and six compounds(L-04, L-06, L-18, L-20, L-21 and L-23) possessed dramatically increased cytotoxicity superior to Gefitinib. Of these initial hits, compound L-21 displayed remarkable cytotoxicity against the tested cell lines with half maximal inhibitory concentration(IC₅₀) values of 4.6 and 2.1 μmol/L, respectively, which was 13.9- to 25.6-fold more potent than positive control.



Synthesis and Secondary Conformations of Homochiral β-Oligopeptides Containing Aryl Side Chains

ZHANG Yonghong, LI Liangchun, YUAN Weicheng, ZHANG Xiaomei

2015, 31(3):  381-387.  doi:10.1007/s40242-015-4423-9

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A series of novel homochiral β-oligopeptides bearing aryl side chains was designed and synthesized from (S)-β-phenyl-β-amino acid derivatives by solution-phase methods. By means of circular dichroism(CD), Fourier- transform infrared spectrometry(FTIR), powder X^-ray diffraction analysis(XRD) and density functional theory(DFT) calculations, we suggest that dipeptide P-2 and tripeptide P-3 adopt random coil-like conformations, pentapeptide P-5 and hexapeptide P-6 adopt stable 12-helix conformations in both solution and solid-state. Meanwhile, tetrapeptide P-4 adopt random coil-like conformation in solution and adopt 12-helix conformation in solid state.



Design, Synthesis and Biological Evaluation of Sulfenimine Cephalosporin Analogues as β-Lactamase Inhibitors

ZHANG Kai, DING Huaiwei, SHI Ailong, HUANG Qi, SONG Hongrui, FU Decai

2015, 31(3):  388-393.  doi:10.1007/s40242-015-4413-y

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A series of sulfenimine cephalosporin derivatives(6a-6t) was designed, synthesized and evaluated for their inhibitory activity against class A β-lactamase(TEM-1) derived from E. coli, and class C β-lactamase (cephalosporinase) derived from wild Bacillus subtilis in cell-free systems. Most of the tested compounds showed enhanced inhibitory activity against class C β-lactamase(cephalosporinase) compared with tazobactam. The most promising compounds 6c and 6o in combination with cefradine(IC₅₀=1.80 and 1.59 μmol/L, respectively) were further investigated against a series of clinical isolated β-lactamase-producing bacterial strains. The results reveal that compounds 6c and 6o in combination with cefradine show two to four times more activity than cefradine alone against methicillin-sensitive Staphylococcus aureus(MSSA) and Klebsiella pneumoniae. The data suggest that the sulfenimine moiety may be beneficial to the activity and selectivity of inhibitors.



Design, Synthesis and Anticancer Activity of Shikonin and Alkannin Derivatives with Different Substituents on the Naphthazarin Scaffold

ZHANG Xu, CUI Jiahua, ZHOU Wen, LI Shaoshun

2015, 31(3):  394-400.  doi:10.1007/s40242-015-4385-y

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Based on the asymmetric reduction of alkannin ketone derivative 4 by diisopinocampheylchloro-borane(DIP-Cl), a series of shikonin and alkannin derivatives was designed, synthesized and their anticancer activities against various kinds of cell lines were evaluated. The in vitro biological experiments demonstrated that compound S-10, a 5,8-O-dimethyl-1,4-dioxime alkannin derivative, not only displayed excellent antiproliferative activity against cancer cells, but also exhibited low toxicity towards normal cells. It could induce HCT-116 cell apoptosis, but had no impact on the cell cycle. The underlying anticancer mechanism of S-10 is most likely different from other shikonin and alkannin derivatives.



Enhanced Survivin siRNA Delivery Using Cationic Liposome Incorporating Fatty Acid-modified Polyethylenimine

YANG Shuang, GUO Zhihua, YANG Xuewei, XIE Jing, Robert J. LEE, JIANG Dan, TENG Lesheng

2015, 31(3):  401-405.  doi:10.1007/s40242-015-5060-z

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We described a novel approach for survivin siRNA cellular delivery via a cationic liposome incorporating fatty acid-modified polyethylenimine. A linoleic acid derivative of branched polyethylenimine(PEI, M_w=25 kDa), PEI-LA, was synthesized and incorporated into the liposome. The properties of the liposome, cytotoxicity, cellular uptake of cancer cells for survivin siRNA, survivin protein downregulation levels were investigated. PEI-modified liposome showed a lower cytotoxicity and delivered survivin siRNA into HeLa cells and A549 cells efficiently compared with PEI-25kDa.



DNA Induced FePt Bimetallic Nanoparticles on Reduced Graphene Oxide for Electrochemical Determination of Dopamine

ZHANG Wenyan, LIU Yang

2015, 31(3):  406-411.  doi:10.1007/s40242-015-4515-6

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FePt bimetallic nanoparticles were formed on reduced graphene oxide(rGO) with the help of double-stranded DNA(dsDNA) via a simple and universal route to obtain a FePt/DNA-rGO composite. The FePt nanoparticles with an average size of about 5 nm were well dispersed on rGO. FePt/DNA-rGO modified glassy carbon electrode(GCE) exhibited excellent electrocatalytic activity for the oxidation of dopamine(DA) with a detection limit of 100 nmol/L(S/N = 3). In addition, the FePt/DNA-rGO based electrochemical sensor showed an excellent selectivity for DA in the presence of ascorbic acid(AA), uric acid(UA) and other interference reagents. The as-prepared electrochemical biosensor shows great promise in the application of clinical diagnostics.



Bilayer Structured Nanowire-array and Nanotube-cluster TiO₂ Photoanode for Efficient Dye-sensitized Solar Cells

YU Jun, ZHANG Chengkai, ZHUANG Jia, QIN Haiyang, HE Quangui, LIANG Qiumei

2015, 31(3):  412-417.  doi:10.1007/s40242-015-5003-8

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Nanowire-array nanotube-cluster bilayer TiO₂ films, consisting of nanowire-array at the bottom layer and nanotube-cluster at the top layer were prepared via a two-step hydrothermal method. One step was a growth process and the other was an etching process. Etching process was used to acquire nanowire-array with a small diameter of 20-25 nm of the nanowire and nanotube-cluster. The bilayer nanostructured films were then modified with TiCl₄. Villous TiO₂ attached to both the inside and outside walls of the nanotube cluster was obtained only by changing the traditional concentration of TiCl₄-treatment to 0.2 mol/L. The novel bilayer photoanode finally revealed a higher efficiency of 5.25% when used in dye-sensitized solar cells(DSSCs).



Electric Field-driven Acid-base Transformation: Proton Transfer from Acid(HBr/HF) to Base(NH₃/H₂O)

LIANG Hailong, CHAI Baojie, CHEN Guanghui, CHEN Wei, CHEN Sheng, XIAO Hailan, LIN Shujuan

2015, 31(3):  418-426.  doi:10.1007/s40242-015-4464-0

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The proton-transfer between ammonia/water and HF/HBr without and with the stimulus of external electric fields(E_ext) was investigated with the ab initio calculations. When external electric field is applied, the proton transfer occurs, resulting in ion-paired H₄N⁺X^- and H₃O⁺X^-(X=Br and F) from hydrogen-bonded complexes in view of the great changes of geometrical structures, dipole moments, frontier molecular orbitals and potential energy surfaces in the critical external electric fields(E_c) of 1.131×107 V/cm for H₃N-HBr, 1.378×108 V/cm for H₃N-HF, 9.358×107 V/cm for H₂O-HBr and 2.304×108 V/cm for H₂O-HF, respectively. Furthermore, one or three excess electrons can trigger the proton transfer from H₃N-HBr and H₃N-HF to H₄N⁺Br^- and H₄N⁺F^-, while two and four excess electrons can induce the proton transfer from H₂O-HBr and H₂O-HF to H₃O⁺Br^- and H₃O⁺F^-, respectively. Compared with that of the analogous NH₃/H₂O-HCl systems, the strength of E_c of proton transfer increases from HBr to HCl and HF for either H₃N-HX or H₂O-HX series, which is understandable by the fact that the acidity sequence is HBr>HCl>HF. And the larger of acidity of conjugated acid, the smaller of needed E_c. On the other hand, the E_c for the systems of NH₃ with a stronger basicity is generally smaller than that of H₂O systems for the same conjugated acid.



Long Lasting Phosphorescence Properties and Multi-peak Fitting on Thermoluminescence of Red LaAlO₃: Eu³⁺ Phosphor

ZUO Yinyan, CHEN Xia, LIU Xiaobin

2015, 31(3):  427-429.  doi:10.1007/s40242-015-4460-4

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Red long lasting phosphorescence(LLP) was firstly observed in LaAlO₃:Eu³⁺ phosphor synthesized by solid state method at 1773 K. It reveals that the Eu³⁺ ions occupy the asymmetric La³⁺ sites, resulting in the orange-red emission of Eu³⁺. The LLP of the optimum LaAlO₃:0.6%Eu³⁺ sample can come to about 2000 s according to a definition of 0.32 mcd/m². The LLP decay curve can not be fitted even by a function of three exponential terms, due to the complicated retrapping process of carriers. The result of a classical multi-peak fitting method on thermoluminescence reveals that the excellent LLP performance of LaAlO₃:Eu³⁺ material originates from the rich distribution of shallow traps(E=0.7875 eV).



Preparation of Magnetic TS-1 and Its Catalytic Activity

LI Yu, XUE Zehui, ZHANG Qi, SUN Cuitao, LI Junping, LIU Laishuan

2015, 31(3):  430-433.  doi:10.1007/s40242-015-4434-6

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Magnetic TS-1 was synthesized with nanosized nickelferrite particles as nuclei via the hydrothermal synthesis and solvent vaporation method. The prepared samples were characterized with N₂ adsorption-desorption isotherms, FTIR spectrometry, Raman spectrometry, X-ray diffraction, Ultraviolet-visible spectroscopy and Vibrating sample magnetometry. The results show that the composite obtained was composed of TS-1 with MFI structure and NiFe₂O₄ with spinel structure, its specific surface area was about 316 m²/g, pore volume was 0.12 cm³/g and pore size distribution was in the range of 0.5-0.7 nm. The catalytic activity of the composite was also investigated by its catalyzing the decomposition of rhodamine B oxidized by H₂O₂ in aqueous solution. In this case Rhodamine B pollutant could be completely degraded within 150 min. Magnetic TS-1 exhibited high photocatalytic efficiency and super paramagnetic nature for cleaning polluted water with the help of magnetic separation.



Flexible Triboelectric Nanogenerator from Micro-nano Structured Polydimethylsiloxane

XIAO Xinze, LÜ Chao, WANG Gong, XU Ying, WANG Jiping, YANG Hai

2015, 31(3):  434-438.  doi:10.1007/s40242-015-4432-8

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Triboelectric nanogenerator (TENG) can convert mechanical energy to electrical energy through contact electrification and electrostatic induction. Single-friction-surface triboelectric nanogenerator (STENG) extends potential application because a finger can be used as one friction surface in the contact electrification. In this work, a fully flexible STENG has been made, consisting of polydimethylsiloxane(PDMS) with micro-nano structures on its observe side and a flexible electrode on its reverse side. The femtosecond laser ablation was introduced to make micro-nano structures on PDMS and Ag nanowires (Ag NWs) were embedded in PDMS to serve as flexible induction electrode. It has been demonstrated that the energy conversion efficiency increases greatly because of the existing micro-nano structures on PDMS. Further, the mechanism of STENG was proved. Owing to the fully flexible characteristics in both the electrode and PDMS, STENG works well when it is adhered on any subject, for example, on clothes by tape.



Improved Visible-light Photocatalytic Properties of ZnFe₂O₄ Synthesized via Sol-gel Method Combined with a Microwave Treatment

FENG Jing, WANG Yuting, ZOU Linyi, LI Bowen, HE Xiaofeng, LIU Shengna, CHEN Tingting, FAN Zhuangjun, REN Yueming, LÜ Yanzhuo

2015, 31(3):  439-442.  doi:10.1007/s40242-015-4428-4

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ZnFe₂O₄(ZFO) was synthesized via a sol-gel method firstly, then the ZFO was irradiated with microwave treatment to obtain M-ZFO using NH₄Cl as dispersant for 10 min to improve the photocatalytic activity. Large particles of ZFO were broken into small and uniform particles by the gases of hydrogen chlorine and ammonia during the decomposition of NH₄Cl. Compared to ZnFe₂O₄ without microwave treatment(ZFO), M-ZFO exhibits smaller particle size, higher surface area and larger saturation magnetization. More importantly, the photocatalytic activity of M-ZFO for methylene blue was increased by 25% compared with that of ZFO.



A Facile Route to Synthesize Sheet-like Na₂Ti₃O₇ with Improved Sodium Storage Properties

XIE Man, WANG Kangkang, CHEN Renjie, LI Li, WU Feng

2015, 31(3):  443-446.  doi:10.1007/s40242-015-4422-x

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A high purity sheet-like Na₂Ti₃O₇ material was synthesized by a new facile solid-state method with hollow sphere TiO₂ as titanium source. X^-Ray diffraction(XRD) measurement proves that no impurity phase existed when the sample was heated at 900 ℃. Charge/discharge measurement was performed in a potential range of 0.01-2.5 V at different current-rates(C-rates). The initial charge/discharge capacities are 191/424 mA·h/g at 0.1 C and still remain as high as 101 mA·h/g after 50 cycles. CV test proves that the large irreversible capacity in the initial cycle results from the formation of the solid electrolyte interface(SEI). However, the electrode presents an increased initial coulombic efficiency in a 1 mol/L NaPF₆ electrolyte compared to that in a 1 mol/L NaClO₄ electrolyte.



Oxygen Electroreduction on CoSe₂ Nanoparticles Prepared via Hydrothermal Method in Acidic Medium

ZHAO Dongjiang, MA Songyan

2015, 31(3):  447-451.  doi:10.1007/s40242-015-4401-2

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CoSe₂ nanoparticles were synthesized via a facile hydrothermal method, and characterized by means of X^-ray diffraction(XRD), scanning electron microscopy(SEM) and transmission electron microscopy(TEM). The synthesized CoSe₂ was composed of crystalline orthorhombic phase and displayed a morphology of short and thin nanobelts. The results of the catalyst experiment demonstrate that the CoSe₂ nanocrystals show high catalytic activity and methanol tolerance in oxygen reduction reaction(ORR) with an open circuit potential(OCP) of 0.80 V(vs. NHE) in 0.5 mol/L H₂SO₂ at 25 ℃. The transfer process of about 3.7 electrons per oxygen molecule was determined during the reduction process and the transfer coefficient and Tafel slope were 0.50 and 118 mV, respectively, in the potential region of 0.64-0.75 V(vs. NHE). The high catalytic activity might be related to the high crystallization of the CoSe₂ powder and the modification of selenium on the cobalt element.



Thermal Characteristics of Room Temperature Inorganic Phase Change System Containing Calcium Chloride

GAO Daolin, GUO Yafei, YU Xiaoping, WANG Shiqiang, DENG Tianlong

2015, 31(3):  452-456.  doi:10.1007/s40242-015-4387-9

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A novel inorganic calcium-based phase change material(PCM-Ca) consisted of 47.1%(mass fraction) water, 47.7% calcium chloride, 2% potassium nitrate, 2% potassium bromide and 1.2% strontium chloride with a solid-liquid phase change temperature of 21.4 ℃ was investigated systematically. Among the components of PCM-Ca, calcium chloride and water act as the latent heat storage materials, and potassium nitrate, potassium bromide and strontium chloride work as the modifier, thickener and nucleating agent, respectively. Thermochemical properties including melting point, latent heat, density and thermal conductivity of the PCM-Ca were measured experimentally. The experimental results indicate that the melting latent heat, thermal conductivity at the melting point and density at room temperature for the PCM-Ca are 203.3 kJ/kg, 1.3637 W·m^-1·K^-1 and 1.55×103 kg/m³, respectively. Moreover, a thirty-run-cycling test showed that the PCM-Ca has a good thermal characteristic with no phase segregation or supercooling, and the maximum deviations of latent heat and phase change temperature are only 0.2% and 1.6%, respectively.



Effect of Nonmagnetic Impurity Doped on the Structural and Magnetic Properties of Quasi-one-dimensional Antiferromagnet LiCuVO₄

YANG Xu, DU Fei, BIE Xiaofei, LI Malin, ZHANG Rongyu, WEI Yingjin, WANG Chunzhong, CHEN Gang

2015, 31(3):  457-460.  doi:10.1007/s40242-015-4338-5

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Zn²⁺ ions doped quasi-one-dimensional spin-chain materials LiCu_1-xZn_xVO₄(x=0, 0.1, 0.2) were prepared by solid-state reaction and the effect of nonmagnetic Zn²⁺ ions on the crystal structure, valence state and magnetic properties of them were studied by X^-ray diffraction(XRD), X^-ray photoelectron spectroscopy(XPS) and dc magnetization. The elongation of a and b axes and the shrinkage of c axis indicate a reduced effect of the Jahn-Teller distortion after Zn²⁺ ions doping, while the valence state of transition metal ions in LiCu_1-xZn_xVO₄ remains unchanged since the equivalence doping of Zn²⁺ ions on the Cu²⁺ sites. The corrected Bonner-Fisher equation fitting to the susceptibility indicates that isolated dimers and spins are created along with the departure from infinite spin chains to finite ones.



Thermodynamic Modeling of KF-CrF₃ Binary System

YIN Huiqin, WANG Kun, XIE Leidong, HAN Han, WANG Wenfeng

2015, 31(3):  461-465.  doi:10.1007/s40242-015-4319-8

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A comprehensive thermodynamic model of KF-CrF₃ system was established. The intermediate phases K₂Cr₅F₁₇, KCrF₄, K₂CrF₅ and K₃CrF₆ were described by the stoichiometric compound model and the liquid phase by associated solution model. All the model parameters were optimized by the experimental phase equilibria data assisted by the first-principles prediction within the framework of the calculation of phase diagram(CALPHAD) method. It is demonstrated that the calculated results are fairly consistent with the experimental data, thus we obtained a set of self-consistent and reliable thermodynamic parameters which could well describe the phase equilibria and thermodynamic properties of KF-CrF₃ system.



Emission and Energy Transfer Characteristics of Coumarin 6 Molecules Doped in Opal Polymer Photonic Crystal

CHI Xiaochun, SUI Ning, WANG Yinghui, ZOU Lu, QIAN Cheng, ZHANG Hanzhuang

2015, 31(3):  466-470.  doi:10.1007/s40242-015-4308-y

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The emission of coumarin 6(C-6) doped in opal polymethylmethacrylate(PMMA) photonic crystal(PC) was effectively manipulated. Meanwhile the energy transfer(ET) of C-6 in PCs, which are infiltrated with sulforhodamine B(S-B), was influenced by the concentration of energy acceptor in solution, the size of PMMA microsphere(SM) and the photonic stop band(PSB). The results should be beneficial to people to further understand the potential application of PCs in optoelectronic fields.



Chelating Properties of Salicylhydroxamic Acid-functionalized Polystyrene Resins and Its Application to Efficient Removal of Heavy Metal Ions from Aqueous Solutions

WANG Ruixin, LEI Caiping, WANG Hongjing, SHI Xiaohui

2015, 31(3):  471-476.  doi:10.1007/s40242-015-4476-9

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Salicylhydroxamic acid(SHA) was covalently bound onto crosslinked polystyrene spheres(CPSs) via the Friedel-Crafts alkylation reaction between chloromethylated CPSs and SHA in the presence of SnCl4 as the Lewis acid catalyst. The resulted SHA-CPSs possessed very strong chelating ability for heavy metal ions. In particular, the saturated adsorption amount of SHA-CPSs for Cu²⁺ ions could reach as high as 34.2 mg/g at 318 K. The chelating capability of SHA-CPSs towards heavy metal ions was pH and temperature dependent. SHA-CPSs also showed selective metal coordination with the chelating capacity decreasing in the order of Cu²⁺>Zn²⁺>>Pb²⁺. The adsorption isotherms conformed well to the Langmuir model, and the adsorption process was found to be entropy-driven and endothermic. Besides, SHA-CPSs possessed the excellent reusability.



Structure and Dynamics of Confined Polymer Melts from Attractive Interaction to Repulsive Interaction Between Polymer and Smooth Wall

LI Sijia, ZHANG Wanxi, YAO Weiguo, SHI Tongfei

2015, 31(3):  477-483.  doi:10.1007/s40242-015-4455-1

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We studied the static and dynamic properties of unentangled polymer chains which have a variable strength of interaction with the confining smooth walls by means of the lattice Monte Carlo simulation based on the bond-fluctuation model, that is, investigated the wall-polymer interactions which systematically vary from attraction to repulsion. A critical value of attractive potential(ε_wc) is found to be -0.6k_BT, and only below it can the adsorption layer of monomers be formed near the wall. At the critical point of attraction ε_wc, attractive interaction counterba- lances the wall-polymer excluded volume effect, which minimizes the confinement effects on both chain dimension and mobility. Influences on both chain dimension and mobility increase with the increasing of either attraction or repulsion imposed by the walls. Despite of the nature and strength of the wall-polymer interaction, with the decrease of film thickness, configurations more parallelly aligned and flattened are adopted by confined chains, and a systematic trend of deceleration is found. Variations of chain dynamics with both film thickness and wall-polymer interaction can be well explained by the corresponding changes in the confinement of the nearest-neighboring particles that surround the chains. Besides, the thickness of the interfacial layer inside polymer films, where chains adopt a flattened “pancake” shape, is about two times the bulk radius of gyration and independent of the wall-polymer interaction.



Synthesis of Liquid-like Trisilanol Isobutyl-POSS NOHM and Its Application in Capturing CO₂

BAI Haipeng, ZHENG Yaping, LI Peipei, ZHANG Aibo

2015, 31(3):  484-488.  doi:10.1007/s40242-015-4443-5

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The trisilanol isobutyl polyhedral oligomeric silsesquioxane(POSS) was fabricated into liquid-like nanoparticle organic hybrid materials(NOHMs) with γ-(2,3-epoxypropoxy)propytrimethoxysilane as corona and polyetheramine M2070 as canopy, and the product was called liquid-like POSS NOHM. The liquid-like POSS NOHM has a low viscosity at room temperature without any solvent and the mass fraction of trisilanol isobutyl POSS was 23.38%. The liquid-like POSS NOHM shows great CO₂ capturing property with a capacity of 2.108 mmol/g(p_CO2=6 MPa). The physical adsorption increased obviously with the pressure going up and it may make a difference between liquid-like POSS NOHMs and traditional monoethamolamine(MEA) based CO₂ absorbent. The recycle property was also studied. The NOHM behaved as fresh product even after 10 cycles.