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2017 Vol.38 No.9
 Published: 10 September 2017

Articles: Inorganic Chemistry
Analytical Chemistry
Organic Chemistry
Physical Chemistry
Polymer Chemistry
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2017 Vol. 38 (9): 0-0 [Abstract] ( 144 ) [HTML 1KB] [PDF 2084KB] ( 280 )   

Articles: Inorganic Chemistry
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WANG Danfeng, YANG Haiyan, NING Yuesheng, ZHAO Binyuan
Morphosynthesis of Porous Silver Cubes on the Surface of Hydrogen-pretreated Monolithic Activated Carbon
2017 Vol. 38 (9): 1503-1511 [Abstract] ( 242 ) [HTML 1KB] [PDF 825KB] ( 151 )   
doi: 10.7503/cjcu20160787

The surface functional groups and pore structures of monolithic activated carbon(MAC) were modified by thermal treatment under hydrogen atmosphere. Then the hydrogen-treated MAC adsorbed Cl- and Ag+ successively, and the as-formed AgCl cubes acted as sacrificial templates, which were in turn reduced by the surface functional groups of MAC, and porous silver cubes were obtained on the surface of MAC through morphosynthetic mechanism. The morphology, phase structure of the products were characterized by scanning electron microscopy(SEM), X-ray diffraction(XRD), respectively. The functional groups of MAC were analyzed using X-ray photoelectron spectroscopy(XPS). The effect of the main experimental conditions on the morpho-logy of silver particles on MAC was investigated, including the temperature of hydrogen treatment, the concentration of Cl- soaking solutions, the concentration of Ag+ solutions, and the types of Ag+ precursor. The results indicated that hydrogen treatment can on one hand reduce the amount of oxygen-containing groups of MAC and tune its reducing ability, and on the other hand improve the specific area of MAC, which may facilitate the adsorption of Cl- and nucleation of AgCl. With hydrogen treatment, accompanied by proper concentrations of Cl- and Ag+, and proper type of Ag+ precursor, well defined porous silver cubes can be obtained on MAC.

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KANG Yanyan, QI Hui, ZHOU Miao, ZHANG Ying, ZHUANG Jiaqi, YANG Junxing, WANG Bowei
Synthesis of Ag:InP/ZnSe Nanocrystals and Their Application in Bioimaging
2017 Vol. 38 (9): 1512-1517 [Abstract] ( 140 ) [HTML 1KB] [PDF 560KB] ( 100 )   
doi: 10.7503/cjcu20170286

Ag:InP nanocrystals with near-infrared(NIR) luminescence properties were synthesized and characterized by means of UV-Vis-NIR absorption spectroscopy, transmission electron microscopy(TEM) and X-ray powder diffraction(XRD). When Ag doping amount was 6% and doping temperature was 200℃, the Ag:InP nanocrystals have the highest luminous efficiency. The emission of as-prepared samples was tunable in the near infrared region by tuning the size of samples. After the surface of Ag:InP nanocrystals was coated with ZnSe, the stability of the particles was improved, and the fluorescence efficiency of the particles was increased from 20% to 45%. Also, the biomedical imaging results indicated that as-prepared Ag:InP/ZnS nanocrystals could be a nice carrier with low toxicity.

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YU Ze, GAO He, ZHENG Kai, LIANG Daxin, LIU Zhiming, PANG Guangsheng, FANG Zhenxing
Preparation and Properties of Surface Functionalized Wood by Nanoscale Manganese Oxide
2017 Vol. 38 (9): 1518-1523 [Abstract] ( 120 ) [HTML 1KB] [PDF 603KB] ( 100 )   
doi: 10.7503/cjcu20170177

Nanoscale manganese oxide modified wood samples were prepared by the hydrothermal method. The morphology of the samples were observed by scanning electron microscope(SEM) and the elemental analysis of the samples was carried out by energy dispersive spectroscopy(EDS), and the corrosion resistance and antibacterial properties of the nanoscale manganese oxide modified wood under different treatment conditions were discussed. Data analysis showed that the corrosion resistance and antibacterial properties of nanoscale manganese oxide modified wood were better than those of untreated wood, and the sample treated by sodium dodecylsulfate as surfactant showed better performance on corrosion resistance and antibacterial properties than those prepared by other methods.

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WANG Mo, LI Xiaowei, SHAO Changlu, ZHAO Yingqian, XIN Jiayu, HAN Chaohan, LI Xinghua, LIU Yichun
Preparation of p-CuO/n-In2O3 Heterojunction Nanofibers and Their Gas Sensing Properties
2017 Vol. 38 (9): 1524-1530 [Abstract] ( 224 ) [HTML 1KB] [PDF 706KB] ( 76 )   
doi: 10.7503/cjcu20170112

p-CuO/n-In2O3 heterojunction nanofibers were prepared by solvothermal method using electrospun In2O3 nanofibers as template. The surface morphologies and microstructures of the composite nanofibers were characterized by field emission scanning electron microscopy(SEM), transmission electron microscopy(TEM), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). It was found that the In2O3 nanofibers were uniformly decorated with CuO nanoparticles, and the surface densities of CuO nanoparticles could be controlled by varing the precursor concentration of cupric acetate. Side-heated gas sensors were prepared based on these composite nanofiers. The p-CuO/n-In2O3 heterojunction nanofibers exhibited high gas responses and low operating temperature for detecting H2S gas compared with pure In2O3 nanofibers.

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XU Zhongxuan, LÜ Guoling
Synthesis and Characterization of a 3D Coordination Polymer with Heterometallic Chains and Honeycombed Nanochannels
2017 Vol. 38 (9): 1531-1535 [Abstract] ( 220 ) [HTML 1KB] [PDF 463KB] ( 109 )   
doi: 10.7503/cjcu20170004

Using 5-(hydroxymethyl)isophthalic acid(H2HIA) as the ligand to assemble with Zn2+ ion and K+ ion, an open 3D coordination polymer named[Zn0.5K0.5(HIA)(H2O)]·xGuest(1) was constructed under solvothermal conditions. Complex 1 contains interesting infinite hetrometallic chains and honeycombed nanochannels. Powder X-ray diffraction(PXRD) and thermogravimetry analyses(TGA) techniques were applied to characterizing complex 1 and the photoluminescent properties of complex 1 were also investigated.

Analytical Chemistry
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TONG Ti, ZHAO Yangyang, FU Yilin, SHAN Guiye
Special Surface Enhanced Raman Scattering on Lung Cancer Tissues Based on Au/Cu Nanorods Substrate
2017 Vol. 38 (9): 1536-1541 [Abstract] ( 150 ) [HTML 1KB] [PDF 519KB] ( 95 )   
doi: 10.7503/cjcu20170233

Au/Cu nanorods were prepared by mixing method. The influence of doping copper ions on the plasmon resonance absorption and morphology of gold nanorods was investigated. The plasmon resonance Raman enhancement effect on Au/Cu alloy nanorods was detected. The Raman molecular vibration information of lung cancer tissues and corresponding non-tumor normal tissues were compared on Au/Cu alloy nanorods substrate. Surface enhanced Raman scattering(SERS) analysis of lung cancer tissues and corresponding non-tumor normal tissues demonstrate that the Raman peaks of cancer tissues are stronger compared to non-tumor normal tissues because the SERS signals of protein molecules in lung adenocarcinoma are influenced by their spatial conformation and molecular symmetry. The results suggest that tissue carcinogenesis increases the symmetry of the molecular structure and the Raman peaks near 1250, 1344, 1408, 1568, 1608 and 2560 cm-1 are relevant to amino-compounds of amide Ⅱ in protein, C-H bending vibration, symmetrical variable angle vibration of CH3 in nucleic acids, inert ring vibration of tryptophan in protein and C-O stretching vibration of amide Ⅰ band in protein with intermolecular antiparallel β-fold and sulfhydryl(S-H) stretching vibration of proteins, respectively. The Raman peak near 2936 cm-1 is generated by the joint action of the symmetric stretching vibration of CH2 and the antisymmetric stretching vibration of CH3 in protein. Herein, SERS based on Au/Cu alloy nanorods as substrate is promising to be an effective method for the detection of lung cancer.

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LIU Huiqiang, PENG Chao, CHEN Ning, LIU Yangping
Novel Fluorescent/EPR Difunctional Probe for Detecting Hypochlorite
2017 Vol. 38 (9): 1542-1548 [Abstract] ( 146 ) [HTML 1KB] [PDF 539KB] ( 92 )   
doi: 10.7503/cjcu20170193

To detect hypochlorite effectively and multimodally in biological system, a novel fluorescence/EPR dual probe CNNOH was designed and synthesized based on coumarin and naphthalimide derivatives. The phy-sicochemical properties of CNNOH and its reaction with hypochlorite were studied in detail by fluorescence, electron paramagnetic resonance(EPR) and ultraviolet-visible spectroscopies. The results showed that hypochlorite can be detected using CNNOH by fluorescence and EPR spectroscopies with integrated advantages of both techniques. Owing to fluorescence resonance energy transfer(FRET) effect between the two fluorophores, the probe exhibits a large Stokes shift(135 nm) and thus effectively eliminates interference from of stray light. This dual probe has multiple advantages, such as low detection limit(0.214 μmol/L), short response time to hypochlorite(ca. 10 s), measurement of hypochlorite over a wide range of concentrations(0-5 mmol/L) as well as good selectivity and stability of CNNOH under physiological conditions. Therefore, the new probe shows great potentials in detecting or imaging hypochlorite in living cells and this molecular design provides new insights into the development of new probes for hypochlorite.

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YANG Xin, ZHANG Di, SONG Limin, XU Qian, XU Hui, LIU Ke
Spectroscopic Studies on Alkaline Autoxidation of Curcumin and Antioxidative Activities of the Product
2017 Vol. 38 (9): 1549-1555 [Abstract] ( 117 ) [HTML 1KB] [PDF 462KB] ( 66 )   
doi: 10.7503/cjcu20170147

Curcumin is a natural antioxidant with strong biological and chemical activity. The curcumin degradation was carried out under weak alkaline conditions at room temperature, integrated used by means of column chromatography, UV, IR, NMR, MS and other spectral analysis techniques, the chemical structure of the major degradation products was isolated and identified. For the reaction process, the qualitative and quantitative studies were carried out from two aspects:substrate elimination and product formation by HPLC-DAD spectroscopy analysis technology. Ascorbic acid was used as a positive control, and its antioxidant activities were evaluated in vitro, by 1,1-diphenl-2-picrylhyrazyl free radical(DPPH·), hydroxyl radical(·OH) and superoxide radical(O2) scavenging assays, and compared with curcumin quantitatively. The results showed that the main degradation of curcumin at room temperature under weak alkaline conditions was autoxidation reaction, both of which conformed to the first order kinetics. the structure of heptadiene -3,5-diketone in curcumin[(1E,6E)-1,7-bis-(4-hydroxy-3-methoxy-phenyl)-1,6-heptadiene-3,5-dione] forms a quinone methide intermediate in the presence of alkaline environment, after a series of oxygenation, hydration, dehydration and rearrangement, the target compounds bicyclopentadiones was a cyclization product with a tetrahydrofuran ring and cyclopentanedione structure in the molecule, we named CURC[6-hydroxy-1-(4-hydroxy-3-methoxyphenoxy)-3-(4-hydroxy-3-methoxyphenyl)-1,3,3a,6a-tetrahydro-4H-cyclopenta[c] furan-4-one]. Based on the established stable and reliable spectrophotometric system, the results of in vitro free radical scavenging activity of CURC and curcumin are as follows. CURC has a certain scavenging activity on DPPH·,·OH and O2, but the action intensity is significantly lower than that of curcumin. The EC50 values were 0.17 mmol/L and 0.022 mmol/L in the DPPH assay, 0.33 mmol/L and 0.098 mmol/L in the·OH assay as well as 0.38 mmol/L and 0.056 mmol/L in the O2 assay, respectively. The obtained results suggest that the pH condition should be strictly controlled during the application of curcumin and avoid the autoxidation reaction.

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ZHAN Yan, ZU Hongru, HUANG Di, LIU Yingliang, HU Chaofan
Synthesis of Fluorescent Graphitic Carbon Nitride Quantum Dots by Solvothermal Ions Intercalation Method for Fe(Ⅲ) Detection
2017 Vol. 38 (9): 1556-1562 [Abstract] ( 512 ) [HTML 1KB] [PDF 667KB] ( 319 )   
doi: 10.7503/cjcu20170115

As a new kind of two dimensional nanomaterials, graphitic carbon nitride(g-C3N4) has extensively attracted interests due to the similar performance with grapheme. A solvothermal method of preparing fluorescent graphitic carbon nitride quantum dots(g-C3N4 QDs) in the presence of KOH intercalation was developed in this paper. The obtained g-C3N4 QDs exhibited excellent water dispersity and fluorescence stability. Transmission electron microscopy(TEM) image showed the diameter of g-C3N4 QDs was about 2.3 nm. There were large amounts of hydrophilic groups on the surface of g-C3N4 QDs exhibited by X-ray photoelectron spectroscopy(XPS) and Fourier transform infrared(FTIR) spectrum analysis. Excitation-dependent photoluminescence behavior was observed by photoluminescence(PL) spectra. Owing to the phenomenon in which Fe3+ ions has great influence on the fluorescence quenching of g-C3N4 QDs, we proposed one fluorescent sensor for the detection of Fe3+ ions, and the detection system exhibited excellent liner relationship with the concentration of 5-100 μmol/L Fe3+ ions, the detection limit for Fe3+ ions was about 0.5 μmol/L, making a highly efficient and sensitive selection for Fe3+ ions.

Organic Chemistry
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FANG Qiusheng, LI Yanhong, CHEN Ling
Synthesis of Novel Anthracene Crown Ethers and the Guest Binding Behaviors
2017 Vol. 38 (9): 1563-1567 [Abstract] ( 92 ) [HTML 1KB] [PDF 438KB] ( 60 )   
doi: 10.7503/cjcu20170317

Two crown ethers bearing anthracene aromatics were synthesized from 9,10-dibromomethyl anthracene via three steps. The host-guest binding behavior between new crown ethers and two π-electron-deficient guests was investigated by means of 1H NMR, UV-Vis spectroscopy and X-ray diffraction analysis. The results revealed that host-guest interaction between anthracene crown ethers and guests was mainly contributed by π-stacking. The association constants determined by UV-Vis spectrum. The result showed anthracene crown ethers had better binding ability than classical bezo-and naphtho-crown ethers, which indicated the introduction of anthracene aromatics could improve the host-guest binding ability of crown ethers significantly.

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DUAN Yongbin, YIN Yan, MENG Fanli, ZHAO Lianhua, LIU Yukun, YUAN Zhe, FENG Yangbo
Design, Synthesis and Biological Evaluation of Benzothiazoles as Highly Potent ROCK Inhibitors Through Molecular Docking and Free Energy Calculations
2017 Vol. 38 (9): 1568-1577 [Abstract] ( 106 ) [HTML 1KB] [PDF 713KB] ( 65 )   
doi: 10.7503/cjcu20170213

Rock has been considered to provide a pharmacological strategy for preventing and treating multiple sclerosis, pulmonary hypertension, glaucoma, cardiovascular disease, erectile dysfunction and cancer. With 3 previously reported and benzothiazole-based ROCK inhibitors(1-3) as the research targets, the structure-activity relationship(SAR) was preliminary revealed from amino acid level by molecular docking after obtaining the stable ROCK2-ligand complexes in the binding pocket through molecular dynamic simulations. Then MM/GBSA free energy calculations of compounds 1-3 showed that there was good correlation between binding affinity(△Gbind) and inhibitory activities, and van der Waals interaction(△GVDW) contributing to △Gbind most. And the key amino acids with outstanding contribution for high inhibition were obtained through free energy analysis. Finally, 3 series of benzothiazoles(D1~D10) were designed according to the results of molecular docking and free energy calculations. In the biological evaluation, compounds D1~D10 exhibited 2-105 nmol/L IC50 values against ROCK2 and 11-288 nmol/L IC50 values against ROCK1. Compounds D3-D5 exhibited higher metabolic stability than reported compounds 1 and 3 in human liver microsome studies. This work not only gave theoretical guidance for the design of highly potent ROCK, but also offered a series of highly active ROCK inhibitors with intellectual property right for fundamental research and application of ROCK.

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SUN Liwei, LUO Jingyi, TANG Shaokun
Synthesis of Dual-functionalized Ionic Liquid and Application in CO2 Absorption
2017 Vol. 38 (9): 1578-1583 [Abstract] ( 234 ) [HTML 1KB] [PDF 443KB] ( 99 )   
doi: 10.7503/cjcu20170117

A new bifunctional ionic liquid was prepared, characterized and applied in the absorption and desorption of CO2. First, 1-methoxyethyl-3-methyl imidazolium glycinate([C3O1mim] [Gly]) was synthesized by two-step method. The molecular structure was characterized and confirmed by 1H, 13C nuclear magnetic resonance(NMR) and Fourier transform infrared(FTIR) spectroscopy. And thermogravimetric(TG) analysis suggested that[C3O1mim] [Gly] had good thermal stability. Then, compared to monoethanolamine(MEA), the CO2 absorption capacity of[C3O1mim] [Gly] was studied in the range of 25-100℃ at normal pressure. By computation, the CO2 absorption capacity can reach 1.26 mol CO2/mol IL at 40℃, which is greatly higher than that of monoethanolamine(0.54 mol CO2/mol MEA). And absorption capacity of CO2 in[C3O1mim] [Gly] would decrease with the increase of temperature from 40℃ to 100℃. Furthermore, the ionic liquid exhibited excellent reversibility and CO2 absorption capacity can be maintained after 5 times of absorption-desorption circulation. Finally, the absorption kinetics of CO2 in[C3O1mim] [Gly] was studied at 40℃. And Pseudo-second-order model is good to describe CO2 absorption in[C3O1mim] [Gly].

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REN Baoyi, HUANG Dan, XU Qin, SUN Yaguang
Synthesis and Properties of a New Compound Derived from Annulated-indigo
2017 Vol. 38 (9): 1584-1589 [Abstract] ( 160 ) [HTML 1KB] [PDF 487KB] ( 92 )   
doi: 10.7503/cjcu20170099

In this paper, a donor-acceptor-type molecule, 2,2'-(-(((2,9-bis(5-(2-decyltetradecyl)thiophen-2-yl)-6,13-dioxo-6,13-dihydrodiindolo[3,2,1-de:3',2',1'-ij] [1,5] naphthyridine-7,14-diyl)bis(thiophene-5,2-diyl))bis(methaneylylidene))bis(3-oxo-2,3-dihydro-1H-indene-2,1-diylidene))dimalononitrile(MT-BAI-TM) was synthesized using the strategy of bay-annulation. The compound possessed deep absorption spectra extending to 820 nm and low-lying LUMO level of -3.98 eV. The distribution of frontier molecular orbits was calculated by density functional theory(DFT). A face-on orientation between MT-BAI-TM molecules in spin-coating film(sample S-1) was observed by grazing incidence wide angle X-ray scattering(GIWAXS). The characteristics of deep absorption, high electron affinity and face-on orientation of the compound indicate the nature of acceptor-type organic semiconductor. Hence, the MT-BAI-TM is an attractive candidate as acceptor materials for potential application in organic photovoltaic devices.

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WANG Lei, ZHENG Guojun, JI Qi, CHEN Bo, GONG Longlong, GAO Congmin, DU Zhenjian, ZHANG Xingmin
Synthesis and Biological Activity of Novel PI3K/mTOR Inhibitors
2017 Vol. 38 (9): 1590-1595 [Abstract] ( 228 ) [HTML 1KB] [PDF 428KB] ( 80 )   
doi: 10.7503/cjcu20170136

A series of new phosphatidylinositol 3-kinase/mammalian target of rapamycin(PI3K/mTOR) inhibitors with optimized synthetic process was designed and synthesized, the correctness of the structure was determined by 1H NMR and LC-MS and the antitumor activities of these compounds were evaluated in 3 tumor celllines by MTT colorimetric method. Compound 11 showed very strong inhibition of MV4-11 cell growth, and was selected as a leading compound for further development of anti-leukemia drug candidate.

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XIAO Shuyan, LI Fei, DONG Zhongping
Solution Structure of Slc11a2-TM6 in Dodecylphosphocholine Micelles
2017 Vol. 38 (9): 1596-1601 [Abstract] ( 148 ) [HTML 1KB] [PDF 510KB] ( 73 )   
doi: 10.7503/cjcu20160884

The structure of isolated peptides from TM6 of Slc11a2 in dodecylphosphocholine(DPC) micelles was investigated using circular dichroism(CD) and nuclear magnetic resonance(NMR) spectroscopy. The results reveal that TM6 of Slc11a2 forms short α-helix in both N-and C-terminal and the two α-helixes are connected by a highly flexible region, the whole peptide is embedded in DPC micelles. H267A mutation makes the helix become longer, while H272A mutation make the helix become slightly shorter.

Physical Chemistry
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WANG Junkai, HAN Lei, HUANG Liang, ZHANG Haijun, LI Junyi, LI Saisai
Density Functional Theory Calculation and Experimental Study of Catalytic Synthesis SiC Nano Powders
2017 Vol. 38 (9): 1602-1610 [Abstract] ( 132 ) [HTML 1KB] [PDF 821KB] ( 62 )   
doi: 10.7503/cjcu20170259

Taking Si55, Si43M12 and Si37M18(M=Fe, Co or Ni) cluster as models, density functional theory(DFT) was used to investigate the catalytic mechanism of Fe, Co and Ni catalysts on the formation of SiC using Si and C as starting materials. The results show that Fe, Co and Ni nano catalysts will form alloy with Si first, and then elongate the bond length of Si-Si and weaken its bond strength, finally activate Si powder. The formation of alloy is favorable to the adsorption of C atom, and then accelerate the reaction process between Si and C atoms. The catalytic performance of Fe is better than Co and Ni. On this basis, 3C-SiC nano powders were synthesized by a microwave reaction method using silicon powders and phenolic resin as raw materials, and ferric/cobalt/nickel nitrate as catalyst precursor. The effects of catalyst type, heat treatment temperature, catalyst content and holding time on the preparation of 3C-SiC were investigated. Results indicated that the addition of Fe, Co and Ni significantly decreased the synthesis temperature of 3C-SiC. Si powder can completely transform into 3C-SiC at 1100℃ for 30 min using 2.0% Fe as catalyst. In contrast, for the sample without any catalysts, corresponding temperature was as high as 1250℃. Moreover, the experiment results also indicated that the catalytic performance of Fe is better than Co and Ni, which is in consistent with the DFT calculations.

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QIAN Mengdan, LUO Wei, NI Zheming, XIA Shengjie, XUE Jilong, JIANG Junhui
Comparative Study on the Properties and Adsorption of Furfural of Pd(111) Surface Before and After Ru Modification
2017 Vol. 38 (9): 1611-1618 [Abstract] ( 92 ) [HTML 1KB] [PDF 671KB] ( 53 )   
doi: 10.7503/cjcu20170189

The properties of Pd(111), Ru-Pd(111) surfaces and their adsorption of furfural were investigated via periodic density functional theory(DFT) calculations. The results of atomic size factor, relative bond length, formation energy and d-band center showed that Ru-Pd(111) surface was more stable and active than Pd(111), Ru modification could improve the geometric configuration. For the adsorption of furfural on Pd(111) and Ru-Pd(111) surfaces, the results showed that when the initial adsorption at P(top-bridge) or P(Pd-fcc-Ru-fcc) site, the adsorption energy was the highest and the adsorption configuration was the most stable. After analyzing Mulliken atomic charge population and the deformation density, it was found that for the adsorption of furfural on Ru-Pd(111) surface, the number of charge transferred was more and the interaction was stronger, therefore it's adsorption energy was higher. The result of state density indicated that the main reason for the adsorption was that the p and d orbitals hybridization existed at -7.34 eV relative to Fermi level. Meanwhile, the p-orbital of furfural shifted to the low-level was more obvious on Ru-Pd(111) surface, so Pd catalyst after Ru modification had better catalytic activity.

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YAN Xiaohong, GE Xia, ZHANG Lin, QI Lijuan, LIU Yang, WEI Shaohua, ZHU Xiaoshu, TANG Yawen
Preparation of Phosphoric Acid-functionalized Pd/C Catalyst by Coordination Reduction and Its Application
2017 Vol. 38 (9): 1619-1626 [Abstract] ( 229 ) [HTML 1KB] [PDF 784KB] ( 152 )   
doi: 10.7503/cjcu20170092

We presented a one-step reduction approach to the synthesis of highly dispersed and ultrafine phosphonate functionalized Pd nanoparticles supported by carbon(Pd/C) using XC-72 as the catalyst support, ethylenediamine tetramethylene phosphonic acid(EDTMPA) as both coordination agent and stabilizer, palladium chloride(PdCl2) as the precursor and sodium borohydride(NaBH4) as the reducing agent, respectively. Transmission electron microscopy(TEM) and X-ray diffraction(XRD) analysis results indicated that the average particle size and the dispersion degree in the Pd/C catalysts are 2.7 nm and 37.1%, respectively, much higher than those of the commercial catalysts. The activation energy of catalytic hydrogenation for rhodamine(RhB) and p-nitrophenol(4-NP) for the obtained catalyst are calculated to be 27.1 and 16.9 kJ/mol, respectively, obviously lower than those in the commercial Pd/C catalyst(57.2 and 55.7 kJ/mol).

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HU Jingwei, CHENG Rui, DING Shunmin, XU Mengmeng, XU Lu, XIAO Weiming, ZHOU Penghui, ZHANG Ning
Diphenylphosphine Functionalized Graphene Oxide Supported Palladium Complex Catalyzed Heck Coupling Reaction
2017 Vol. 38 (9): 1627-1632 [Abstract] ( 330 ) [HTML 1KB] [PDF 518KB] ( 124 )   
doi: 10.7503/cjcu20170086

The graphene oxide was functionalized by diphenylphosphine through covalent bond. The functio-nalized graphene oxide was used to immobilize palladium via the coordination bonds between the diphenylphosphine and palladium. The as-synthesized catalyst(GO-P-Pd) was characterized by Fourier transform infrared spectroscopy(FTIR), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS) and applied in the Heck coupling reaction. The result shows that GO-P-Pd exhibits excellent catalytic performance with high activity and stability. And the catalyst can also be applied to catalyze a wide scope of substrates.

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ZHANG Dong, LI Tingting, QIU Hailong, WEI Yingjin, WANG Chunzhong, CHEN Gang, YUE Huijuan
Preparation and Characterization of N-doped Li2FeSiO4/C Cathode Materials for Lithium Ion Batteries
2017 Vol. 38 (9): 1633-1638 [Abstract] ( 119 ) [HTML 1KB] [PDF 577KB] ( 65 )   
doi: 10.7503/cjcu20170060

N-doped lithium iron silicates(N-doped Li2FeSiO4, N-LFs) was prepared with sol-gel method. X-Ray diffraction, field emission scanning electron microscopy, X-ray photoelectron spectroscopy, galvanosta-tic charge-discharge and electrochemical impedance spectra were used to investigate the effect of nitrogen doping on the characteristics of Li2FeSiO4. The results show that nitrogen does enter the cystal strucutre of Li2FeSiO4, resulting in smaller particle size and better kinetic properties, as well as higher specific capacity and rate capability. The doped sample could deliver a specific capacity of 130 mA·h/g in the first discharge and retain 124 mA·h/g after 50 cycles with the retention of 95%.

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LIANG Xiaodan, FAN Ye, FANG Yun, XIA Yongmei, CHENG Ruohui
Investigation of Vesiculation of Conjugated Linoleic Acid Assisted by Monolauryl Phosphate
2017 Vol. 38 (9): 1639-1644 [Abstract] ( 176 ) [HTML 1KB] [PDF 699KB] ( 110 )   
doi: 10.7503/cjcu20170057

A safe and mild anionic surfactant monolauryl phosphate(MLP) was blend with conjugated linoleic acid(CLA) that acted as the model fatty acid, and the vesiculation of CLA was observed in the weakly acidic to neutral pH range by DLS and TEM. Various charged species of the above two molecules with pH variation were investigated by means of pH titration, and molecular interaction among these species was reasoned. The impetus driving vesiculation of CLA assisted by MLP in the weakly acidic to neutral pH range was ascribed to hydrogen bonding and ion dipole interaction between CLA and MLP.

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YIN Jinchao, CHEN Yukai, JIANG Jianzhong, CUI Zhenggang
Synthesis and Properties of pH and Redox Dual-switchable Surfactant
2017 Vol. 38 (9): 1645-1653 [Abstract] ( 181 ) [HTML 1KB] [PDF 892KB] ( 92 )   
doi: 10.7503/cjcu20170054

A new dual-stimuli responsive surfactant intermediate 11-tertiary aminehendecyl-carbonyl-ferrocenyl(C11-N-Fe) was synthesized. The structure of the product was characterized by mass spectra and 1H NMR. The dual-stimuli responsive properties of C11-N-Fe were investigated by optical transmittance and cyclic voltammograms. The results show that C11-N-Fe has good dual-stimuli properties. pH and redox dual-stimulated responsive foams can be prepared by C11-N-Fe hydrochloride surfactant. Moreover, the defoaming process triggered pH or redox reaction can be completed within 2 min. C11-N-Fe hydrochloride surfactant can also act as the emulsifier for n-decane/water system, because of it contains rigid ferrocenyl on hydrophobic chain. The C11-N-Fe hydrochloride emulsion with uniform particle size can be prepared. Besides, the stability of the emulsion becomes more stable with increasing of the concentration of C11-N-Fe hydrochloride surfactant. Furthermore, the emulsion can also be triggered by pH and redox dual-stimuli.

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HE Wenli, CHEN Meng, QIAN Dongjin
Pd(Ⅱ)-Directed Layer-by-layer Assembly of Multiporphyrin Arrays on Silica Nanoparticle Surfaces for Photocurrent Generation and Photochromism of Viologens
2017 Vol. 38 (9): 1654-1662 [Abstract] ( 177 ) [HTML 1KB] [PDF 666KB] ( 75 )   
doi: 10.7503/cjcu20160840

Pyridyl-functionalized silica nanoparticles(nanoSiO2 BPy) were prepared, on the surfaces of which the Pd(Ⅱ)-directed multiporphyrin arrays were constructed by using the layer-by-layer(LBL) technique with zinc tetrapyridylporphyrin(ZnTPyP) as multi-dentate linkers to produce the nanoSiO2 BPy@(Pd/ZnTPyP)n hybrid material. Thermogravimetric analysis revealed a mass loss of approximately 17% of the total mass that was attributed to the decomposition of organic species in the nanoSiO2B Py@(Pd/ZnTPyP)3 hybrid. For the ZnTPyP in the hybrids, the Soret absorption band appeared at about 426 nm, the fluorescent emission bands appeared at about 605 and 655 nm, and the emission lifetime was approximately 1.78 ns. All these data were much similar to those of ZnTPyP in the dilute DMSO solutions, suggesting that the porphyrin-porphyrin interactions were weak and no porphyrin aggregates formed in the hybrid. The silica nanoparticle sizes slightly increased from 10-16 nm to 15-20 nm, which was attributed to the fact that the multiporphyrin arrays were immobilized on the particle surfaces. Cyclic voltammograms of the hybrid in the casting films revealed two couples of redox peaks in the potential range of -0.6-2.4 V(vs. Ag/AgCl), corresponding to the electron transfer processes of porphyrin oxidation. Finally, the indium tin oxide electrodes covered with the nanoSiO2 BPy@(Pd/ZnTPyP)3 hybrid were used as the photosensitizers for the light-induced current generation and photochromism of ethyl viologens.

Polymer Chemistry
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LI Guili, HUANG Jingjing, ZHANG Huanhuan, YUAN Chaosheng, SHAO Chunguang, YING Jin, WANG Yaming, CAO Wei, LIU Chuntai, SHEN Changyu
Formation and Structure Analysis of Interfacial Cylindrites Induced by Silkworm Silk Fiber in Poly(lactic acid) Based Composites
2017 Vol. 38 (9): 1663-1669 [Abstract] ( 116 ) [HTML 1KB] [PDF 677KB] ( 77 )   
doi: 10.7503/cjcu20170194

Thin films of poly(lactic acid)(PLA) were prepared using solution method. At different temperatures and fiber-pulling speeds, the morphology of cylindrites induced by a single silkworm silk fiber(SF) in PLA films was investigated by polarized optical microscopy(POM) and Fourier transform infrared spectroscopy(FTIR). The results show that there is a critical fiber-pulling speed, above which the continuous cylindrites structure could be generated on the fiber surface, whereas discontinuous cylindrites would form at a speed lower than that value. Besides, there also exists another special speed defined as saturation fiber-pulling speed, and once the pulling rate exceeds that value, the degree of crystallization and orientation will reach a plateau. Moreover, at the same temperature, the induction period of cylindrites nuclei reduces and its nuclei density and the orientation increase with raising the fiber-pulling speed; under a given fiber-pulling speed, compared to 130℃, the induction period of cylindrites is shorter, and its nuclei density, growth rate as well as final crystallinity are much higher at 120℃.

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GU Yuanbo, HU Yanhong, DU Lei, DENG Shifeng, ZHOU Yan, RU Lingao
Reinforcement and Tougheness of Quartz Fiber/Silicon-containing Arylacetylene with Heat-resistant Polyetherimide Macromolecular Coupling Agent
2017 Vol. 38 (9): 1670-1677 [Abstract] ( 188 ) [HTML 1KB] [PDF 724KB] ( 61 )   
doi: 10.7503/cjcu20170149

A novel acetylene-terminated polyetherimide macromolecular coupling agent(BDA-K) was designed and synthesized, and its effects on the interfacial reinforcement and toughness of the quartz fiber(QF) reinforced silicon-containing aryl-alkyne(PSA) matrix composites were investigated. The interlaminar shear strength(ILSS), flexural strength and notched impact strength increased by 54.1%, 59.0% and 23.8% compared with those of untreated at room temperature. The retention of ILSS and flexural strength reached 89.0% and 89.6% at 250℃ and 63.3% and 67.9% at 500℃, respectively. The FTIR and XPS spectra indicate that BDA-K takes part in PSA curing and effective chemical bonds form between BDA-K and QF. Owing to the introduction of heat-proof groups i.e. the imide rings to BDA-K backbone, TGA results reveal that the value of Td5 is up to 489℃. The interphase morphologies by SEM show that soft and moderate macromolecule layers constructed between the matrix and the fiber treated with BDA-K, which improves the mechanical strength and toughness of the QF/PSA composites.

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YOU Yanwei, XIAO Changfa, WANG Chun, HUANG Qinglin, CHEN Mingxing, HUANG Yan
Preparation and Properties of Poly(tetrafluoroethylene-co-hexafluoropropylene) Hollow Fiber Membranes
2017 Vol. 38 (9): 1678-1686 [Abstract] ( 508 ) [HTML 1KB] [PDF 1030KB] ( 384 )   
doi: 10.7503/cjcu20170053

Poly(tetrafluoroethylene-co-hexafluoropropylene)(FEP) hollow fiber membranes(HFMs) were prepared by melt spinning method with FEP as polymer matrix, water solubility composite powder as pore-forming agent and dioctyl phthalate(DOP) as diluent. The effects of different concentrations of acid and alkali on the structure and properties of FEP HFMs were studied. The results show that the prepared FEP HFMs have a microporous structure with stretched pores, interface microporous and dissolved microporous, and the sponge-like microporous structure is evenly distributed on the cross-section. After 60 d immersed in 25% NaOH and H2SO4 solution, the chemical structure of the membranes has been unaffected, while the average pore size becomes larger and the pore size distribution narrows. The retention rates of break strength reach 86.8% and 80.8%, respectively. The acid and alkali resistance study indicates that the FEP HFMs have excellent chemical and thermal stability compared to commercial PVDF HFMs.

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HUANG Haihong, ZHANG Baoyu, ZHAO Zhipei
Degradation and Characterization of Recycling Carbon Fiber/Epoxy Resin Composites in Supercritical n-Butanol
2017 Vol. 38 (9): 1687-1694 [Abstract] ( 102 ) [HTML 1KB] [PDF 603KB] ( 56 )   
doi: 10.7503/cjcu20170037

Recycling carbon fibers from carbon fiber/epoxy resin(CF/EP) composites using supercritical n-butanol were reported. The quantitative relationship between the degradation rate of epoxy resin and recycling process parameters was proposed through response surface methodology. The influence of process parameters on the degradation rate of epoxy resin was investigated by graphical optimization. Besides, the microstructure, the graphitization degree, the surface chemistry and the mechanical properties of the recycled carbon fibers were analyzed by scanning elcetron microscopy(SEM), atomic force microscopy(AFM), X-ray photoelectron spectrometry(XPS), Raman spectrum and single-filament tensile strength testing. The results show that the error between the actual and the theoretical degradation rate is within ±5.5%, and the reaction temperature has the greatest impact on the degradation rate of epoxy resin, followed by the reaction time, KOH concentration and n-butanol volume. Given the optimal process parameters(i.e., reaction temperature at 330℃, reaction time at 60 min, KOH concentration at 0.0538 mol/L, and feed ratio at 0.024 g/mL), there were no residual resin and graphitization on the surface of the recycled carbon fibers; the average roughness(Ra) and O/C ratio showed little change comparing with those of the original carbon fibers; and the average tensile strength and Young's modulus were about 93.58% and 94.87% of those of the original carbon fibers, respectively.

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LI Zhiming, DING Qiang, GU Xiaojun, XIN Hong, BAI Binglian, LI Min
Organogel and Photo-responsive Behaviour of Hydrazide Derivatives Containing Azobenzene Groups
2017 Vol. 38 (9): 1695-1700 [Abstract] ( 125 ) [HTML 1KB] [PDF 600KB] ( 46 )   
doi: 10.7503/cjcu20170019

The hydrazide derivatives containing azobenzene groups N-(3,4-n-oxyphenyl)-N'-4-(azophenyl)-benzohydrazide Dn(n=7, 8, 10) with different terminal alkyl chain lengths were designed and synthesized. Dn can form a stable organogel and the terminal alkyl chains play crucial roles in improving the gel ability and thermodynamic stability. The main driving forces of gel formation are intermolecular hydrogen bonds between amide groups, π-π interactions among azobenzene groups and van der Waals forces between alkyl chains. Irradiation of the solution by UV light can lead to trans-cis isomerization of the azobenzene units. Although the conversion efficiency of cis-azobenzene in solution is notable, the photo-induced trans-cis isomerization of azobenzene in the gel cannot induce gel-sol.

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WU Jing, GUO Jing, ZHANG Sen, GONG Yumei, ZHANG Hong
Correlativity of Characterization for Sodium Alginate/Antarctic Krill Protein by Salt Concentration
2017 Vol. 38 (9): 1701-1708 [Abstract] ( 251 ) [HTML 1KB] [PDF 739KB] ( 64 )   
doi: 10.7503/cjcu20170015

Sodium alginate/antarctic krill protein composite material(SA/AKP) was obtained by wet spinning. The hydrogen bonds of SA/AKP composite material were analyzed by Fourier transform infrared spectroscopy(FTIR), the effects of salt concentration on the crystallinity, fluidity and morphology of the composite material were studied by XRD, rheometer and SEM. Experiment manifested the existence of intramolecular and intermolecular hydrogen bonds in SA/AKP system. The strength of intermolecular hydrogen bonds was enhanced with the increase of NaCl in the composite material. At the same time, the increase of salt concentration led to SA/AKP composite material's crystallinity increasing, the rheological properties decreasing at first and then increasing, and mechanical properties increasing at first and then decreasing. SA/AKP fiber SEM images showed that crystallized salt was separated from the fiber, and the surface structure of the composite fiber gradually decreased and became denser and smoother.Finally, AKP was completely oriented in the SA/AKP composite system.

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