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Science china chemistry 2005年第z1期48卷 50-54页

作者： WANG Feili,TANG Zongxun,LI Shuni,HU Daodao,ZHAO Hongan,HU Huaimin & ZHOU Zhongyuan Department of chemistry,Northwest University / Shaanxi Key Laboratory of Physico-lnorganic chemistry,Xi’an 710069,china Shaanxi Normal University,Xi’an 710062,china chengdu institute of organic chemistry,chinese academy of sciences,chengdu 610041,china 1. Department of chemistry Northwest University / Shaanxi Key Laboratory of Physico-lnorganic Chemistry 710069 Xi’an China 2. Shaanxi Normal University 710062 Xi’an China 3. chengdu institute of organic chemistry Chinese Academy of Sciences 610041 Chengdu China

The single crystal of [Ba(H2O)2(C6H12O6)2Cl2] was obtained based on the phase equilibrium results. Its structure was determined by X-ray crystallographic analysis. The crystals are monoclinic and in space group C2/c with a = 1.901 7(2) nm, b = 0.682 13(8) nm, c = 0.162 60(2) nm, β = 96.593(2)° and V = 2.095 3(4) nm3, Z = 4, DC = 1.917 g·cm-3. In its solid state, this supramolecular complex is a three-dimensional network with double layers connected by hydrogen bondings. The molecule structure of [Ba(H2O)2(C6H12O6)2Cl2] has a central barium ion that is coordinated to two water molecules, two chlorides, and four hydroxyls from the two inositols. Losing the coordinating water is controlled by random nucleation and growth mechanism (n = 2/3) and 3-dimensional diffusion mechanism (n = 2).

关键词： barium complex, inositol, crystal structure, water loss mechanism.

SiO/CNTs:A new anode composition for lithium-ion battery

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Science china chemistry 2009年第12期52卷 2047-2050页

作者： REN YuRong1,2,3?,QU MeiZhen1 & YU ZuoLong1 1 chengdu institute of organic chemistry,chinese academy of sciences,chengdu 610041,china 2 College of chemistry,Jilin Normal University,Siping 136000,china 3 Graduate University of chinese academy of sciences,Beijing 100039,china 1. chengdu institute of organic chemistry Chinese Academy of Sciences Chengdu 610041 China 2. College of chemistry Jilin Normal University Siping 136000 China 3. Graduate University of chinese academy of sciences Beijing 100039 China

A new anode composition SiO/CNTs (carbon nanotubes) has been prepared by chemical vapor deposition (CVD) method. The results of scanning electron microscopy (SEM) confirm that CNTs deposit on small SiO particles,form a cage,and enwrap SiO particles tightly. SiO/CNTs anode composition exhibits an initial discharge and charge capacity of 1171 and 789 mAh/g,and maintains a reversible capacity of 500 mAh/g after 80 cycles. The improvement of the cyclic performance for SiO/CNTs composition is related to the maintaining of the electric network during cycling,which benefits from a tight contact between CNTs and SiO particles.

关键词： SiO/CNTs CVD composition anode Li-ion battery

Synthesis, crystal structure and properties of binuclear manganese complex [(bipy)_2Mn_2(/J-O)(/i-Ac)_2(H_2O)_2](ClO_4)_2

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chinese Science Bulletin 2000年第12期45卷 1079-1082页

作者： LI Jun, YANG Shuming, ZHANG Fengxing, TANG Zongxun, SHI Qizhen & ZHOU Zhongyuan1. Department of chemistry, Northwest University, Xi’an 710069, china 2. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china Correspondence should be addressed to Li Jun Department of chemistry Northwest University Xi’an China chengdu institute of organic chemistry Chinese Academy of Sciences Chengdu China

Binuclear manganese complex [(bipy)2Mn2(μ-O)(μ-Ac)2(H2O)2](CIO4)2 was synthesized by the reaction of MnAc3 · 2H2O with 2,2’-bipyridine in the HAc-NaAc buffer (pH = 4.0). X-ray diffraction result for the single crystal shows that the crystal is monoclinic, space group C2/C, with a = 3.4082(7), 6 = 0.8644(2), c= 2.174 9(4) nm,β= 105.2°, V =6.186(2) nm3, Z= 8. There are two very strong peaks of UV-Vis spectrum in the range of 400-600 nm, which are similar to those of Mn catalase and Mn ribonuleotide reductase extracted from organisms. Cyclic voltammogram shows that the complex in CH3CN undergoes quasi-reversible one-electron reduction and oxidation at E1/2=1.15V.

关键词： binuclear manganese complex crystal structure synthesis properties.

Kinetics and reaction mechanism of phenol hydroxylation catalyzed by La-Cu_4FeAlCO_3

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Science china chemistry 2005年第6期48卷 530-537页

作者： CHEN Chunxia1,2, XU Chenghua1, FENG Liangrong1, SUO Jishuan1 & QIU Fali1 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. Graduate School of the chinese academy of sciences, Beijing 100039, china 1. chengdu institute of organic chemistry Chinese Academy of Sciences 610041 Chengdu China 2. Graduate School of the chinese academy of sciences 100039 Beijing China

The present work synthesizes La-Cu4FeAlCO3 catalyst under microwave irradiation and characterizes its structure using XRD and IR techniques. The results show that the obtained La-Cu4FeAlCO3 has a hydrotalcite structure. In the phenol hydroxylation with H2O2 catalyzed by La-Cu4FeAlCO3, the effects of reaction time and phenol/H2O2 molar ratio on the phenol hy-droxylation, and relationships between the initial hydroxylation rate with concentration of the catalyst, phenol, H2O2 and reaction temperature are also investigated in details. It is shown the phenol conversion can reach 50.09% (mol percent) in the phenol hydroxylation catalyzed by La-Cu4FeAlCO3, under the reaction conditions of the molar ratio of phenol/H2O2 1/2, the amount ratio of phenol/catalyst 20, reaction temperature 343 K, reaction time 120 min, 10 mL distilled water as solvent. Moreover, a kinetic equation of v = k[La ? Cu 4 FeAlCO 3 ][C 6 H 5 OH][H 2 O 2]. and the activation energy of Ea=58.37 kJ/mol are obtained according to the kinetic studies. Due to the fact that the HO-Cu+-OH species are detected in La-Cu4FeAlCO3/H2O2 system by XPS, the new mechanism about the generation of hydroxyl free radicals in the phenol hydroxylation is pro-posed, which is supposed that HO-Cu+-OH species are transition state in this reaction.

关键词： rare earth, hydrotalcite, microwave irradiation, phenol hydroxylation, kinetics, reaction mechanism.

RING-OPENING COPOLYMERIZATION OF DL-LACTIDE AND POLY(ETHYLENE GLYCOL) INITIATED BY LANTHANUM ACETATE AND APPLICATION OF THE COPOLYMER AS MATRIX OF MICROSPHERES CONTAINING VIBRIO CHOLERA ANTIGENS

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chinese Journal of Polymer Science 1999年第3期17卷 265-270页

作者： Xian-mo Deng Xiao-hong Li Ming-long Yuan Xiong-wei Li Cheng-dong Xiong Zhi-tang Huang Wen-xiang Jia chengdu institute of organic chemistry, chinese academy of sciences, chengdu, 610041, china institute of chemistry, chinese academy of sciences, Beijing, 100080, china West china University of Medical sciences, chengdu, 610041, china chinese Acad Sci Chengdu Inst Organ Chem Chengdu 610041 Peoples R China chinese Acad Sci Inst Chem Beijing 100080 Peoples R China W china Univ Med Sci Chengdu 610041 Peoples R China

Poly-dl-lactide-poly(ethylene glycol) (PELA) triblock copolymers were synthesized with lanthanum acetate as the initiator. PELA microspheres with entrapped Vibrio Cholera antigen and outer membrane protein (OMP) were prepared by a double emulsion W/O/W based on solvent extraction methods. The obtained microspheres showed smooth and spherical surface and their size varied between 0.5 and 5.0 mu m, which are suitable for oral targeting delivery system. The distribution tests in rabbits and mice through scanning electronic micrography and fluorescence microscope indicated that microspheres have successfully reached the immunization-related tissues, such as the liver, spleen and intestinal peyer's patches, following oral administration. The PELA microspheres were also evaluated as an efficient antigen delivery system by enhancing a higher protective ratio against live Vibrios Cholera.

关键词： poly-dl-lactide-poly(ethylene glycol) Vibrio Cholera antigen lanthanum acetate microsphere protective ratio

Study on the coating of nano-scale SiO_2 film on the surface of nanocrystalline Mg-Al layered double hydroxides

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Science china chemistry 2005年第2期48卷 107-114页

作者： ZHANG Zejiang1,2,3, MEI Xiujuan2, XU Chenghua1 & QIU Fali1 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. Sichuan Fire Research institute of Public Security Ministry, chengdu 611830, china 3. Graduate School of the chinese academy of sciences, Beijing 100039, china Correspondence should be addressed to Zhang Zejiang (email: zzjzzjzz@***) 1. chengdu institute of organic chemistry Chinese Academy of Sciences 610041 Chengdu China 2. Sichuan Fire Research institute of Public Security Ministry 611830 Chengdu China 3. Graduate School of the chinese academy of sciences 100039 Beijing China

The coating process of a nano-scale SiO2 film on the nanocrystalline Mg-Al layered double hydroxides via a sol-gel process was investigated. The uniform and dense SiO2film with a thickness of about 5 nm on the nano-LDHs particles was characterized by the solubility test in the dilute HNO3 or HCl acid, TEM and FT-IR, XRD, TG and DSC. The chemical shifts of binding en- ergies of Al 2p, Mg 2p, Si 2s and O 1s on the coated particles indicate that the coating of the SiO2 nano-film on the surface of the nano-LDHs proceeds through the formation of Mg-O-Si and Al-O-Si bonds. The thermal analysis shows that both the SiO2-coated nano-LDHs and the nano-LDHs have a similar mass loss process, in which there are three obvious stages of mass loss in the temperature range of 40—700℃. Furthermore, the more the coatedamount of SiO2on the surface of the nano-LDHs is, the less the mass loss of the samples is at 700℃.The nano- LDHs have two obvious endothermic peaks at 244.67℃ and 430.13℃, whose corresponding heat absorption capacities are 412.28 J/g and 336.30 J/g, respectively. In contrast, the coated nano-LDHs have only one endothermic peak at 243.60℃ with a heat absorption capacity of 221.25 J/g.

关键词： layered double hydroxides, nanocrystalline, silica, coating.

IN SITU INTERFEROMETRIC STUDY ON THE GELATION PROCESS OF POLYACRYLIC ACID GELS

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chinese Journal of Polymer Science 2000年第4期18卷 373-377页

作者： Ying Guan Qiang Chen Xian-min Zhang Yu-xing Peng Jian Xu Polymer Physics Laboratory, Center for Molecular Science, institute of chemistry, chinese academy of sciences, Beijing 100080, china Department of Information & Electronic Engineering, Zhejiang University, Hangzhou 310027, china chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china chinese Acad Sci Inst Chem Ctr Mol Sci Polymer Phys Lab Beijing 100080 Peoples R China Zhejiang Univ Dept Informat & Elect Engn Hangzhou 310027 Peoples R China chinese Acad Sci Chengdu Inst Organ Chem Chengdu 610041 Peoples R China

In situ interferometry was used to investigate the gelation process of polyacrylic acid (PAA) gels. The basic principle of the in situ interferometry technique is illustrated. It can give sufficient information for non-destructive and successful investigation of the whole gelation process. The effect of initiator concentration on the gelation process was studied. The polymerization rate of AA increases with increasing initiator concentration. The error arising from the thermal effect in the gelation process can be neglected.

关键词： in situ interferometry gelation polyacrylic acid

Study on fire-retardant nanocrystalline Mg-Al layered double hydroxides synthesized by microwavecrystallization method

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Science china chemistry 2004年第6期47卷 488-498页

作者： ZHANG Zejiang1, XU Chenghua1, QIU Fali1, MEI Xiujuan2, LAN Bin2 & ZHANG Shuosheng2 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. Sichuan Fire Research institute of Public Safety Ministry, chengdu 611830, china 1. chengdu institute of organic chemistry Chinese Academy of Sciences 610041 Chengdu China 2. Sichuan Fire Research institute of Public Safety Ministry 611830 Chengdu China

Nanocrystalline Mg-Al layered double hydroxides with the particle size being 10—40 nm were firstly prepared by the technology of the microwave-crystallization and the vari- able-speed addition of the alkali. The obtained samples were characterized by TEM and XRD. The roles of the microwave and addition rate of the alkali were also discussed in the present work. The thermal decomposition activation energy of the nano-LDHs was calculated according to their TG, DTG and DSC curves by the Ozawa method. The results showed that the thermal decom- position of the nano-LDHs had four steps. Thereby the decomposition model of the nano-LDHs was supposed according to the analysis of their thermal decomposition. After PS, ABS, HDPE and PVC were filled with the nano-LDHs, their LOI values could be increased up to 28, 27, 26 and 33, respectively. When the fire-retardant coating contained 1.9% of the nano-LDHs that was 0.27 times the dosage of the conventional TiO2, its fire endurance time reached 32.75min that was 7.05 min longer than that of the best coating containing TiO2 according to the model big-panel combustion test method.

关键词： layered double hydroxides, nanocrystal, microwave synthesis, thermal decomposition, fire-retardant performance.

Preparation of Pt/K_2La_2Ti_3O_(10) and its photo-catalytic activity for hydrogen evolution from methanol water solution

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Science china chemistry 2006年第2期49卷 162-168页

作者： CUI Wenquan1,3, LIU Li2, FENG Liangrong1, XU Chenghua1, LI Zijian1, Lü Shaojie1 & QIU Fali1 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. chemistry Department, Sichuan University of Science & Engineering, Zigong 643033, china 3. Graduate School of the chinese academy of sciences, Beijing 100039, china Correspondence should be addressed to Qiu Fali 1. chengdu institute of organic chemistry Chinese Academy of Sciences Chengdu 610041 China 3. Graduate School of the chinese academy of sciences Beijing 100039 China 2. chemistry Department Sichuan University of Science & Engineering Zigong 643033 China

A layered perovskite-type oxide K2La2Ti3O10 was prepared with high-temperature solid-state reaction, and characterized with X-ray diffraction (XRD) and ultraviolet-visible diffuse re-flectance spectroscopy (UV-Vis DRS). Platinum was loaded onto K2La2Ti3O10 as a co-catalyst with different methods. The dispersion of platinum on K2La2Ti3O10 was determined with HOT method. The photocatalytic activity of Pt/K2La2Ti3O10 was studied. This catalyst showed much higher activity in hydrogen evolution reaction than Ni/K2La2Ti3O10. The effects of different amounts of loaded platinum and several preparation methods were evaluated. The best achieved hydrogen evolution rate was 233.88 μmol·h?1 by Pt(2%)/K2La2Ti3O10. A possible band structure and mechanism were discussed based on the results.

关键词： photocatalysis hydrogen platinum K_2La_2Ti_3O_(10) support

Synthesis,thermal decomposition and crystal structure of copper(Ⅱ)α,β-unsaturated carboxylate with urea

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chinese Science Bulletin 1999年第7期44卷 602-605页

作者： WANG Yaoyu, SHI Qian, SHI Qizhen, GAO Yici and ZHOU Zhongyuan Department of chemistry, Northwest University, Xi’ an 710069, china Department of chemistry, Lanzhou University , Lanzhou 730000, china chengdu institute of organic chemistry , chinese academy of sciences , chengdu 610041, china

A detailed synthesis is described for binuclear cage ternary complexes Cu2A4 [（NH2）2CO]2, where A = CH2 =CH—COO- and CH2 =C（CH3）—COO-. Elemental analysis and thermal analysis have been investigated. The molecular structure of Cu2 （CH2 = CH—COO）4[（NH2）2CO]2 was determined by single crystal X-ray diffraction. The material forms blue crystal with tetragronal symmetry, space group P42/n, a = b = 1. 239 35（6） nm, c = 1. 398 05 （16） nm, Z = 4. There exists, a magnetic exchange interaction between the two paramagnetic Cu atoms. The Cu—Cu bond length is 0.260 94 nm.

关键词： copper(Ⅱ) α β-unsaturated carboxylate urea ternary complex thermal decomposition crystal structure.