Catalytic Combustion of Methane over Ti-Pillared Clay Supported Copper Catalysts

A natural montmorillonite, produced from Laiyang of Shandong Province, was pillared by Tipolycations to form Ti-pillared clay (Ti-PILC), and characterized by BET surface area, infrared spectra and thermal analysis. The characterization results show that Ti-PILC has a larger surface area and more hydroxyl groups than that of the natural clay, thus was used as the catalytic carriers to prepare supported Cu catalysts (Cu/TiopILC). The 20%Cu/Ti-PILC with 10mmol/g of Ti/clay shows a high catalytic performance of methane combustion in the temperature range of 400-500℃.     

Extraction of the Volatile and Semivolatile Compounds in Seeds of Cuminum cyminum L. Using Hydrodistillation Followed by Headspace-Ionic Liquid-Based Single-Drop Microextraction

Hydrodistillation (HD) coupled with headspace single-drop microextraction by using ionic liquid (IL) as the extraction solvent, followed by gas chromatography analysis technique, was successfully developed to determine the volatile and semivolatile compounds in seeds of Cuminum cyminum L. In the proposed method, a 1.5-??L microdrop of 1-octyl-3-methylimidazolium hexafluorophosphate, working as the extraction solvent was suspended in the headspace of a 50-mL round-bottom sample flask. After extracting for 30?min, both IL and target analytes were injected into the gas chromatographic system by thermal desorption for 5?s under 240?°C. Then, the IL was retracted back to the microsyringe. Thus, the capillary column should not be contaminated and a clean chromatogram was obtained. The parameters affecting extraction performance were investigated and optimized. The extraction efficiency of the proposed method was compared with that of HD, which is a standard extraction method. The contents of constituents in the extract obtained by the proposed method were close to those obtained by HD. It seems to be an environmentally friendly, time-saving, high efficiency and low solvent consumption technique and would be useful, especially for aromatic plants analysis.     

Construction of 1D and 2D Zinc Coordination Polymers Based on Organic Carboxylate Anions and Flexible Imidazole‐Containing Ligand

Two novel zinc coordination polymers {[Zn(PhCOO)₂(bmix)]}_n 1 and {[Zn(ada)(bmix)]·(H₂O)₂}_n 2 (bmix = 1,4‐bis(2‐methylimidazole‐1‐ylmethyl)benzene, H₂ada = adipic acid), were obtained by the hydrothermal reactions of bmix and zinc acetate with two carboxylate anions, respectively. Structural analyses show that complex 1 possess a one‐dimensional helix chain structure, 2 takes two‐dimensional corrugated (4,4) layer motif. The structural differences of two complexes indicate that organic carboxylate anions play important roles in the formation of such zinc(II) coordination architectures.     

Improving dispersion and integration of single‐walled carbon nanotubes in epoxy composites by using a reactive noncovalent dispersant

Uniform dispersion and strong interfacial interaction are two critical prerequisites for application of single‐walled carbon nanotubes (SWNTs) in polymer composites. To endow the composites with multifunctional feature, no damage on the chemical/electronic structure of SWNTs is also usually required. With these ends in view, two epoxide‐containing pyrene derivatives (EpPys) were designed, synthesized, and used as reactive noncovalent dispersants for developing multifunctional epoxy/SWNT composites. One having longer chain length between epoxide group and pyrene moiety, that is, EpPy‐16, shows higher dispersing efficiency and provides the nanotube dispersion with better stability, thus picking up for subsequent studies. Systematic characterization on SWNT/EpPy‐16 hybrid demonstrates that 13.2 wt % of EpPy‐16 is adsorbed on the SWNT surface through strong π‐stacking interaction, and intrinsic electronic structure of SWNTs is basically reserved. The solution‐based process adopted here preserves the good SWNT dispersing state in dispersion into the composites. Simultaneously, enhanced interfacial interaction is also realized by using EpPy‐16, which interacts noncovalently with SWNT but connects covalently to epoxy network. As a result, the composites acquire 37 and 22% increments in tensile strength and Young's modulus, respectively, relative to that of neat resin. A low‐electrical percolation threshold of 0.1 wt % SWNTs and improved thermal properties were also observed. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

分光光度法测定果蔬中残杀威残留量

在碱性条件下残杀威水解生成酚盐,在盐酸介质中对氨基苯磺酸与亚硝酸根发生重氮化反应,上述所得酚盐和重氮化产物在氨性溶液中偶联生成偶氮染料,此偶联产物的最大吸收波长为427nm,据此提出了分光光度法测定果蔬中残杀威含量的方法。残杀威的质量浓度在0.17～2.04mg·L-1范围内与其吸光度呈线性关系,检出限(3s/k)为0.03mg·L-1。方法用于测定果蔬中残杀威的含量,相对标准偏差(n=5)在0.3%～0.7%之间,加标平均回收率为96%。     

二维氧化钛纳米页

单层氧化钛纳米页(titania nanosheets)是一种厚度仅为0.7 nm的新型二维纳米材料,具有许多不同于块体氧化钛的优异性质,如:高各向异性、单晶性质、胶体和聚电解质特性、大比表面积、高表面能和量子尺寸效应等。在光电转换、磁光效应、高介电常数器件、电化学能量储存、湿敏传感器、自清洁和光催化等领域极具应用前景。本文首先总结了氧化钛纳米页的基本性能,如:光吸收性能、光致发光性能、光电化学性能、光诱导亲水性能和晶相转变温度差异等,概述了氧化钛纳米页的制备及组装方法,接着分别以薄膜片、纳米管、中空微球、超薄多层复合薄膜为代表,介绍了氧化钛纳米页组装得到的新型材料及其特点,然后介绍了氧化钛纳米页的掺杂改性,从拓宽光吸收带边、提高电子迁移速率和提高磁光效应三个角度,归纳总结了离子掺杂与氧化钛纳米页性能之间的关系,最后对氧化钛纳米页未来的研究发展趋势提出了展望。     

海绵Spongia sp.化学成分的研究（I）

应用气相色谱－质谱联用技术从海绵Ｓｐｏｎｇｉａ ｓｐ．中分离鉴定出４个化学成分：１．－氯－２,２－二对氯苯基乙烯（ＤＤＭＵ,Ｉ）、１,１－二氯－２,２－二对氯苯基乙烯（ＤＤＥ,Ⅱ）、１,１－二氯－２,２－二对氯苯乙烷（ＤＤＤ,Ⅲ）和角鲨烯（Ⅳ）。前３个化合物是首次从Ｓｐｏｎｇｉａ属海绵中分离得到。     

Rare-Earth–Transition-Metal Organic–Inorganic Hybrids Based on Keggin-type Polyoxometalates and Pyrazine-2,3-dicarboxylate

Five rare-earth–transition-metal (RE–TM) heterometal organic–inorganic hybrids based on Keggin-type silicotungstates and mixed ligands H2pzda (pzda=pyrazine-2,3-dicarboxylate) and en (en=ethylenediamine) (enH2)[Cu(en)2(H2O)]2{[Cu(en)2][Cu(en)2(H2O)][(α-SiW11 O39)RE(H2O)(pzda)]}2⋅n H2O (n≈4; RE=YIII ( 1 ), DyIII ( 2 ), YbIII ( 3 ), and LuIII ( 4 )) and [Cu(en)2(H2O)]2{[Cu(en)2]2[Cu(pzda)2][(α-H2SiW11O39)Ce(H2O)]2}⋅n H2O ( 5 ; n≈8) have been hydrothermally synthesized and structurally characterized. Compounds 1–5 all contain the dimeric mono-RE substituted Keggin [RE(α-SiW11O39)]210− subunits linked by H2pzda ligands. Interestingly, 1–4 exhibit discrete structures, in which the H2pzda ligand acts as a tetradentate ligand to bind the RE and Cu cations, whereas 5 displays a 1D double-chain architecture, in which the H2pzda ligand adopts a new pentadentate mode to connect the Ce and Cu cations. To our knowledge, 1–5 represent the first monovacant Keggin-type silicotungstates containing both RE–TM heterometals and mixed ligands. The luminescence of 2 is derived from the combination of the DyIII cations and H2pzda ligands, whereas the luminescence properties of 1 and 3–5 are attributable to the H2pzda ligands.     

New sulfonated engineering polymers via the metalation route. II. Sulfinated/sulfonated poly(ether sulfone) PSU Udel and its crosslinking

New mixed sulfinated/sulfonated polysulfone PSU Udel has been produced by partial oxidation of sulfinated PSU with NaOCl. From the mixed sulfinated/sulfonated PSU, thin crosslinked polymer films have been produced by S-alkylation of the residual sulfinate groups with α,ω-diiodoalkanes having 4–10  (CH₂) units. The advantages of the partial oxidation process using NaOCl are as follows: (1) The desired oxidation degree can be adjusted finely. (2) No side reactions take place during oxidation. (3) The partially oxidized polymers is stable at ambient temperature. By variation of the oxidation degree of the sulfinated/sulfonated prepolymer and by variation of the chain length of the diiodo crosslinker, crosslinked membranes with a large range of properties in terms of ionic conductivity, swelling, and permselectivity have been produced. The partially oxidized polymers have been characterized by redox titration, ¹H-NMR, and FTIR. The crosslinked membranes have been characterized in terms of ionic conductivity (resistance), permselectivity, and swelling in dependence on ion-exchange capacity and oxidation degree of the prepolymers. In addition, the thermal stabilities of the membranes have been determined by TGA, and FTIR spectra have been recorded on the crosslinked films. Selected membranes show low ionic resistances, low swelling, and good temperature stability which makes them promising candidates for application in (electro)membrane processes. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1441–1448, 1998     

红外光谱法研究LB膜中的分子取向

The structure information of orientation and packing of molecular chains can be obtained from infrared transmission and reflection-absorbance (RA) spectra. In the present paper, on the basis of Umemura et al., their FORTRAN program of minicomputer was developed and can be run on 486 personal computer. By comparison of infrared transmission and RA intensities, surface enhancement factors and molecular orientation angle were calculated using the above program, and the influence of complex refractive index, angle of incidence, and thickness of LB film were discussed. These results are consistent with that of Umemura et al.