助剂Fe对Ir/SiO2催化剂的巴豆醛选择性加氢性能的影响

以SiO2为载体采用分步浸渍法制备了Fe/Ir/SiO2催化剂,考察了助剂Fe对Ir/SiO2催化剂气相巴豆醛选择性加氢性能的影响.采用X射线粉末衍射(XRD)、CO化学吸附、H2-程序升温还原(H2-TPR)和拉曼光谱(Raman)等技术对催化剂进行了表征.结果表明,助剂Fe能有效提高Ir/SiO2催化剂的巴豆醛转化率和巴豆醇选择性.Fe含量为0.087%的0.087Fe/Ir/SiO2催化剂的反应性能最佳,反应进行9 h的巴豆醛转化率36.9%,巴豆醇选择性83%.随着催化剂CO吸附量的下降(Fe覆盖的增加),催化剂的转换频率(turn over frequency,TOF)明显增加,这表明Fe促进Ir/SiO2催化剂表面活性位的加氢活性.然而,Fe的掺杂使得Ir/SiO2催化剂存在明显的活性下降现象,归因于Fe导致Ir/SiO2催化剂表面积炭和CO中毒.     

以D-樟脑酸与1,4-二（咪唑-1-基）丁烷为配体构筑的两个配位聚合物的结构与磁性

水热合成了2个以D-樟脑酸(D-H2cam)与1,4-二(咪唑-1-基)丁烷(1,4-bimb)为配体的配位聚合物:[Co(D-cam)(1,4-bimb)]n·4nH2O(1)和[Ni(D-cam)(1,4-bimb)]n(2)。通过X-射线单晶衍射,元素分析,红外光谱,XRD分析,热重,和磁性分析对其结构进行了表征。测定了这两个聚合物的磁性。结构分析表明,1为P2空间群,其链状结构由氢键作用连接形成二维结构;2为Pna21空间群,呈四重穿插的dia网络结构。     

Synthesis and Insecticidal Evaluation of Novel Phthalic Diamides Containing 1,2,3‐Triazoles via Click Reaction

A series of novel phthalic diamide derivatives containing 1,2,3‐triazole moiety were synthesized using one‐pot click chemistry approach and characterized by ¹H NMR and HRMS. The insecticidal activity against armyworm (Mythimna separata), Tetranychu scinnabarinus and cowpea aphid (Aphis craccivora) was evaluated. Compounds 4II‐a and 4II‐i showed 50% insecticidal activity against armyworm (Mythimna separata) at the concentration of 4 mg/L and one‐third of the compounds had moderate activity against Tetranychus cinnabarinus at 500 mg/L.     

A ladder conjugated polymer transducer for solid-contact Cu2+-selective electrodes

In recent years, there has been a pronounced interest in solid-contact ion-selective electrodes （SC-ISEs）, with emphasis on the use of conducting polymers as ion-to-electron transducer. In this work, a ladder conjugated polymer, thieno[3,2-b]thiophene （LCPT）, was investigated in fabricating Cu2＋-selective electrodes for the first time. The resulting electrodes were characterized by electrochemical impedance spectroscopy （EIS）, chronopotentiometry, and the water layer test. Results proved that the active LCPT facilitates the ion-to-electron transduction, and avoids the detrimental aqueous layer formed at the interface of SC-ISEs.     

碳纤维基能源器件研究和应用进展

半个多世纪以来,碳纤维及碳纤维增强复合材料因其优异的力学性能、比强度、比模量、轻质、导电性以及热/化学稳定性,逐渐成为航空航天、建筑、运输、生物医用、体育用品以及电子电气等诸多应用领域一类非常重要的高性能结构材料。近二十多年来,得益于纳米材料与技术以及高效可再生能源器件的迅速发展,力学性能突出的碳纤维(包括工业化碳纤维、碳纤维织物、碳纳米纤维以及碳纳米管纤维等)凭借高的导电性、电化学特性、多孔以及表面可修饰性等优点,开始作为良好的电极材料应用于多种电化学能源器件与光电转换能源器件中,并得到了广泛的研究。本文首次综述了碳纤维基能源器件的研究进展,从认识碳纤维的发展历史与应用出发,介绍了碳纤维的表面功能化与电极制备的相关基础知识,重点综述了当前国内外碳纤维能源器件的发展概况,详细介绍了碳纤维作为功能电极材料在燃料电池、微生物燃料电池、锂离子电池、电化学电容器以及太阳能电池等领域的研究和发展概况。最后,通过分析当前碳纤维能源器件研究领域的现状,对该领域在材料制备工艺、电极设计、器件性能优化与器件集成技术等方面面临的挑战和未来研究方向进行了预测和探讨。     

3D amorphous carbon and graphene co-modified LiFePO4 composite derived from polyol process as electrode for high power lithium-ion batteries

Amorphous carbon and graphene co-modified LiFePO_4 nanocomposite has been synthesized via a facile polyol process in connection with a following thermal treatment.Various characterization techniques,including XRD.Mossbauer spectra,Raman spectra,SEM,TEM,BET,O_2-TPO,galvano charge-discharge,CV and EIS were applied to investigate the phase composition,carbon content,morphological structure and electrochemical performance of the synthesized samples.The effect of introducing way of carbon sources on the properties and performance of LiFePO_4/C/graphene composite was paid special attention.Under optimized synthetic conditions,highly crystalized olivine-type LiFePO_4was successfully obtained with electron conductive Fe_2P and FeP as the main impurity phases.SEM and TEM analyses demonstrated the graphene sheets were randomly distributed inside the sample to create an open structured LiFePO_4 with respect to graphene,while the glucosederived carbon mainly coated over LiFeP04 particles which effectively connected the graphene sheets and LiFePO_4 particles to result in a more efficient charge transfer process.As a result,favorable electrochemical performance was achieved.The performance of the amorphous carbon-graphene co-modified LiFePO_4 was further progressively improved upon cycling in the first 200 cycles to reach a reversible specificcapacity as high as 97 mAh·g~(-1) at 10 C rate.     

Adsorption separation performance of H2/CH4 on ETS-4 by concentration pulse chromatography

To exploit an effective adsorbent to separate hydrogen and methane, microporous titanium silicate molecular sieve NaETS-4 was synthesized and modified by strontium. The adsorption characteristics and diffusion behaviors of the prepared titanosilicate molecular sieve were studied by concentration pulse chromatography. And the effects of ion-exchange and dehydration temperature on adsorbent structure and gas diffusion were also discussed. The results showed that the thermal stability and Henry＇s Law constants were enhanced and micropore diffusivity decreased after exchanging Na＋ with Sr2＋. With the increase of dehydration temperature, Henry＇s Law constant and micropore diffusivity of CI-I4 decreased in both NaETS-4 and SrETS-4. While for 1-12 in SrETS-4, the increase of Henry＇s Law constant and the decrease of diffusion rate can be attributed to the shrinks of pore diameter resulting from the relocation of Sr2＋. Correspondingly, the kinetic selectivity of H2/CH4 reached 8.91 indicating its potentiality in separating H2 and CH4.     

黄油中8种类固醇激素的液相色谱/串联质谱检测

建立了黄油中雌酮、α-雌二醇、β-雌二醇、雌三醇、睾酮、表睾酮、孕酮和丙酸睾酮8种类固醇激素的凝胶渗透色谱(GPC)-液相色谱/串联质谱(LC-MS/MS)检测方法。样品用乙酸乙酯-环己烷(1∶1,V/V)提取,提取液经GPC柱净化除脂,GPC浓缩液采用C18色谱柱(100 mm×2.0 mm i.d.,3.0μm)分离,以乙腈和水为流动相进行梯度洗脱,电喷雾电离多反应监测模式进行定性和定量分析。8种类固醇激素以基质匹配外标法定量,药物在1.0~20.0μg/kg线性范围内相关系数(r)均大于0.999;方法检出限(S/N=3)为0.04~0.30μg/kg,定量限LOQs(S/N=10)为1.0μg/kg;添加水平为1.0,2.0,4.0μg/kg时,回收率范围在64.1%~110%之间;相对标准偏差(RSD)小于11%。结果表明,本方法准确、可靠,满足黄油中8种类固醇激素的检测分析要求。     

Synthesis,Crystal Structure and MMCT Property of a New Mixed-valence Cyanide-bridged Binuclear Complex

A new mixed-valence cyanide-bridged complex, Br3Fe(μ-NC)RuBr(dppm)2(dppm = bis(diphenylphosphino)methane), was obtained through the reaction between trans-(dppm)2ClRuCN and FeBr3. Its crystal structure was characterized. Electronic absorption spectra indicate the existence of metal-to-metal charge transfer(MMCT) and this complex is Class Ⅱ mixed valence complexes according to the classification of Robin and Day. Magnetic analysis shows it is paramagnetic.     

Synthesis and Antibacterial Activity of Novel 5,5′-(Pyridine-2,6-Diyl)bis(4-Arylideneamino-3-Mercapto-1,2,4-Triazole)-Related Derivatives

The reaction of 5,5′-(pyridine-2,6-diyl)bis(4-amino-3-mercapto-1,2,4-triazole) with various aromatic aldehydes in acetic acid yielded the corresponding 5,5′-(pyridine-2,6-diyl)bis(4-arylideneamino-3-mercapto-1,2,4-triazole) derivatives. The structures of the synthesized compounds as well as their intermediates were confirmed by elemental analysis, infrared spectra, ¹H NMR spectra and mass spectra studies. All the synthesized title compounds were screened for their antibacterial activities, and the preliminary results revealed that some of them showed good activities against Escherichia coli and Pseudomonas aeruginosa.