5-异烟酰胺异钛酸构筑的Cu(Ⅰ)-Eu和Ni(Ⅱ)-Eu化合物的合成、晶体结构和性质研究

利用不同过渡金属盐在溶剂热中合成了2个新型杂核化合物{[CuEu₂（INAIP）₃（HCOO）（H₂O）₃]·3H₂O}_n（1）和{[NiEu₂（INAIP）₄（H₂O）₄]·4H₂O}_n（2）（INAIP=异烟酰胺吡啶基异酞酸根）,并对其进行了元素分析、IR及X-射线衍射法表征。晶体结构研究表明：配合物1和2都属于三斜晶系,P1空间群。晶胞参数：配合物1a=1.0887（3）nm,b=1.5158（4）nm,c=1.5644（2）nm,V=2.3332（10）nm³,Z=2,D_c=1.955g·cm^-3,μ=3.203mm^-1,F（000）=1352,R_int=0.027,R₁=0.0505,wR₂=0.1309。配合物2a=1.0134（3）nm,b=1.0836（6）nm,c=1.3741（2）nm,V=1.4530（9）nm³,Z=1,D_c=1.878g·cm^-3,μ=2.554mm^-1,F（000）=818,R_int=0.0458,R₁=0.0341,wR₂=0.0869。配合物1是由配体异烟酰胺吡啶基异酞酸连接而成的三维二重贯穿sqc27拓扑结构,而配合物2是由配体异烟酰胺吡啶基异酞酸连接稀土铕离子形成二维层状结构,该二维层通过Ni-O和Ni-N键连接成三维非贯穿网络结构。配合物1和2具有典型的稀土铕离子红色荧光和高的热稳定性。     

苯二甲酸衍生物及含氮配体构筑的两个镍配位聚合物的合成、晶体结构与热稳定性研究

使用硝酸镍分别与2个含取代基的苯基二羧酸3-硝基邻苯二甲酸（3-NPAH₂）和5-溴间苯二甲酸（H₂BIPA）以及2个刚性含氮配体4,4’-联吡啶（4,4’-bipy）、1,4’-二咪唑基二苯（L=1,4’-bis（imidazol-yl）benzene）在水热条件下合成了2个镍配位聚合物,即,[Ni（3-NPA）（4,4’-bipy）（H₂O）]_n（1）和[Ni（BIPA）（L）]_n（2）。表征了2个化合物的红外光谱、元素分析、热重、X-射线单晶衍射以及X-射线粉末衍射。化合物1是三斜晶系,P1空间群,含有[Ni（OCO）₄Ni]双核单元,该双核单元再通过4,4’-联吡啶连接而成一个二维单层结构。层与层之间通过羧酸氧原子与配位水分子之间产生氢键作用。化合物2是单斜晶系,P2₁/c空间群,含有[Ni₂（COO）₂]双核单元,该双核单元进一步通过BIPA^2-构成了一个双链结构,该双链再通过1,4’-二咪唑基二苯桥联配体连接形成了一个三维框架结构。此外,热重分析结果显示化合物2具有较高的热稳定性。     

微波辅助合成石墨烯/氧化镍复合材料及其表征

本文通过微波辅助的方法,快速而有效地在热膨胀石墨烯(RG)的缺陷上原位合成氧化镍纳米颗粒,形成石墨烯/氧化镍复合材料(RG/NiO)。利用X-射线衍射(XRD),拉曼光谱(Raman),傅里叶变换红外(FTIR),扫描电镜(SEM),透射电镜(TEM),热重-差热(TGA-DSC)对所制备样品的结构、形貌和NiO含量在复合材料中的含量进行表征。结果表明,热膨胀石墨烯层数约7~8层,层间距约为0.35nm,缺陷多,在水热和微波处理后抗氧化性明显变差。复合材料中氧化镍颗粒平均粒径为25nm,均匀而密集地分散在石墨烯平面上,同时在复合材料中的含量为19.8%。     

碳钢低压冷喷涂铝涂层的海水耐蚀性

本文以Al和10%体积比Al2O3的混合粉末为原料,使用便携式低压冷喷涂设备,在Q235碳钢基体上喷涂了Al涂层. 测试涂层自腐蚀电位及动电位极化曲线,结合扫描电镜观察涂层表面及截面微观形貌,研究了低压冷喷涂Al涂层在海水中电化学腐蚀行为,并与高压冷喷涂和热喷涂铝涂层的耐蚀性比较. 结果表明,低压冷喷涂铝涂层结构较为致密,其耐蚀性比高压冷喷涂铝涂层的略低,而明显优于热喷涂铝涂层.     

Spectral and Thermal Studies of Some New Metal Complexes Derived from N-[(Phenylamino)Thioxomethyl] Hydrazinocarbonyl Methyl Pyridinium Chloride (PTHMPC)

New metal complexes derived from the reaction of N-[(phenylamino)thioxomethyl] hydrazino carbonyl methyl pyridinium chloride (H₂L; PTHMPC) with some metal salts of the general formula MX₂ [(X = Cl^? and/or CH₃COO^?; M = Cd(II), UO₂(II), Mn(II) and Zr(IV)] were synthesized and characterized by elemental analyses, spectral analyses (IR, UV-vis., ¹H NMR), thermal analyses (TGA, DTG), and conductance and magnetic measurements. The results showed that the ligand exists in metal complexes either in the keto form or in the enol form. Moreover, the IR spectral data suggest that the acetate ion behaves in a monodentate manner. Semi-empirical calculations ZINDO/1, PM3, and AM1 have been used to study the molecular geometry and the harmonic vibrational spectra of the ligand and its metal complexes with the purpose of assisting the experimental assignment of the complexes. Generally, there is an agreement between the observed and the calculated spectra. Finally, the thermodynamic parameters (ΔE*, ΔH, ΔG, and ΔS) have been calculated from the data of thermal analyses (TGA and DTG).

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Chemical Preparation,Thermal Behavior,Kinetic, and IR Studies of MnK4(P3O9)2.2H2O,Crystallographic Data of a New Cyclotriphosphate MnK4(P3O9)2, and Quantum Chemical Calculations for the P3O3− 9 Ion

Abstract

Chemical presparation, thermal behavior, and infrared (IR) studies are discussed for the cyclotriphosphate MnK₄(P₃O₉)₂.2H₂O and its anhydrous form MnK₄(P₃O₉)₂. The total dehydration of MnK₄(P₃O₉)₂.2H₂O, between 200 and 550 °C, leads to its anhydrous form MnK₄(P₃O₉)₂. MnK₄(P₃O₉)₂ is a new cyclotriphosphate crystallizing in the rhombohedral system and is stable until its melting point at 560 °C. The thermal behavior of MnK₄(P₃O₉)₂.2H₂O has been investigated and interpreted by comparison with IR absorption spectrometry and X-ray diffraction experiments. Two different methods, Ozawa and KAS (Kissinger-Akahira-Sunose), were selected in studying the kinetics of thermal behavior of the title compound. Quantum chemical calculations were made for the P₃O ^3? ₉ ion.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.

GRAPHICAL ABSTRACT     

Microbial Screening of Copolymers of N‐Vinylimidazole with Phenacyl Methacrylate: Synthesis and Monomer Reactivity Ratios

N‐vinylimidazole (VIM), and phenacyl methacrylate (PAMA) copolymerized with different feed ratios using 1,4‐dioxane as a solvent and α,α'‐azobisisobutyronitrile (AIBN) as an initiator at 60°C. Structure and composition of copolymers for a wide range of monomer feed were determined by elemental analysis (content of N for VIM‐units) and by Fourier transform infrared spectroscopy through recorded analytical absorption bands for VIM (670 cm^?1 for C‐N of imidazole ring) and PAMA (1730 cm^?1 for C?O of ester group) units, respectively. Monomer reactivity ratios for VIM (M₁)‐PAMA (M₂) pair were determined by the application of conventional linearization methods such as Fineman‐Ross (F‐R) and Kelen‐Tüdös (KT) and a nonlinear error invariable model method using a computer program RREVM. The molecular weights (_w and _n) and polydispersity indices of the polymers were determined using gel permeation chromatography (GPC). Thermal behaviors of copolymers with various compositions were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Also, the apparent thermal decomposition activation energies (ΔE_d) were calculated by Ozawa method using the SETARAM Labsys TGA thermobalance. The antibacterial and antifungal effects of polymers were also tested on various bacteria, fungi and yeast.     

Dynamic Release of Propranolol HCl from Cationic Ion–Exchanger–Loaded Calcium Alginate Beads

The dynamic release of drug propranolol HCl from the propranolol HCl–resin complex (PRC) loaded calcium alginate beads has been studied in the buffer media of pH 1.2 at the physiological temperature 37°C. The PRC encapsulated beads demonstrated nearly 58.04% release while naked PRC particles released 98.00% drug in 24 h in the gastric fluid. The amount of drug released was found to increase with and decrease in the amount of sodium alginate in the beads. Similarly, with the increase in the amount of entrapped PRC particles within the beads, the quantity of drug released was also observed to increase. The degree of crosslinking of beads also affected the release kinetics. Interestingly, the release from naked PRC particles followed ‘first‐order’ kinetics while PRC particles, entrapped in calcium–alginate beads, exhibited ‘diffusion controlled’ release behavior as indicated by liner nature of fractional release vs. √t plot.