Vibrational Spectra of Thiazole-2-Carboxylic Acid and Thiazole-2-Carboxylate Ion

The i-r. spectra of thiazole-2-carboxylic acid and thiazole-2-carboxylate ion as CsI pellets and Nujol mull as well as Raman spectrum of an aqueous solution of the salt have been investigated. Most vibrations have been assigned on the basis of group frequencies and by correlation between the spectra of both molecules. The -COOH characteristic vibrations have been assigned as vibrations of the intermolecularly associated species.     

Preparation and Characterization of a Bipolar Membrane Modified by Copper Phthalocyanine 16-Carboxylic Acid and Acetyl Ferrocene

A bipolar membrane (BPM) of carboxymethyl cellulose (CMC) and chitosan (CS) with superior performance was prepared based on the macromolecules containing metal elements. A carboxymethyl cellulose cation layer was modified by copper phthalocyanine 16-carboxylic acid (CuPc(COOH)₁₆) to improve its ion exchange capacity as well as cation transfer rate and promote water splitting at the intermediate layer. Chitosan was crosslinked with acetyl ferrocene to prepare the anion layer. A casting method was used to prepare the BPM which showed excellent physical and chemical properties after modification. To improve the compatibility of the anion-exchange layer and cation-exchange layer, polyethylene glycol (PEG) was blended with both the CMC and CS. Scanning electron microscopy (SEM) images illustrated a structure that consisted of an anion layer and a cation layer that were closely combined with each other. The swelling results implied a proper hydrophilic performance and good shape stability in an alkali solution ([OH^?]≤10 mol·L^?1) of the BPM. After modification, the BPM with the metal elements exhibited good thermal stability, as shown by the thermogravimetry (TG) results. Compared with the BPM that was unmodified, both the AC impedance and the working voltage were decreased sharply. Furthermore, the modified BPM exhibited higher ion penetrability which is beneficial for its wide application.     

不同有机碱对铕-2-羟基喹啉-4-羧酸配合物发光性能的影响

分别在有机碱三乙胺、三丙胺和三丁胺的作用下,使用2-羟基喹啉-4-羧酸(H2hqc)与EuCl3·6H2O反应制备了3种配合物Eu(Hhqc)3(TEL)、Eu(Hhqc)3(TPL)和Eu(Hhqc)3(TBL)。通过元素分析、热重分析、摩尔电导率、紫外光谱、荧光光谱、荧光寿命和量子产率等对配合物进行了表征。所有配合物均在580,592,613,654,702 nm附近产生5条谱带,为Eu3+的特征发射,归属为5D0→7FJ(J=0,1,2,3,4)能级间的跃迁,荧光寿命分别为2.22,3.29,3.31 ms,量子产率分别为0.011,0.019,0.028。随着有机胺碳链长度的增加,配合物的荧光强度依次增大,表明有机碱参与了配合物的分子组成。     

Preparation of Poly (L-lactic Acid) Microsphere

Poly (L-lactic acid) (PLLA) microspheres were prepared by a solvent evaporation method based on an oil/water emulsion. The effect of the mass ratio of PLLA and poly(vinyl alcohol) (PVA) on the formation of the microspheres was discussed, and the influence of extraction speed of dichloromethane on the microsphere morphology was also studied. Moreover, the influences of the PLLA concentration and the volume ratio of water phase to dichloromethane phase were investigated. The results showed that stable microspheres can be obtained under the conditions that the mass ratio of PLLA to PVA is 20:1. Porous microspheres were obtained under faster evaporating speed of dichloromethane. The microsphere size increased with increasing PLLA concentration. The microsphere size also increased with the increase of the volume ratio of water phase to dichloromethane phase.     

Preparation and Characterization of Poly(Methyl Methacrylate) Coated TiO2 Nanoparticles

Titanium dioxide (TiO₂) nanoparticles were modified with poly(methyl methacrylate) (PMMA) to improve the dispersion stability of the nanoparticles in a dielectric medium and to reduce the density mismatch between TiO₂ and a dielectric medium for a microcapsule‐type electrophoretic display application. Nanoparticles were coated with PMMA by in situ dispersion polymerization. The PMMA‐coated TiO₂ nanoparticles were characterized by fourier transform‐infrared spectrometrey (FT‐IR), electrophoretic light scattering (ELS), and scanning electron microscopy (SEM). Density of PMMA‐coated TiO₂ nanoparticles was found to be dependent on the thickness of the PMMA coating on the nanoparticles. An increase of thermal stability of the PMMA layer and the contents of PMMA on the surface of the nanoparticles were measured via thermogravimetric analysis (TGA).     

铕-2-羟基喹啉-4-羧酸配合物的合成及光谱性能

以Eu3+为中心离子,2-羟基喹啉-4-羧酸(H2hqc)、1,10-菲罗啉(Phen)和三苯基氧磷(TPPO)为配体,合成了新型配合Eu(Hhqc)3(H2O)、Eu(Hhqc)3Phen(H2O)5和Eu(Hhqc)3TPPO(H2O)5.用元素分析和红外光谱对配合物进行了表征,IR表明配合物Eu(Hhqc)3Phen(H2O)5的Δν值大于钠盐Δν值,配合物中羧酸根以单齿方式配位.而配合物Eu(Hhqc)3(H2O)和Eu(Hhqc)3TPPO(H2O)5Δν值均小于钠盐的Δν值,表明配合物中羧酸根与Eu3+呈螯合双齿配位方式.室温下测定了配合物的荧光光谱,研究了它们的荧光性能.结果表明,配合物均在581,594,615,654和703nm附近产生五条谱带,为Eu3+的特征发射,归属为5 D0→7 FJ(J=0,1,2,3,4)能级间的跃迁,第二配体Phen和TPPO的引入对Eu3+的荧光发射有明显增强作用,且Phen效果更好.     

聚甲基丙烯酸甲酯-功能化多壁碳纳米管的制备及性能

"以羧基多壁碳纳米管、甲基丙烯酸甲酯作为原料,过氧化苯甲酰作为引发剂,采用原位聚合法制备聚甲基丙烯酸甲酯-功能化多壁碳纳米管．利用投射电子显微镜、扫描电子显微镜、核磁共振、傅立叶转换红外光谱,热重分析和拉曼光谱对合成产物进行分析表征．结果表明,聚甲基丙烯酸甲酯共价接枝到羧基碳纳米管表面,羧基碳纳米管的含量影响合成产物的表观形态．核磁共振研究表明聚甲基丙烯酸甲酯-功能化多壁碳纳米管在氘代氯仿中有一定的溶解性．"     

Preparation and Characterization of Composites Based on Poly (Butylene Succinate) and Poly (Lactic Acid) Grafted Tetracalcium Phosphate

Tetracalcium phosphate (TTCP, Ca₄(PO₄)₂O) was functionalized by poly (l-lactic acid) (PLLA) in order to improve the dispersion of TTCP particles in poly (butylene succinate) (PBS) matrices, and then a series of the PLLA grafted TTCP/PBS (g-TTCP/PBS) composites were prepared via melt processing. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), tensile analysis, differential scanning calorimetry (DSC), thermogravimetric analysis (DTG/TGA) and melt rheological analysis were used to investigate the structure and properties of the g-TTCP/PBS composites. The results revealed that l-lactide could be grafted onto the surface of TTCP, and the g-TTCP/PBS composites showed the best mechanical properties when the content of g-TTCP was 10 wt%. The crystallization temperature of g-TTCP/PBS composites tended to increase with the increase of g-TTCP contents. The functionalized particles played an important role in augmenting the thermal degradation rate and the complex viscosity of the composites due to their unique structure and the reasonable interfacial interaction between the particles and PBS matrix.     

Preparation and Characterization of Poly(L-lactic acid)/Polybutadiene Block Copolymers

A two-step process to prepare poly(L-lactic acid) (PLLA)/polybutadiene (PB) block copolymers was studied. Melt polymerization was used to prepare poly(L-lactic acid) terminated with hydroxy groups, at the same time hydroxy-terminated polybutadiene and 1,6-hexamethylene diisocyanate were employed to synthesize isocyanate-terminated polybutadiene (ITPB). Then PLLA and ITPB were reacted with different PB/PLLA weight ratios. Consequently, a series of PLLA/PB copolymers with linear or crosslinked chains was obtained. Viscosity of the linear copolymer was measured by an Ubbelohde viscometer. Swelling characteristics and crosslink density of the crosslink copolymer were investigated. Fourier transform infrared and proton nuclear magnetic resonance were used to characterize the structure of the copolymer, and dynamic mechanical analysis (DMA) was applied to characterize its thermal properties. Mechanical property measurements showed that a toughened PLLA polymer was synthesized. Atomic force microscope was utilized to characterize its micro-morphology.     

一种高电导率PVA聚合物电解质的制备与表征

通过溶液浇注法制备了一种polymer in salt型PVA KOH H2O聚合物电解质.对该电解质进行了X射线衍射、热性质及电化学性质测试与分析.X射线衍射显示PVA和KOH在聚合物电解质中均以非晶态存在.随着KOH含量的增加,聚合物的玻璃转化点温度逐渐上升,而电解质电导率也随之增加.该电解质的电化学窗口可达1.4V,阻抗测试显示当电解质组成PVA/KOH为1/3(质量比)时,室温电导率可达0.15S/cm,电导率与温度关系符合Arrhenius方程.该电解质热力学稳定性好,机械强度高、电化学性质优越.     

Optimization of Preparation Techniques for Poly(Lactic Acid-Co-Glycolic Acid) Nanoparticles

Microparticles and nanoparticles of poly(lactic acid-co-glycolic acid) (PLAGA) are excellent candidates for the controlled release of many pharmaceutical compounds because of their biodegradable nature. The preparation of submicron PLAGA particles poses serious challenges that are not necessarily present when preparing microparticles. We have evaluated several combinations of organic solvents and surfactants used in the formulation of PLAGA nanoparticles. Critical factors such as the ability to separate the nanoparticles from the surfactant, the ability to re-suspend the nanoparticles after freeze-drying, formulation yield and nanoparticle size were studied. The smallest particles were obtained using the surfactant/solvent combination of sodium dodecyl sulfate and ethyl acetate (65 nm) and the largest particles were obtained using poly(vinyl alcohol) and dichloromethane (466 nm). However, the optimal nanoparticles were produced using either acetone or ethyl acetate as the organic solvent and poly(vinyl alcohol) or human serum albumin as the surfactant. This is because the most critical measure of performance of these nanoparticles proved to be their ability to re-suspend after freeze-drying.     

卤代苯甲酸-TPTZ铽配合物的合成、表征及荧光性能

分别以对溴苯甲酸和对碘苯甲酸为第一配体,2,4,6.三吡啶基三嗪(TPTZ)为第二配体,以铽为中心,La3+、Y3+、Cd3+为掺杂离子,合成了8种铽及其掺杂配合物,对其进行了C、H、N元素分析及稀土络合滴定、紫外光谱、红外光谱和荧光光谱测定.推测配合物的组成为:Tb(P-BrBA)3(TPTZ)·2H2O和Tb(P-...     

Preparation and Characterization of Poly(Vinyl Alcohol) (PVA)/SiO2, PVA/Sulfosuccinic Acid (SSA) and PVA/SiO2/SSA Membranes: A Comparative Study

Abstract

New organic–inorganic nanocomposites based on PVA, SiO₂ and SSA were prepared in a single step using a solution casting method, with the aim to improve the thermomechanical properties and ionic conductivity of PVA membranes. The structure, morphology, and properties of these membranes were characterized by Raman spectroscopy, small- and wide-angle X-ray scattering (SAXS/WAXS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), water uptake (Wu) measurements and ionic conductivity measurements. The SAXS/WAXS analysis showed that the silica deposited in the form of small nanoparticles (～ 10?nm) in the PVA composites and it also revealed an appreciable crystallinity of pristine PVA membrane and PVA/SiO₂ membranes (decreasing with increasing silica loading), and an amorphous structure of PVA/SSA and PVA/SSA/SiO₂ membranes with high SSA loadings. The thermal and mechanical stability of the nanocomposite membranes increased with the increasing silica loading, and silica also decreased the water uptake of membranes. As expected, the ionic conductivity increased with increasing content of the SSA crosslinker, which is a donor of the hydrophilic sulfonic groups. Some of the PVA/SSA/SiO₂ membranes had a good balance between stability in aqueous environment (water uptake), thermomechanical stability and ionic conductivity and could be potential candidates for proton exchange membranes (PEM) in fuel cells.     

Isothermal Crystallization and Melting Behavior of Composites Composed of Poly(L-lactic Acid) and Poly(glycolic Acid) Fibers

Several composites of poly (L-lactic acid) (PLLA) with poly (glycolic acid) (PGA) fibers were prepared. The isothermal crystallization kinetics and melting behavior of PLLA and all of the composites were characterized by using differential scanning calorimetry. The experimental data were processed by using the Avrami equation. The relative parameters, such as the Avrami exponent and half-time crystallization, revealed that PGA fibers had positive effects on the crystallization of PLLA, but these effects had only a minimal dependence on the PGA fiber content. Moreover, at low isothermal crystallization temperatures (85°C～110°C), recrystallization during the heating scan was observed, which could lower the melting point of the samples to a certain extent.     

MgxZn1-xO粉体的制备及性能表征

MgxZn1-xO材料是一种新型的光电功能材料,近年来受到人们的广泛关注.文章采用Sol-Gel法制备了MgxZn1-xO粉体,研究Mg含量对MgxZn1-xO结构和发光性能的影响,结果表明在x从0到1的整个区间中MgxZn1-xO样品存在六方纤锌矿与面心立方两种结构,当x＜0.2时为六方纤锌矿结构,x＞0.8时为面心立方结构,在两者之间为其混合结构;光谱分析表明不同组分的MgxZn1-xO样品均具有紫外和可见发射特性,紫外发射峰位于370～384 nm,可见发射峰位于468 nm附近;粉体的平均粒径在100 nm左右.     

对氯苯甲酸-2,4,6-三吡啶基三嗪稀土配合物的合成、表征及发光性能

以对氯苯甲酸为第一配体,2,4,6-三吡啶基三嗪(TPTZ)为第二配体,分别以铕、铽和镝为中心,合成了10种稀土配合物,并进行了元素分析、稀土络合滴定、等离子光谱、紫外光谱、红外光谱和发光光谱测定。配合物的组成为:RE(p-ClBA)3(TPTZ).2H2O和RE0.5Ln0.5(p-ClBA)3(TPTZ).2H2O(RE=Eu3+,Tb3,+Dy3+;Ln=La3,+Gd3,+Y3;+p-ClBA=对氯苯甲酸根;TPTZ=2,4,6-三吡啶基三嗪),均为非电解质;对氯苯甲酸的羧基氧原子与稀土离子配位,2,4,6-三吡啶基三嗪以主配位点上的3个氮原子与稀土离子配位;铕配合物的发光强度大于铽配合物的,镝配合物发光最弱;在上述3种发光稀土配合物中分别掺入发光惰性稀土离子镧、钆及钇后,发光强度有不同改变,掺入镧可明显增强铕、铽的发光强度,钆可敏化铕、铽和镝的发光,而钇的敏化作用较弱。表明:掺杂配合物并不完全是两种简单配合物的机械混合,而是有混配配合物生成。     

Preparation and Characterization of Poly(ethylene oxide)/Graphene Nanocomposites from an Aqueous Medium

The nanocomposite films of a functionalized graphene sheet (FGS) and poly(ethylene oxide) (PEO) were cast from the physical blend of an aqueous FGS dispersion assisted by sodium dodecyl sulfate and an aqueous PEO solution. The thermal properties observed by differential scanning calorimetry suggested that FGS had a nucleating effect on the PEO crystallization. However, we found FGS actually hindered the growth of PEO crystals. The dynamic mechanical properties indicated that FGS effectively reinforced the matrix PEO. The FGS also efficiently improved the electric conductivity of PEO. With the addition of 2 parts of FGS per 100 parts of PEO, the conductivity was increased by more than 10³-fold from that of pristine PEO.     

黄腐酸平台化合物制备及特性构成光谱表征

近年来煤基高附加值化学品提取制备的前沿科学研究发现,黄腐酸平台化合物（FAPC）作为一类具有特殊功效的团簇族特性组装分子集合体,在现代农业、生物医药及功能材料等方面有良好应用前景,黄腐酸平台化合物制备提取基础理论及化学构成研究具有重要科学意义;简介了黄腐酸平台化合物基于不同源物质的制备提取方法,重点阐述了煤基物选择解离规律、黄腐酸平台化合物特征官能团构成及自组装结构特性的光谱解析,研究结果表明：酸碱反应、离子交换、生物转化及微波等途径,可以实现黄腐酸平台化合物选择性制备提取;通过红外、核磁共振、荧光光谱、电子与振动光谱及分子模拟等手段,能够从不同光谱谱图特征指认对制备所得黄腐酸平台化合物分子群组分进行分子结构、官能团、分子链、自组装空间构型、基团结构及构建方式有效检测表征;多谱图综合揭示黄腐酸平台化合物主要由羧羟基、酚羟基、醌基和羰基类分子构成;选择性解离生成的活性小分子因相关分子特性取向形成自组装集体,具备界面友好、微纳米尺寸、电学储能及良好生物相容性特点;通过对比分析对黄腐酸平台化合物制备规律进行了优缺点揭示,并对黄腐酸平台化合物未来理论研究与应用前景做了展望。     

2-芳氧甲基苯并咪唑-1-乙酰肼的NMR谱的表征

利用酯3的肼解合成出了8个2-芳氧甲基苯并咪唑-1-乙酰肼(4). 其中4c、4d、4f和4g是新化合物. 利用元素分析、IR 和¹H NMR谱对目标化合物4进行了结构表征. 利用2D NMR谱(包括¹H-¹H COSY、HSQC、HMBC 和 NOESY) 对代表化合物4e进行了¹H 和¹³C NMR的归属及空间结构确定. 通过变温实验和溶剂实验(DMSO-d₆ 和CDCl₃)研究了化合物4e的互变异构. 实验结果表明,室温下,DMSO中,目标化合物4存在着酮式和亚胺醇式这两种异构体的互变,其中酮式占 88.2%~92.6%;而在CDCl₃中,仅以亚胺醇形式存在.     

Temperature and pH-Responsive Polyacrylamide/Poly(Acrylic Acid) Interpenetrating Polymer Network Nanoparticles

The synthesis, by two sequential inverse microemulsion polymerizations, of interpenetrating polymer networks (IPN) formed by polyacrylamide (PAM) and poly(acrylic acid) (PAA) and their response to changes in pH and temperature are reported here. The temperature and pH responses of the IPN nanoparticles are compared with those of polyacrylamide and random copolymers of polyacrylamide and poly(acrylic acid) P(AM-co-AA) nanoparticles also made by inverse microemulsion polymerization. We found that only the IPN nanogels exhibited a sharp swelling increase with temperature associated with its Upper Consolute Solution Temperature, driven by hydrogen bonding interactions, and with pH, driven by electrostatic repulsions of the PAA carboxylic groups, especially at pHs larger than the pK_a of the PAA. The ?-potentials of the PAM, P(AM-co-AA) and IPN nanogels were measured as a function of pH and temperature, to determine the effects of these two variables, which in turn, affected the swelling of the nanogels. Field emission scanning electron microscopy revealed that the IPN nanogels were spheroidal with sizes similar to those determined by dynamic light scattering.