Crystal structure of mixed sodium-potassium paradodecatungstate 6-hydrate

The crystal structure of K7Na3[H2W12O42]3 . 6H(2)O was determined by X-ray crystallography,and refined to R=0.0864 based on 7024 observed reflections (I>2 sigma(I)). The crystallographic parameters are a=11.755(2), b=13.0493(3), c=16.289(3) Angstrom; alpha=77.13(3)degrees, beta=82.92(3)degrees, gamma=89.65(3)degrees, triclinic, space group, P (1) over bar, V=2416.7(8) Angstrom(3), Z=2, M-r=3330.98, D-cal=4.578Mg/m(3), F(000)=2904; mu (MoK alpha)=29.170mm(-1), T=293K. Two independent polyanions are centered respectively at 1,1,1/2 and 1/2, 1/2, 0, approximately perpendicular to each other with dihedral angle between the equatorial planes of the molecules at 96 degrees. K+ and Na+ respectively occupy the clefts of the two discrete polyanions.

Phase identification in a series of liquid crystalline TPP polyethers and copolyethers having highly ordered mesophase structures. 6. Structure changes from smectic to columnar phases in a series of copolyethers containing odd and even numbers of methylene units in equal molar composition

A series of liquid crystalline copolyethers has been synthesized from 1-(4-hydroxy-4'-biphenyl)-2-(4-hydroxyphenyl)propane and different alpha,omega-dibromoalkanes [coTPP(n/m)]. In this report, coTPPs having n = 5, 7, 9, 11 and m = 12 are studied, which represent copolyethers having both varying odd number and a fixed even number of methylene units. The compositions were fixed at an equal molar ratio (50/50). These coTPPs(nlm) show multiple phase transitions during cooling and heating in differential scanning calorimetry experiments. The undercooling dependence of these transitions is found to be small, indicating that these transitions are close to equilibrium, Although the coTPPs possess a high-temperature nematic (N) phase, the periodicity order along the chain direction is increasingly disturbed when the length of the odd-numbered methylene units decreases from n 11 to 5. in the coTPPs(5/12, 7/12, and 9/12), wide-angle X-ray diffraction experiments at different temperatures show that, shortly after the N phase formation during cooling, the lateral molecular packing improves toward a hexagonal lattice, as evidenced by a gradual narrowing of the scattering halo. This process represents the possible existence of an exotic N phase, which serves as a precursor to the columnar (Phi(H)) phase. A further decrease in temperature leads to a (PH phase having a long-range ordered, two-dimensional hexagonal lattice. In coTPP(11/12), the phase structures are categorized as highly ordered and tilted, smectic and smectic crystal phases, similar to homoTPPs, such as the smectic F (S-F) and smectic crystal G (SCG) phases. An interesting observation is found for coTPP(9/12), wherein a structural change from the high-temperature Phi(H) phase to the low-temperature S-F phase occurs. It can be proven that, upon heating, the well-defined layer structure disappears and the lateral packing remains hexagonal. The overall structural differences in this series of coTPPs between those of the columnar and highly ordered smectic phases are related to the disorders introduced into the layer structure by the dissimilarity of the methylene unit lengths in the comonomers.

Studies on the interfacial adhesion between functionalized polypropylene and polyamide 1010

The interface behavior of polyamide 1010 (PA1010) and polypropylene (PP) was studied. In order to improve their interfacial adhesion, functional PP was prepared by means of grafting glycidyl methacrylate (GMA) on PP main chains and used instead of plain PP. Several technological characterizations were performed here on their interfaces. ESCA was used to confirm that some kind of reaction occurred between end groups of PA1010 and epoxy species of PP-g-GMA. The peel test was adopted to measure interfacial adhesion. It was found that the fracture energy of interfaces between PA1010 and PP-g-GMA was dramatically increased with the content of GMA. Their interfaces were observed as being blurred by using SEM and TEM and a crack that could be seen in the case of the interfaces of the PA1010 and the plain PP disappeared.

Polyimides from 3,3 '-dioxo-[1,1 ']-spirodiphthalan-5,5 ',6,6 '-tetracarboxylic dianhydride

A novel dianhydride, 3,3'-dioxo-[1,1']-spirodiphthalan-5,5',6,6'-tetracarboxlic dianhydride, was synthesized and used as a monomer to prepare polyimides with several diamines via a conventional two-stage procedure. The intermediate poly(amic-acid)s had inherent viscosities of 0.84-1.71 dL/g and could be thermally converted into lightly yellow, transparent, flexible and tough films. Films cast from chemically imidized polyimides were transparent and colorless. The glass transition temperatures (Tg) were > 400 degrees C, and the 5% weight-loss temperatures were > 420 degrees C in N-2 and in air. The solubilities of these polyimides in various solvents were evaluated. The mechanical properties of some polyimides were also tested. (C) 1999 Elsevier Science Ltd. All rights reserved.

Preparation of the HIPS/MA graft copolymer and its compatibilization in HIPS/PA1010 blends

The graft copolymer of high-impact polystyrene (HIPS) grafted with maleic anhydride (MA) (HIPS-g-MA) was prepared with melt mixing in the presence of a free-radical initiator. The grafting reaction was confirmed by infrared analyses, and the amount of MA grafted on HIPS was evaluated by a titration method. 1-5% of MA can be grafted on HIPS. HIPS-g-MA is miscible with HIPS. Its anhydride group can react with polyamide 1010 (PA1010) during melt mixing of the two components. The compatibility of HIPS-g-MA. in the HIPS/PA1010 blends was evident. Evidence of reactions in the blends was confirmed in the morphology and mechanical behavior of the blends. A significant reduction in domain size was observed because of the compatibilization of HIPS-g-MA in the blends of HIPS and PA1010. The tensile mechanical properties of the prepared blends were investigated, and the fracture surfaces of the blends were examined by means of the scanning electron microscope. The improved adhesion in a 15% HIPS/75% PA1010 blend with 10% HIPS-g-MA copolymer was detected. The morphology of fibrillar ligaments formed by PA1010 connecting HIPS particles was observed. (C) 1999 John Wiley & Sons, Inc.

Synthesis, properties and crystal structure of charge-transfer salt (DBTTF)(6)HSiMo12O40H2O

Charge-transfer salt (DBTTF)(6)HSiMo(12)O(40)4H(2)O was synthesized by electrocrystallization and characterized by IR spectrum and electronic spectrum. Its magnetic property, conductivity and crystal structure were determined. The title compound consists of heteropoly anions, water molecules and DBTTF columns which are formed by repeated arrangement of tetramer (DBTTF), in the direction of 15 degrees to the a axis in the tunnel constituted by the anions and other type of DBTTF. The title compound is paramagnetic and semiconducting. (C) 1998 Elsevier Science Ltd. All rights reserved.

Effect and mechanism in compatibilization of poly(styrene-b-2-ethyl-2-oxazoline) diblock copolymer in poly(2,6-dimethyl-1,4-phenylene oxide) poly(ethylene-ran-acrylic acid) blends

The compatibilization effect of poly(styrene-b-2-ethyl-2-oxazoline) diblock copolymer, P(S-b-EOx), on immiscible blends of poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) and poly(ethylene-co-acrylic acid) (EAA) is examined in terms of phase structure and thermal, rheological and mechanical properties, and its compatibilizing mechanism is investigated by Fourier-transform infrared spectroscopy. The block copolymer, synthesized by a mechanism transformation copolymerization, is used in solution blending of PPO/EAA. Scanning electron micrographs show that the blends exhibit a more regular and finer dispersion on addition of a small amount of P(S-b-EOx). Thermal analysis indicates that the grass transition of PPO and the lower endothermic peal; of EAA components become closer on adding P(S-b-EOx), and the added diblock copolymer is mainly located at the interface between the PPO and EAA phases. The interfacial tension estimated by theological measurement is significantly reduced on addition of a small amount of P(S-b-EOx). The tensile strength and elongation at break increase with the addition of the diblock copolymer for PPO-rich blends, whereas the tensile strength increases but the elongation at break decreases for EAA-rich blends. This effect is interpreted in terms of interfacial activity and the reinforcing effect of the diblock copolymer, and it is concluded that the diblock copolymer plays a role as an effective compatibilizer for PPO/EAA blends. The specific interaction between EAA and polar parts of P(S-b-EOx) is mainly hydrogen bonding. (C) 1998 Elsevier Science Ltd. All rights reserved.

基质辅助激光解吸电离-飞行时间质谱表征6氟双酚A芳香环状聚醚酮(砜)

应用基质辅助激光解吸电离飞行时间质谱,在不同阳离子剂的存在下,对6氟双酚A聚芳醚酮(砜)环状低聚物的结构进行了确认,研究了环状化合物对金属离子的选择性及激光质谱表征含氟环状低聚物的适宜条件.

尼龙1010/6及尼龙1010/66基本物理性能与组成的关系

尼龙1010/6 和尼龙1010/66 的基本物理性能随着组成的改变而改变,尼龙1010 含量高时,共聚物密度大于计算值;含量低时,共聚物密度小于计算值.尼龙1010 含量20%左右时,共聚物具有较大吸水率

Phase transition temperature of HPT(2,3,6,7,10,11-hexa-n-pentyloxytriphenylene) from molecule dynamic simulation

Molecule dynamics simulation was used on HPT(2,3,6,7,10,11-hexa-n-pentyloxytriphenylene), which is a discotic Liquid crystal. From analyzing the energy and displacement varying with the temperature, the phase transition temperature of PM6MPP can be predicted. The deviations of T-g, T-m and T-i due to the MD time scale are small enough that it should be possibly used to predict the material properties especially when more powerful computers are available.

Compatibilizing effect of polystyrene-block-poly(4-vinylpyridine) for poly(2,6-dimethyl-1,4-phenyleneoxide) chlorinated polyethylene blends

The compatibilizing effect and mechanism of compatibilization of the diblock copolymer polystyrene-block-poly(4-vinylpyridine) P(S-b-4VPy) on immiscible blends of poly(2,6-dimethyl-1,4-phenylene oxide) (PPO)/chlorinated polyethylene (CPE) were studied by means of scanning electron microscopy (SEM), differential scanning calorimetry (DSC), mechanical properties and FTIR measurements. The block copolymer was synthesized by sequential anionic polymerization and melt-blended with PPO and CPE. The results show that the P(S-b-4VPy) added acts as an effective compatibilizer, located at the interface between the PPO and the CPE phase, reducing the interfacial tension, and improving the interfacial adhesion. The tensile strength and modulus of all blends increase with P(S-b-4VPy) content, whereas the elongation at break increases for PPO-rich blends, but decreases for CPE-rich blends. The polystyrene block of the diblock copolymer is compatible with PPO, and the poly(4-vinylpyridine) block and CPE are partially miscible.

The characterization of the interfacial reaction in polyamide 1010 poly(propylene)-graft-(glycidylmethacrylate) blends

Binary blends of polyamide 1010/poly(propylene) and polyamide 1010 (PA1010)/poly(propylene)-graft-(glycidyl methacrylate) (PP-g-GMA) were prepared. The epoxy groups in PP-g-GMA react with the amino end-groups in PA1010, thus a PA1010-graft-PP copolymer is formed and acts as a compatibilizer between PA1010 and PP-g-GMA. The reaction was confirmed by electron spectroscopy for chemical analysis (ESCA) and attenuated total reflection (ATR)-FTIR spectroscopic analysis, and also evaluated by the stability of the suspension obtained by dissolving the blends in formic acid and by the morphologies of the blends.

Structure and Conformation of 2,3,6, 7,10,11-hexakispentyloxytriphenylene by TEM and Computer Simulation

Experimental electron diffraction patterns and high resolution images were used to determine the space group and unit cell dimensions of 2,3,6,7,10,11-hexakispentyloxytriphenylene. Subsequently the molecular conformation was calculated by energy minimized package in Cerius2. Using this method, we got the HPT crystal structure: space group: P6/mmm; lattice type: hexogonal; the lattice parameters are a = b = 20.3 angstrom, c = 3.52 angstrom, = = 90 degrees, = 120 degrees. The core of HPT is not perpendicular to the column. The angle between a axis and HPT core plane is 9 degrees which cannot be seen in b-c projection. The simulated ED patterns and HREM images are good agreement with the experimental ED patterns and HREM images.

In-situ microscopic FTIR spectroelectrochemical study of the reduction of K3Fe(CN)(6) in polymer electrolyte

Cyclic voltammetry and in-situ microscopic FTIR spectroelectrochemistry were used for the electrochemical and vibrational characterizations of the reduction process of K3Fe (CN)(6) in polyethylene glycol(PEG) with LiClO4 as supporting electrolyte at a Pt microelectrode. The rate of electron transfer is a function of the concentration of the supporting electrolyte. The redox potentials and cyclic voltammetric currents vary with Li/O molar ratio. The bl-situ spectroelectrochemistry shows that the infrared spectra are influenced by the concentration of LiClO4. The bridging cyanide groups with a structure Fe-I-C drop N ... Fe-I-C drop N are formed during the reduction process of K3Fe (CN)(6). There may be an activated complex between the Lif cation and the complex anion.