The non-oxidative thermal degradation of poly (Di-2-chloroethyl itaconate)

The non-oxidative thermal degradation of poly (di-2-chloroethyl itaconate) (PD2CEI) was studied by TG and by analysing the thermal products. The major processes occurring during thermal analysis are crosslinking, depolymerisation and carbonisation. The thermal degradation activation energy increased with increasing sample mass loss. The thermal degradation of PD2CEI was compared to that of the structurally similar poly(2-chloroethyl methacrylate) (P2CMA).     

光催化降解染料ZnO催化剂的性能

光催化法是20世纪70年代发展起来的新型水处理技术，即以某些半导体材料为催化剂，利用光催化法来降解环境污染物。该方法工艺简单，成本较低，在常温下能使大多数不能或难于生物降解的有毒有机物彻底氧化分解。近年来研究最多的是TiO2，由于其带隙较宽(3．2eV)，只能吸收波长λ≤387nm的紫外光，因此研制新型光催化剂仍是重要课题。     

Determination of Lercanidipine Hydrochloride and Its Impurities in Tablets

The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for determination of lercanidipine hydrochloride and its synthetic impurities, degradation and oxidative products in Carmen^® tablets. The best separation was performed on Zorbax SB C18 column, 250 x 4.6 mm, particle size 5 m. Acetonitrile-water-triethylamine 55:44.8:0.2 (v/v/v) was used as a mobile phase with flow rate 1 mL min^–1. pH was adjusted to 3.0 with orthophosphoric acid. UV detection was performed at 240 nm. Duration of chromatographic run was about 12 min for six examined compounds. The chromatographic conditions for the determination of lercanidipine hydrochloride and its related substances were the same, but the concentration of lercanidipine hydrochloride was 0.03 mg mL^–1 for assay and 0.3 mg mL^–1 for related substances. The validation of the method performance characteristics (figures of merits, quality of parameters) was established to be adequate for the intended use. The evaluation of number of parameters, such as selectivity, linearity, accuracy, specificity, precision (repetability and reproducibility), sensitivity and detection and determination limits is entailed.Acknowledgements This work was supported by the Institute of Pharmacy of Serbia, Belgrade and by the Ministry for Science, Technology and Development of Serbia, Contact: 1458     

Recyclability of a layered silicate-thermoplastic olefin elastomer nanocomposite

A multiple-pass study was undertaken with a layered silicate-thermoplastic olefin elastomer (TPO) nanocomposite to study the impact of processing history on the properties of the material. A set of 10 passes were completed through a co-rotating intermeshing twin-screw extruder with samples collected to monitor changes in the composite. The microstructure of the nanocomposite was characterized using TEM, XRD, FT-IR, steady and complex shear rheology, and mechanical testing. With progressive passes through the extruder, the TPO nanocomposite experienced both delamination of the organoclay as well as thermo-oxidative degradation. The onset and extent of degradation were found to be unaffected by the presence of the organoclay species in the polymer, though, inclusion of a maleated compatibilizer led to increased chain scission. The generated carbonyl groups along the polymer chain as a result of oxidation were speculated to have a significant effect on the developing percolating network of clay within the material and on the final rheological properties of the composite. Despite the occurrence of degradation in the nanocomposite during recycling, its rheological and mechanical properties remained significantly higher than those of the unfilled resin.     

A model for thermal degradation of hybrid nanocomposites

A model is developed for thermal degradation of polymer nanocomposites. A composite is thought of as an equivalent network of linear chains with attached side-groups. Thermal degradation is treated as combination of (i) binary scission (fragmentation) of backbone chains, and (ii) detachment of side-groups and their subsequent annihilation (diffusion to the surface of a sample and desorption). An explicit solution is derived for the kinetic equation. This solution involves three adjustable parameters that are found by fitting observations on isotactic polypropylene reinforced with carbon nanofibres. Good agreement is demonstrated between the experimental data and the results of numerical simulation.     

Influence of the thermal degradation on the dielectric properties of a thermoset

The thermal degradation of an epoxy system consisting of a diglycidyl ether of bisphenol A (DGEBA, n=0) and m-xylylenediamine (m-XDA) was studied by both thermogravimetric analysis (TG) and dielectric analysis (DEA). It has been checked a deviation of the typical behaviour in the Arrhenius plot expected for this kind of systems, owing to the thermal degradation. Both, structural relaxation time and conductivity values, were represented as a function of the mass loss, that allow a relationship to be obtained between characteristic relaxation time and the degree of degradation at the beginning of the degradation process.     

Colour formation in poly(ethylene terephthalate) during melt processing

The discolouration, that occurs in virgin poly(ethylene terephthalate) - PET during melt processing, was studied using various bulk and surface analytical techniques. Proton nuclear magnetic resonance (¹H NMR) was used to study the bulk chemical changes occurring in the polymer during thermo-oxidative degradation. Chemical derivatisation with trifluoroacetic anhydride (TFAA) was used to label the hydroxyl groups introduced on the polymer surface by thermal oxidation.From the surface analysis studies using photoacoustic Fourier transform infrared spectroscopy (PA/FT-IR), diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) and X-ray photoelectron spectroscopy (XPS) it was evident that colour formation starts initially with the hydroxylation of the terephthalic ring. Further, the formation of additional carbonyl functionalities and conjugated chromophoric systems complete the colour formation process.     

Atom transfer radical polymerization of 1-phenoxycarbonyl ethyl methacrylate monomer

Atom transfer radical polymerization conditions with copper(I) bromide/2,2^′-bipyridine (Cu/2,2^′-bpy) as the catalyst system were employed for the homopolymerization and random copolymerization of 1-phenoxycarbonyl ethyl methacrylate (PCMA) with methyl methacrylate (MMA). Temperature studies indicated that the polymerizations occurred smoothly in bulk at 110 °C. Poly(PCMA)(polydispersity index=1.27) homopolymer was characterized and then used as macroinitiator for increasing its molecular weight. The homopolymerization of PCMA was also carried out under free radical conditions using 2,2^′-azobisisobutyronitrile as an initiator.The monomer and polymers were characterized by FT-IR and ¹H and ¹³C-NMR techniques. The glass transition temperatures, the solubility parameters and average-molecular weights of the polymers were determined. Thermal stabilities of the polymers were given as compared with each other by using TGA curves. Thermal degradation products of poly(PCMA)s obtained by ATRP and free radical polymerization were compared with each other by using ¹H-NMR technique.     

Wavelength effect on the photoinduced reaction of polymethylmethacrylate

Polymethylmethacrylate (PMMA) containing benzophenone (BP) was photo-irradiated with monochromatic radiation of wavelength 260–360 nm using the Okazaki Large Spec-trograph (OLS). On irradiation of PMMA films containing BP in air, the sensitized main-chain scission and photocrosslinking of PMMA took place simultaneously. These reactions are dependent on irradiation wavelength. The threshold wavelength for both reactions is found to be ca. 380 nm. The number of main-chain scission and amount of gel increased with the increase of BP concentration in PMMA. Photosensitized main-chain scission favors the irradiation of radiation at ca. 280 nm and photocrosslinking takes place efficiently with the exposure of 340 nm radiation. A possible mechanism for photosensitized reaction is proposed. © 1995 John Wiley & Sons, Inc.     

水热法制备纳米ZnS的光催化性能研究

采用水热法制备了结晶良好的ZnS纳米粒子,通过XRD、FT-IR、TEM、UV-Vis DRS等手段对所合成的ZnS粉体的结构、粒度和理化性能进行表征,并以亚甲基蓝为目标降解物,评价了ZnS粉体在紫外光和可见光下的光催化性能。研究结果表明,水热法制备的纳米ZnS为典型的六方晶系,粒径大致为10～20 nm,不论是在紫外光或可见光下对亚甲基蓝均具有优异的脱色率,呈现出良好的光催化性能。