Synthesis and characterization of novel diimide–dinaphthols and resulting poly(urethane–imide)s

Novel diols containing imide groups were prepared via condensation of aromatic dianhydrides with 5‐amino‐1‐naphthol. The diimide–dinaphthols prepared were characterized by conventional methods and used to synthesize new poly(urethane–imide)s (PUIs). All the polymers were characterized and their physical properties, such as solubility, solution viscosity, thermal stability, and thermal behaviour were studied. The polymers obtained showed more thermal stability than typical polyurethanes because of the presence of the imide groups. Copyright © 2003 Society of Chemical Industry     

Homogenization of hardness distribution and distortion in high pressure gas quenching

Quenching with gases rather than oil or other liquid media has the advantages of reducing the risks concerning health and environment, while simultaneously homogenizing the quenching results and minimizing distortion due to a wide range of possible process parameter variations and the pure convective heat transfer. In this contribution, a coupled solution for increasing homogenization of quenching results within high pressure gas quenching will be presented. In the first stage, an experimental test facility was set up for flow investigations and in the second stage a numerical simulation model was generated. The numerical and experimental results of the flow through the chamber were compared for several boundary conditions. Finally, after complete verification of the simulation, the model may be used to assist in parameter variation for optimization of homogeneous high pressure gas quenching.     

A Practical Method to Derive Sample Temperature during Nonisothermal Coupled Thermogravimetry Analysis and Differential Scanning Calorimetry Experiments

Nonisothermal thermogravimetry differential scanning calorimetry (TG‐DSC) mounting is intensively used for the determination of kinetic parameters and reaction heat along the chemical transformation of a solid. Nevertheless, when tests are performed with heating rates as high as those encountered in industrial processes, e.g., several tens of K min^–1, there is great uncertainty in the knowledge of the exact sample temperature. In this work, a method to derive a simple mathematical expression is proposed and fully described in order to calculate the real sample temperature throughout a temperature‐ramped test on a commercial apparatus. The furnace temperature and the heat flow signals were used, together with the crucible specific heat and the heating rate. A number of validation tests were performed to derive similar reaction rates for a reference. First‐order kinetic reactions were presented and reconciled over a large range of heating rates from 3 to 50 K min^–1.     

Effect of polymerization conditions on o‐phenylenediamine and o‐phenetidine oxidative copolymers

A series of new o‐phenylenediamine (OPD)/o‐phenetidine (PHT) copolymers with partly phenazine‐like structures has been successfully synthesized at three polymerization temperatures by chemically oxidative polymerization in four different polymerization media. The molecular structures and properties of the resulting OPD/PHT polymers were investigated by IR, UV–vis and high‐resolution ¹H NMR spectroscopies, and DSC, in order to ascertain the effect of reaction temperature, comonomer ratio and acid medium. The copolymerization mechanism of OPD with PHT monomers has been proposed. It is found that the statistical OPD/PHT copolymer obtained at a temperature of 118 °C has a higher degree of polymerization than that obtained at 12–17 °C. The OPD content in the copolymers calculated from NMR spectroscopic analysis is higher than that in the feed OPD content, whereas the OPD content calculated from element analysis is slightly lower than the feed OPD content. It can be predicted that denitrogenation takes place in the OPD units during the polymerization process at OPD/PHT molar ratios of 90/10 and 100/0. These OPD/PHT copolymers exhibit a much better solubility than the OPD homopolymer, hence suggesting an incorporation of PHT units into the phenazine structure of the homopolymer. The thermal behavior of the copolymers was also studied. Copyright © 2004 Society of Chemical Industry     

Oil Spill Cleanup from Sea Water by Sorbent Materials

Three sorbents were compared in order to determine their potential for oil spill cleanup. Polypropylene nonwoven web, rice hull, and bagasse with two different particle sizes were evaluated in terms of oil sorption capacities and oil recovery efficiencies. Polypropylene can sorb almost 7 to 9 times its weight from different oils. Bagasse, 18 to 45 mesh size, follows polypropylene as the second sorbent in oil spill cleanup. Bagasse, 14 to 18 mesh size, and rice hull have comparable oil sorption capacities, which are lower than those of the two former sorbents. It was found that oil viscosity plays an important role in oil sorption by sorbents. All adsorbents used in this work could remove the oil from the surface of the water preferentially.     

Magnetic Resonance Visualisation of Flow and Pore Structure in Packed Beds with Low Aspect Ratio

Different NMR techniques were combined to obtain the structure and velocity information for a systematic investigation of fixed beds with low aspect ratio (tube diameter to particle diamter, d_t/d_p) in the range 1.4 to 32. The structure of the void space was determined for a variety of packed beds of glass beads or regular and irregular porous pellets by magnetic resonance imaging (MRI). Based on the images the radial distribution of the voids within the bed was obtained. Ordering effects were found even for non‐spherical and polydisperse particles, and a maximum of the fluid density near the tube wall was confirmed for all pellet geometries and sizes. By combining MRI with velocity encoding, velocity profiles and distributions of flow velocity components of a single fluid phase through packed beds have been acquired. The radial velocity distribution follows an oscillatory pattern which largely reflects the ordering of the particles, which can be accessed from the density distribution of the interparticle fluid. Maximum velocities of up to four times the average value were found to occur near the tube wall. This wall effect was observed for all but the smallest particles, where the aspect ratio was d_t/d_p = 32. Moreover, a visualisation of flow pattern in the presence of packed particles was achieved by using a tagging technique, and the stationary flow field could be identified for an experimental time of several hours.     

Morphology development in polyethylene/polystyrene blends: the influence of processing conditions and interfacial modification

The influence of processing conditions and interfacial modification on the morphology evolution and the composition range within which fully co‐continuous high density polyethylene/polystyrene blend structures can exist during blending in a single screw extruder was studied. Blends ranging from pure A to pure B component, with and without compatibilizer, were prepared under two different shear rates. It was found that high shear rates displaced the breakdown–coalescence balance of the dispersed nodules to the side of coalescence, narrowing the percolation domain and the critical composition for full co‐continuity decreased with increasing shear rates. The addition of a tri‐block compatibilizer induced the percolation threshold of the polystyrene phase to begin at lower percentages of polyethylene but the phase inversion point did not change. The experimental results are discussed in the light of various theoretical models. Copyright © 2005 Society of Chemical Industry     

Influence of the silicon surface treatment by plasma etching and scratching on the nucleation of diamond grown in HFCVD - a comparative study

A comparative study for the nucleation of diamond was carried out using surface treatment like (i) surface scratching with 1 μm diamond paste and (ii) surface etching using chlorine plasma at different RF powers (50, 100 and 150 W). Atomic force microscopic study shows variation in roughness from 31 nm to 110 nm. Scratching results in random scratches, whereas plasma etches a surface uniformly. Scanning electron microscopic observations show well faceted crystallites with a predominance of angular shaped grains corresponding to 〈100〉 and 〈110〉 crystallite surfaces for the scratched as well as plasma etched substrate. Surface etching at 150 W plasma power results in a better growth in comparison with 50 and 100 W plasma powers. Chlorine-radical is found responsible for the changes in the growth morphology. Raman spectroscopy shows a sharp peak at 1,332 cm⁻¹ and a peak at ∼1,580 cm⁻¹ for both samples.