Two‐phase production of cyclohexene and cyclooctene oxides in water as an approach to pollution prevention

Liquid–liquid two‐phase epoxidation from cyclohexene and cyclooctene in aqueous potassium peroxymonosulfate (commercially available as Oxone^®) solution was studied as an application in pollution prevention. To avoid potential emissions of volatile organic compounds an aqueous solution was employed to replace the usual chlorinated solvents used in epoxide production. A droplet column reactor and stirred tank reactor were used to investigate two‐phase synthesis of epoxide. An aqueous Oxone^® solution was used to oxidize a dispersion of alkene droplets and form epoxide. The study of aqueous epoxidation in both reactors showed that the epoxidation of alkenes can be represented as a first order reaction with respect to alkene. The salting out effect of Oxone^® concentration was studied in both reactors and found to be very similar at optimal conditions. In comparing the two reactors, it was found that the droplet column reactor produces larger quantities of product per unit reactor volume for the same reaction time. The objective of this study is to provide an alternative reactor design and synthesis route that can meet pollution prevention goals. Copyright © 2004 Society of Chemical Industry     

Study of the morphology and mechanical properties of polypropylene composites with silica or rice‐husk

The mechanical, morphological behavior and water absorption characteristics of polypropylene (PP) and silica, or PP and rice‐husk, composites have been studied. The silica used in this study as filler was a commercial type produced from soluble glass or rice husks. The compatibilizing effect of PP grafted with monomethyl itaconate (PP‐g‐MMI) and/or with vinyltriethoxysilane (PP‐g‐VTES) as polar monomers on the mechanical properties and water absorption was also investigated. In general, a high loading of the studied fillers in the polymer matrix increases the stiffness and the water absorption capacity. This effect is more noticeable in the tensile modulus of the PP/silica composite with PP‐g‐VTES as compatibilizer. However, the increase of the rice‐husk charge as a natural filler in the PP matrix decreases the stiffness, and in the presence of PP‐g‐MMI as compatibilizer in PP/rice‐husk, the tensile modulus and water absorption of the composite were improved. The better adhesion and phase continuity in the PP/silica and PP/rice‐husk composites with different compatibilizers was confirmed by the morphological study. Copyright © 2004 Society of Chemical Industry     

Schwingfestigkeit von Schraube‐Mutter‐Verbindungen

High cycle fatigue of bolted connections Extensive tests regarding the influences on the fatigue of bolt‐nut‐connections of preloading with torsion, of preloading with yielding, of loading with superimposed bending and of the tested lot are processed. These influences are not yet known according to VDI 2230. New testing devices were designed for these tests, which allow a far less expensive operation and may easily be used for bolts of diameters up to M100 and testing frequencies up to 1000 Hz. The validity of fatigue resistance according to VDI 2230 is specified with respect to the test results. The determined influence of the tested lots is unexpectedly high. The manufacturing process of bolts should be improved to minimize this influence.     

Synthesis,characterization and properties of functionalized styrene–maleimide copolymers

New functionalized styrene–maleimide copolymers were prepared by free radical copolymerization of styrene (St) and N‐4‐carboxybutylmaleimide (NBMI) in chloroform, using 2,2′‐azobisisobutyronitrile (AIBN) as initiator. Monomer and copolymer characterization was carried out by ¹H‐ and ¹³C‐NMR. Copolymer composition was determined by elemental analysis and Fourier‐transform infrared (FTIR) spectroscopy. The glass transition temperature (from DSC) and the thermogravimetric analysis (TGA) of the copolymers were consistent with the thermal behavior and stability observed for alternating St–maleimide copolymers. St–NBMI copolymers crosslinked with divinylbenzene (DVB) were also synthesized and their cation exchange properties evaluated in order to assess the capacity of the new copolymers to bind metallic ions. Copyright © 2005 Society of Chemical Industry     

2,4,6‐Trichlorophenol and phenol removal in methanogenic and partially‐aerated methanogenic conditions in a fluidized bed bioreactor

A fluidized bed bioreactor (FBBR) was operated for more than 575 days to remove 2,4,6‐trichlorophenol (TCP) and phenol (Phe) from a synthetic toxic wastewater containing 80 mg L^?1 of TCP and 20 mg L^?1 of Phe under two regimes: Methanogenic (M) and Partially‐Aerated Methanogenic (PAM). The mesophilic, laboratory‐scale FBBR consisted of a glass column (3 L capacity) loaded with 1 L of 1 mm diameter granular activated carbon colonized by an anaerobic consortium. Sucrose (1 g COD L^?1) was used as co‐substrate in the two conditions. The hydraulic residence time was kept constant at 1 day. Both conditions showed similar TCP and Phe removal (99.9 + %); nevertheless, in the Methanogenic regime, the accumulation of 4‐chlorophenol (4CP) up to 16 mg L^?1 and phenol up to 4 mg L^?1 was observed, whereas in PAM conditions 4CP and other intermediates were not detected. The specific methanogenic activity of biomass decreased from 1.01 ± 0.14 in M conditions to 0.19 ± 0.06 mmolCH₄ h^?1 gTKN^?1 in PAM conditions whereas the specific oxygen uptake rate increased from 0.039 ± 0.008 in M conditions to 0.054 ± 0.012 mmolO₂ h^?1 gTKN^?1, which suggested the co‐existence of both methanogenic archaea and aerobic bacteria in the undefined consortium. The advantage of the PAM condition over the M regime is that it provides for the thorough removal of less‐substituted chlorophenols produced by the reductive dehalogenation of TCP rather than the removal of the parent compound itself. Copyright © 2005 Society of Chemical Industry     

Preparation of glucose oxidase immobilized in different carriers using radiation polymerization

Glucose oxidase (EC 1.1.3.4) was immobilized on different polymeric materials using different immobilization techniques (entrapping by γ‐irradiation, and covalent binding using epichlorohydrin). Studies were carried out to increase the thermal stability of glucose oxidase (GOD) for different applications. The activity and stability of the resulting biopolymers have been compared with those of free GOD. The effect of different polyvinyl alcohol/polyacrylamide (PVA/PAAm) compositions of the copolymer carrier on the enzymatic activity of the immobilized GOD was studied. The maximum enzymatic activity was obtained with the composition ratio of PVA/PAAm of 60:40. The behaviour of the free and immobilized enzyme was analysed as a function of pH. A broadening in the pH profile (5.5–8) was observed for immobilized preparations. The activity and stability of the resulting biopolymers produced by immobilization of GOD onto different carriers have been compared, in both aqueous and organic media, with those of the free GOD. The enzyme's tolerance toward both heat and organic solvent was enhanced by immobilization onto polymers. The addition of different concentrations of organic solvents (10–50%, v/v) to the enzyme at higher temperature (60 °C) was found to stabilize the enzyme molecule. The strongest stabilizing effect on the enzymatic activity was achieved at a concentration of 10%. Copyright © 2005 Society of Chemical Industry     

Ozonation of CI Reactive Black 5 using rotating packed bed and stirred tank reactor

This study investigates the ozonation of CI Reactive Black 5 (RB5) by using the rotating packed bed (RPB) and completely stirred tank reactor (CSTR) as ozone contactors. The RPB, which provides high gravitational force by adjusting the rotational speed, was employed as a novel ozone contactor. The same ozone dosage was separately introduced into either the RPB or the CSTR for the investigation, while the experimental solution was continuously circulated within the apparatus consisting of the RPB and CSTR. The decolorization and mineralization efficiencies of RB5 in the course of ozonation are compared for these two methods. Moreover, the dissolved and off‐gas ozone concentrations were simultaneously monitored for the further analysis. As a result, the ozone mass transfer rate per unit volume of the RPB was significantly higher because of its higher mass transfer coefficient and gas–liquid concentration driving force. Furthermore, ozonation kinetics was found to be independent of the gravitational magnitude of an ozone gas–liquid contactor. Therefore, the results suggest employing RPBs as ozone‐contacting devices with the advantage of volume reduction. The experimental results, which can be used for further modeling of the ozonation process in the RPB, also show the requirement of correct design for the RPB. Consequently, the present study is useful for the understanding of practical application of RPBs. Copyright © 2004 Society of Chemical Industry     

The importance of electrochemistry-related etching in thegate-groove fabrication for InAlAs/InGaAs HFETs

For the first time, the surface metal on nonalloyed ohmic electrodes is found to significantly change the profiles of gate grooves, when resist openings are employed to monitor drain current during wet-chemical gate recess for sub-micron InAlAs/lnGaAs heterojunction field-effect transistors (HFETs). The surface metal of Ni enhances the etching rate in comparison with that in the absence of electrodes by a factor of 4 and 10, laterally and vertically, which is favorable to fabricate deep gate grooves with small side etching. The Pt surface metal, however, leads to preferential etching of InGaAs over InAlAs, which can be useful to realize large side etching. The existence of an electrochemistry-related etching component, which arises when the ohmic electrodes are present during recess etching, is considered to be responsible for these behaviors     

Modified atmosphere packaging of a mixed prepared vegetable salad dish

The aim of this study was to design a modified atmosphere package for a mixed vegetable salad consisting of 75 g of cut carrot, 55 g of cut cucumber, 20 g of sliced garlic and 50 g of whole green pepper. Respiration data of all the components were combined with film permeability data to predict package atmospheres and design optimal packages for experimental testing for improved shelf-life of the produce. The optimal package avoided minimum O₂ and maximum CO₂ tolerance limits, and chilling injury temperatures for any component. A pouch form package made of 27 mm low density polyethylene developed a modified atmosphere of 2.0–2.1% O₂ and 5.5–5.7% CO₂, which was beneficial for all components and provided better quality retention than other test packages.