Effect of Adding Transition Metals to Copper on the Dehydrogenation Reaction of Ethanol

The present work aims to investigate the effect adding Ag, Co, Ni, Cd and Pt to copper on ethanol dehydrogenation. The catalysts synthesized by deposition–precipitation method were characterized using various physicochemical methods such as N₂ adsorption–desorption, TPR, SEM–EDX, XRD, XPS and TGA–DSC-MS. Catalytic evaluation results revealed that the predominant product of the reaction was acetaldehyde. Monometallic copper or mixed with Cd, Ag or Co show good catalytic performances. Adding nickel to copper improves the process conversion but reduces acetaldehyde selectivity, giving rise to methane in produced hydrogen. Pt-Cu/SiO₂ catalyst guides the reaction towards diethyl ether. Time on stream tests performed during 12 h at 260 °C, showed that adding Cd to Cu enhances its stability by over 30% of conversion, this is explained by the reduction of copper crystallites sintering, which makes Cd-Cu/SiO₂ a promising catalyst for the production of acetaldehyde by ethanol dehydrogenation.

Graphic Abstract

     

A modified design approach for compact ultra‐wideband microstrip filters

A modified design approach for compact ultra‐wideband microstrip filters with cascaded/folded stepped‐impedance resonators is described. The key feature of the proposed method is to facilitate stronger coupling between stepped‐impedance resonators and, at the same time, eliminate the requirement of extremely small gaps in coupled‐line sections, as found in traditional designs. Simulations and measurements demonstrate that the filters designed with this technique exhibit good reflection, insertion‐loss, and group‐delay performance within the 3.1–10.6 GHz band. © 2009 Wiley Periodicals, Inc. Int J RF and Microwave CAE 2010.     

Simultaneous Microwave Extraction and Separation of Volatile and Non-Volatile Organic Compounds of Boldo Leaves. From Lab to Industrial Scale

Microwave extraction and separation has been used to increase the concentration of the extract compared to the conventional method with the same solid/liquid ratio, reducing extraction time and separate at the same time Volatile Organic Compounds (VOC) from non-Volatile Organic Compounds (NVOC) of boldo leaves. As preliminary study, a response surface method has been used to optimize the extraction of soluble material and the separation of VOC from the plant in laboratory scale. The results from the statistical analysis revealed that the optimized conditions were: microwave power 200 W, extraction time 56 min and solid liquid ratio of 7.5% of plants in water. Lab scale optimized microwave method is compared to conventional distillation, and requires a power/mass ratio of 0.4 W/g of water engaged. This power/mass ratio is kept in order to upscale from lab to pilot plant.     

A new continuous-flow recycle microwave reactor for homogeneous and heterogeneous chemical reactions

A new continuous-flow recycle microwave reactor suitable for organic synthesis has been developed to handle 0.51 quantities of reagents. The apparatus, which is designed for laboratory use, operates at atmospheric pressure in open- or closed-loop mode. It is fitted with a temperature control system. We describe this novel reactor and illustrate its efficiency with examples of organic syntheses carried out using both homogeneous and heterogeneous reactions.     

Microwave-assisted extraction kinetics of terpenes from caraway seeds

The process conditions during the extraction of carvone and limonene from caraway seed (Carum carvi L.) with microwave-assisted extraction have been studied with respect to microwave power, radiation dose and extraction time in order to obtain the secondary metabolites selectively. Using classical solid–liquid extraction, limonene, carvone and fatty oils in both the raw material and the residual matrix material were extracted. Yields of limonene, carvone and total oil (C₁₆, C₁₈) were determined by GC and GC/MS analysis for both extracts. The effects of microwaves on cell walls and cells destruction could be seen on SEM micrographs.     

Ultrasound-Assisted Aromatisation with Condiments as an Enabling Technique for Olive Oil Flavouring and Shelf Life Enhancement

Olive oil flavour represents the most important factor that influences customer’s perception for quality. In this study, an innovative aromatisation approach that enhanced quality and shelf life of olive oil is tested by means of in situ ultrasound-assisted extraction of Carum carvi L. seeds in olive oil. After the flavouring process, carvone and limonene, representing 99 % of caraway essential oil, were identified in virgin olive oil as revealed by headspace solid-phase microextraction gas chromatograph coupled to mass spectrometer (HS-SPME gas chromatograph (GC)/mass spectrometer (MS)) analyses. Furthermore, kinetic studies indicate that flavouring rate in ultrasound-assisted system is faster than conventional aromatisation producing very stable aromatised oil with no changes in quality. This fact is attributed to ultrasound contribution to mass transfer intensification of essential oil components from seeds to the bulk medium, confirmed by scanning electron micrograph (SEM) micrographs in which cell damage and exudation of its main content are illustrated. However, it is important to note that ultrasound-treated samples produce higher degrees of conjugated dienes and conjugated trienes compared to conventional maceration. Nevertheless, this increase is not alarming and remains within permitted values of the European Community and the International Olive Oil Council (IOOC). Ultrasound-flavouring system stands as a fast alternative aromatisation method, which allows on top shelf life enhancement and olive oil quality preservation.     

Rapid and Green Analytical Method for the Determination of Quinoline Alkaloids from Cinchona succirubra Based on Microwave-Integrated Extraction and Leaching (MIEL) Prior to High Performance Liquid Chromatography

Quinas contains several compounds, such as quinoline alkaloids, principally quinine, quinidine, cinchonine and cichonidine. Identified from barks of Cinchona, quinine is still commonly used to treat human malaria. Microwave-Integrated Extraction and Leaching (MIEL) is proposed for the extraction of quinoline alkaloids from bark of Cinchona succirubra. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. Optimal conditions for extraction were obtained using a response surface methodology reached from a central composite design. The MIEL extraction has been compared with a conventional technique soxhlet extraction. The extracts of quinoline alkaloids from C. succirubra obtained by these two different methods were compared by HPLC. The extracts obtained by MIEL in 32 min were quantitatively (yield) and qualitatively (quinine, quinidine, cinchonine, cinchonidine) similar to those obtained by conventional Soxhlet extraction in 3 hours. MIEL is a green technology that serves as a good alternative for the extraction of Cinchona alkaloids.     

Combined extraction processes of lipid from Chlorella vulgaris microalgae: microwave prior to supercritical carbon dioxide extraction

Extraction yields and fatty acid profiles from freeze-dried Chlorella vulgaris by microwave pretreatment followed by supercritical carbon dioxide (MW-SCCO(2)) extraction were compared with those obtained by supercritical carbon dioxide extraction alone (SCCO(2)). Work performed with pressure range of 20-28 Mpa and temperature interval of 40-70 °C, gave the highest extraction yield (w/w dry weight) at 28 MPa/40 °C. MW-SCCO(2) allowed to obtain the highest extraction yield (4.73%) compared to SCCO(2) extraction alone (1.81%). Qualitative and quantitative analyses of microalgae oil showed that palmitic, oleic, linoleic and α-linolenic acid were the most abundant identified fatty acids. Oils obtained by MW-SCCO(2) extraction had the highest concentrations of fatty acids compared to SCCO(2) extraction without pretreatment. Native form, and microwave pretreated and untreated microalgae were observed by scanning electronic microscopy (SEM). SEM micrographs of pretreated microalgae present tearing wall agglomerates. After SCCO(2), microwave pretreated microalgae presented several micro cracks; while native form microalgae wall was slightly damaged.     

Sono–Soxhlet: In Situ Ultrasound-Assisted Extraction of Food Products

An improvement of Soxhlet extraction was designed and developed. The extraction process (Sono–Soxhlet) of oils from crushed dried olives was performed using an ultrasonic horn in situ to provided rapid and complete recovery of analytes from the matrix. The results were compared to conventional Soxhlet extraction using physicochemical characterization and gravimetric analysis and showed a substantial reduction in the extraction time without interfering on composition and quality of target extracts.