Flow-mode synthesis of biodiesel under simultaneous microwave-magnetic irradiation

In this study, aiming at optimization of a novel continuous biodiesel production system was developed by combining technologies based on microwaves and magnetic fields. Factors affecting microwave-assisted biodiesel (alkyl esters) production reaction were analyzed in this investigation. Studied factors included magnetic field intensity (0, 0.225 and 0.450 T), microwave power (400, 821, and 1181 W), percentages of KOH and NaOH catalysts at constant concentrations of 1 wt% (0, 50% and 100%), and percentages of ethanol and methanol at a constant molar ratio of 6:1 (0, 50% and 100%). Response Surface Methodology (RSM) was used to optimize the reaction conditions. RSM-based analysis indicated that, all independent parameters had significant effects on the reaction efficiency. Results of the investigations reveal that the largest effects on the conversion efficiency were due to type of alcohol and magnetic field intensity. The optimized conditions were found to be a magnetic field intensity of 0.331 T, a microwave power of 677.77 W, catalyst percentages of 30.35% and 69.65% for KOH and NaOH, respectively, and alcohol percentages of 80.47% and 19.53% for methanol and ethanol, respectively. Under the optimal conditions, yield of the reaction was 96.2%.     

Simultaneous Enzymatic Transesterification and Esterification of an Acid Oil Using Fermented Solid as Biocatalyst

This work studied the enzymatic synthesis of fatty acid ethyl esters (FAEE) for potential use as biodiesel via simultaneous esterification and transesterification of acid oil from macaúba in a solvent-free system. A fermented and dry babassu cake with lipase activity from Rhizomucor miehei was used as biocatalyst. FAEE content above 85% was achieved after 96 h of reaction with enzyme loading of 13 U per g of oil, 120 mmol of hydrous ethanol (95% ethanol and 5% water)/20 mmol of oil (molar ratio ethanol:oil of 6:1), at 40 °C. After two consecutive enzymatic reactions, 90.8 wt% FAEE content was obtained. These results demonstrate a promising transesterification/esterification method for FAEE production from an acid and low-cost oil and the process has potential to decrease the costs of enzymatic biodiesel production.     

Microwave Drying Kinetics of Okra

In this work, the effects of power level and sample mass on moisture content, moisture ratio, drying rate, and drying time of Turkey okra (Hibiscus esculenta L.) were investigated using microwave drying technique. Various microwave power levels ranging from to 180 to 900 W were used for drying of 100 g of okra. To investigate the effect of sample mass on drying, the samples in the range of 25 to 100 g were dried at microwave power level of 360 W. To determine the kinetic parameters, the drying data were fitted to various models based on the ratios of the differences between the initial and final moisture contents and equilibrium moisture content. Among of the models proposed, Page's model gave a better fit for all drying conditions used. The activation energy for microwave drying of okra was calculated using an exponential expression based on Arrhenius equation and was found to be 5.54 W/g.     

Synthesis of Biodiesel through Catalytic Transesterification of Various Feedstocks using Fast Solvothermal Technology: A Critical Review

The fossil fuel reserves are depleting at a more rapid rate as a result of the population growth and the ensuing energy utilization. Biodiesel is a mixture of fatty acid methyl esters produced from the transesterification of plant oils or animal fats. Moreover, the source of raw materials and manufacturing costs have become the major hurdle in the commercialization of biodiesel; thus, alternative sources such as the use of waste oils and non-edible oils together with biodiesel production techniques have long been considered. Selecting an appropriate feedstock and increasing production yield are two important approaches to decrease the costs of biodiesel production. Typically, biodiesel, which operates with electrical or conventional heating to generate high efficiency of the product, consumes a huge amount of power in a long reaction time. In contrast, chemical reactions speed up by microwave irradiation which results in producing high yields of product in a shorter chemical reaction time. In this extensive article, an effort has been made to review the use of microwave technology including multi-feedstock and recent studies on microwave-assisted heterogeneously catalyzed processes for biodiesel production. The heterogeneous catalyst performance has also been covered, including the measurement of their pysico-chemical properties. The microwave irradiation used for the synthesis of biodiesel is also included. In addition, the reaction variables impacting the transesterification process, such as heating system, microwave power, type and amount of heterogeneous catalyst, oil/methanol molar ratio, reaction time, temperature and mixing intensity, are covered. The final part of this article will cover the details of previously performed work on heterogeneous catalysts. Finally, energy balances for the traditional and microwave-based processes, conclusions, and recommendation on the topic are presented. The aim this article is to focus on recent studies on microwave-assisted heterogeneously catalyzed processes.     

Microwave polymerization of poly(methyl acrylate): Conversion studies at variable power

Methyl acrylate (MA) was polymerized by microwave radiation at three different powers, namely, 200, 300, and 500 W. The percentage conversion of the reaction was followed by Fourier transform infrared (FTIR) spectroscopy. The specimen temperature during the polymerization process was measured to select a suitable temperature for comparison with the conventional method. The results indicate that a similar comparable temperature of about 52° was found for all the microwave power settings tested. The microwave polymerization process was compared with that of the thermal method at 52(±1)° under comparable reaction conditions. The reaction rate enhancement of the microwave polymerization compared to the thermal method was found to be as follows: 275% for the 500 W, 220% for the 300 W, and 138% for the 200 W, indicating a significant correlation between the reaction rate enhancement and the level of microwave power used.     

Optimization of Microwave-Assisted Extraction of Astaxanthin from Haematococcus Pluvialis by Response Surface Methodology and Antioxidant Activities of the Extracts

Abstract

Microwave-assisted extraction (MAE) was applied for the extraction of astaxanthin from Haematococcus pluvialis and response surface methodology (RSM) was used to optimize extraction parameters to the content of astaxanthin. Four independent variables such as microwave power (W), extraction time (sec), solvent volume (mL), and the number of extraction were optimized in this paper. The optimal conditions were determined and tri-dimensional response surfaces were plotted from the mathematical models. The F-test and p-value indicated that microwave power, extraction time, the number of extraction, and their quadratic had a highly significant effect on the response value (p <0.01), then the solvent volume and the interaction effects of microwave power and the number of extraction also displayed significant effect (p <0.05). Considering the extraction efficiency, the optimized conditions of MAE were as follows: microwave power was 141 W, extraction time 83 sec, solvent volume 9.8 mL, the number of extraction four times. About 594 ± 3.02 µg astaxanthin was extracted from Haematococcus pluvialis the dried powders (100 mg) under the optimal conditions, and it close to the predicted contents (592 µg). The antioxidant activities of the extracts obtained under optimal conditions were analyzed, and the results showed that the extracts presented strong ability of inhibiting the peroxidantion of linoleic acid, exhibited strong radical-scavenging properties against the DPPH, as well as strong reducing power.     

Analysis of Energy Consumption in Drying Process of Non-Hygroscopic Porous Packed Bed Using a Combined Multi-Feed Microwave-Convective Air and Continuous Belt System (CMCB)

In this study, the analysis of energy consumption during the drying of non-hygroscopic porous packed bed by combined multi-feed microwave-convective air and continuous belt system (CMCB) was investigated experimentally. By using a combined multi-feed microwave-convective air and continuous belt system drier, the microwave power was generated by means of 12 compressed air-cooled magnetrons of 800 W each that give a maximum of 9.6 kW. The power setting could be adjusted individually in 800 W steps. Hot air with the maximum working temperature of 240°C was generated using 24 units of electric heater where the total power capacity is 10.8 kW. Most importantly, this work focused on the investigation of drying phenomena under industrialized microwave processing. In this analysis, the effects of the drying time, hot air temperature, porous structure (F-Bed and C-Bed), and location of magnetrons on overall drying kinetics and energy consumption were evaluated in detail. The results showed that the overall drying and energy consumption depend upon the porous structure, hot air temperature, and location of magnetrons. Furthermore, using the continuous microwave application technique had several advantages over the conventional method, such as shorter processing times, volumetric dissipation of energy throughout a product, and less energy consumption. The results presented here provided fundamental understanding for the drying process using a combined multi-feed microwave-convective air and continuous belt system in industrial size.     

Optimization of Microwave-Vacuum Drying of Button Mushrooms Using Response-Surface Methodology

Button mushrooms (Agaricus bisporous) were dried in a microwave-vacuum dryer up to a final moisture content of around 6% (d.b.). The effect of microwave power level (115 to 285 W), system pressure (6.5 to 23.5 kPa), and slice thickness (6 to 14 mm) on drying efficiency and some quality attributes (color, texture, rehydration ratio, and sensory attributes) of dehydrated mushrooms were analyzed by means of response surface methodology. A rotatable central composite design was used to develop models for the responses.Analysis of variance showed that a second-order polynomial model predicted well the experimental data. The system pressure strongly affected color, hardness, rehydration ratio, and sensory attributes of dehydrated mushrooms. A lower pressure during drying resulted in better quality products. Optimum drying conditions of 202 W microwave power level, 6.5 kPa pressure, and 7.7 mm slice thickness were established for microwave vacuum drying of button mushrooms. Separate validation experiment was conducted at the derived optimum conditions to verify the predictions and adequacy of the models.     

Drying uniformity analysis of pulse-spouted microwave–freeze drying of banana cubes

This article reports the investigation of the drying uniformity of a new drying technique called pulse-spouted microwave–freeze drying. A computer vision technique and mathematical statistics were used to evaluate the drying uniformity. The results show that low microwave power results in prolonged drying time (the drying time of 1 W/g was 6 h, which was longer than that for 2 and 3 W/g), whereas spouting time and the time interval show less influence on the drying time. Analysis from infrared camera photos reveals that lower microwave power, longer spouting interval, and longer spouting time could improve the temperature distribution. Sample 4 (power: 2 W/g, time: 3 s, interval: 300 s) had the best temperature distribution uniformity.     

Microwave Drying Kinetics of a Thin-Layer Liquorice Root

Liquorice root (LR) (Glycyrrize glabra) is known as a sweetener and medicine plant. Drying kinetics of LR with initial moisture content of 49.5% (wet basis (w.b)) were experimentally investigated in a microwave drying system. The drying experiments were carried out at different drying temperatures (40, 45, 50, and 55°C) and microwave power levels (250, 500 and 750 W). Several models from literature were selected to fit the experimental data. The fit quality of models was evaluated using the coefficient of determination (R²), sum square error (SSE), and root mean square error (RMSE). A new model has been proposed for LR drying in the microwave drying. This new model best describes the experimental data for LRs. The activation energy was calculated to be 46.807 kJ/mol and effective diffusivity ranged from 2.9 × 10^?9 to 5.41 × 10^?9 m²/s, depending on drying temperatures at constant microwave power level.     

Ultrasound-Enhanced Subcritical Water Extraction of Volatile Oil from Lithospermum erythrorhizon

An ultrasonic probe was introduced into the kettle of subcritical water extraction device to extract volatile oil from Lithospermum erythrorhizon. The effect of temperature, pressure, ultrasonic power, and frequency on the extraction yield was studied. Gas chromatography-mass spectrometry (GC-MS) was applied to the analysis of the compositions of volatile oil. The mechanism of ultrasonic enhanced subcritical water extraction (USWE) was discussed. The results showed that the ultrasound-assisted enhancement effect of 20 KHz was better than that of 36 KHz and increased with output power (0 ～ 250 W). The subcritical water extraction yield increased from 1.87% to 2.39% via ultrasonic oscillation (250 W, 20 KHz) at a temperature of 160°C and a pressure of 5 MPa in the 25-minute extraction. Nineteen components were identified chiefly consisting of 18 carbon unsaturated fatty acid methyl esters, hexadecanoic acid methyl ester and pentadecane. Mechanism of USWE was cavitation and mechanical effect.     

Optimizing Drying Conditions for Vacuum-Assisted Microwave Drying of Green Peas (Pisum sativum L.)

Green peas were dried in a vacuum-assisted microwave drying system. The effects of microwave power levels (100–300 W) and system vacuum (50–400 mm Hg) on drying parameters (viz. drying efficiency and drying time) and some quality attributes (viz. linear shrinkage, apparent density, green color, rehydration, and sensory attributes) of dehydrated peas were analyzed by means of response surface methodology. A face-centered central composite design was used to develop models for the responses. Analysis of variance showed that a second-order polynomial model predicted well the experimental data. The system microwave power level strongly affected quality attributes of dehydrated peas and drying parameters. A higher vacuum during drying resulted in a better quality product. Microwave power of 237.31 W and a 360.22 mm Hg vaccum were found to be optimum drying conditions for vacuum-assisted microwave drying of green peas.     

Ultrasonic Pretreatment Transesterification for Solid Basic-Catalyzed Synthesis of Fatty Acid Methyl Esters

Generally, ultrasound irradiation is required throughout the reaction for fatty acid methyl esters (FAME, namely, biodiesel) production, which is energy-consuming and difficult to scale-up. In order to improve the industrial application of ultrasonic technology, a systematic study of ultrasonic pretreatment solid basic (Na₂SiO₃)-catalyzed transesterification for FAME production from cottonseed oil was carried out, and the effect of ultrasonic waves on the properties of Na₂SiO₃ catalyst was assessed by X-ray diffraction (XRD), Fourier transform Infrared (FTIR) and scanning electron microscopy (SEM) characterization of fresh and collected catalysts. An ultrasonic frequency of 30 kHz, ultrasonic power of 200 W and ultrasonic pretreatment irradiation time of 30 min was determined to guarantee a satisfactory degree of transesterification. The optimum production was achieved in the reaction system at 45 °C with methanol/cottonseed oil molar ratio 5:1, catalyst dosage 3% and stirring speed 350 rpm resulting in a FAME yield of above 97% after 60 min of reaction under mechanical stirring with the ultrasonic pretreatment process. The new process has a shorter reaction time, a more moderate reaction temperature, a less amount of methanol and catalyst than only the mechanical stirring process without essential damage to activity and the structure of catalyst. These results are of great significance for applying the ultrasonic pretreatment method to produce FAME.     

Comparison of two alternatives of combined drying to process blueberries (O'Neal): Evaluation of the final quality

In this work, we examined and compared two combined alternatives for the drying of blueberries (O’Neal). Pretreatments of osmotic dehydration (60°Brix sucrose solution at 40°C for 6 h) and hot air drying (HAD) (60°C, 2.5 m/s for 90 min) were performed to reach the same water content. Pretreated blueberries were then dried by microwave at different microwave output power values: 562.5, 622.5, and 750 W. The combined drying processes were also compared with HAD alone (control). The effects of the processes over blueberries were studied in terms of decrease in water content, drying rate (DR), mechanical properties (firmness and stiffness), optical properties (L*, a*, and hue angle (h)), antioxidant capacity, and rehydration capacity. The hot air–microwave drying decreased the process time and presented a high drying rate compared with the osmotic dehydration–microwave processes and the control drying. In terms of quality, the antioxidant and rehydration capacities were the most affected. The results showed that the best drying method to obtain the desired final product was the hot air–microwave drying (750 W).     

Estimation of Effective Moisture Diffusivity of Okra for Microwave Drying

The effect of microwave output power and sample amount on effective moisture diffusivity were investigated using microwave drying technique on round okra (Hibiscus esculentus L.). The various microwave output powers ranging from 180 to 900 W were used for the determination of effective moisture diffusivity for constant sample amount of 100 g okra. To examine the effect of sample amount on effective moisture diffusivity, the samples in the range of 25–100 g were dried at constant microwave output power of 360 W. By increasing the microwave output powers and decreasing the sample amounts, the effective moisture diffusivity values ranged from 20.52 × 10^?10 to 86.17 × 10^?10 and 34.87 × 10^?10 to 11.91 × 10^?9 m²/s^?1, respectively. The modeling studies were performed to illustrate the relationship between the ratio of the microwave output power to sample amount and effective moisture diffusivity. The relationship between drying constant and effective moisture diffusivity was also estimated.     

Biodiesel Production from Soybean Oil Catalyzed by Li<Subscript>2</Subscript>CO<Subscript>3</Subscript>

In the present study, we synthesized biodiesel from soybean oil through a transesterification reaction catalyzed by lithium carbonate. Under the optimal reaction conditions of methanol/oil molar ratio 32:1, 12 % (wt/wt oil) catalyst amount, and a reaction temperature of 65 °C for 2 h, there was a 97.2 % conversion to biodiesel from soybean oil. The present study also evaluated the effects of methanol/oil ratio, catalyst amount, and reaction time on conversion. The catalytic activity of solid base catalysts was insensitive to exposure to air prior to use in the transesterification reaction. Results from ICP-OES exhibited non-significant leaching of the Li₂CO₃ active species into the reaction medium, and reusability of the catalyst was tested successfully in ten subsequent cycles. Free fatty acid in the feedstock for biodiesel production should not be higher than 0.12 % to afford a product that passes the EN biodiesel standard. Product quality, ester content, free glycerol, total glycerol, density, flash point, sulfur content, kinematic viscosity, copper corrosion, cetane number, iodine value, and acid value fulfilled ASTM and EN standards. Commercially available Li₂CO₃ is suitable for direct use in biodiesel production without further drying or thermal pretreatment, avoiding the usual solid catalyst need for activation at high temperature.     

Drying Kinetics and Bioactivity of Beetroot Slices Pretreated in Concentrated Chokeberry Juice and Dried with Vacuum Microwaves

Beetroot slices 18 mm in diameter and with a thickness of 9.6, 6.3, 3.35, or 2.6 mm were pretreated in 40°Bx chokeberry juice at a temperature of 50°C for 2 h and then dried by a vacuum-microwave (VM) method at different microwave power levels, such as 120, 240, 360, 480, and 480/120 W. The drying kinetics were described by a fitted model that incorporated contributions from the surface area of the samples, microwave power, and VM processing time. As the microwave power during VM drying increased, the bioactive potential decreased for untreated samples and increased for pretreated samples. Increasing the samples' specific surface area resulted in shorter drying time, lower temperature of the material during drying, and enhanced quality of the dried product. For osmotically pretreated beetroot slices with a specific surface area of 827 ± 18 m²m^?3, a final VM drying step at 240 W is recommended to produce high quality vegetable snacks.     

Non-Uniformity of Surface Temperatures of Grain after Microwave Treatment in an Industrial Microwave Dryer

In this study, temperature rise and non-uniformity of heating of grain with different moisture contents after microwave treatment were investigated. The temperature anomalies after microwave treatment were measured for barley and wheat at four moisture levels (12, 15, 18, and 21% wet basis) and for canola at five moisture levels (8, 12, 15, 18, and 21% wet basis). Fifty grams of grain samples were heated in a laboratory scale, continuous-type, industrial microwave dryer (2450 MHz) at five power levels (100, 200, 300, 400, and 500 W) and two exposure times (28 and 56 s). Grain samples were thermally imaged using an infrared thermal camera as soon as they came out from the microwave chamber. Average, maximum, and minimum temperatures were extracted from each thermal image and the difference between maximum and minimum temperatures (ΔT) was calculated. The grain type had significant effect on the surface temperatures after microwave treatment. The surface temperatures increased with microwave powers and exposure times but decreased with moisture content. The average surface temperatures after microwave treatment were between 72.5 and 117.5°C, 65.9 and 97.5°C, and 73.4 and 108.8°C for barley, canola and wheat, respectively, when the applied microwave power was 500 W. At the same power level, the maximum surface temperature was between 100.3 and 140.0°C, 77.8 and 117.7°C, and 98.3 and 130.9°C for barley, canola, and wheat, respectively. Non-uniform heating patterns were observed for all three grain types at all moisture contents, power levels, and exposure times. The ΔT was in the range of 7.2 to 78.9°C, 3.4 to 59.2°C, and 9.7 to 72.8°C for barley, canola, and wheat, respectively. The location of hot and cold spots may vary in different dryers based on the position of magnetron and other components, but almost similar non-uniform heating pattern is expected in all microwave dryers. Therefore, this non-uniformity must be taken into consideration while developing microwave processing systems for grains.     

Energy efficiency of a scaled-up microwave-assisted transesterification for biodiesel production

We propose a scalable and energy-efficient microwave-assisted chemical reactor for biodiesel production, which is composed of a partially modified conventional 10-L stainless steel vessel and a microwave coupler to enable an optimized microwave injection of 99% power efficiency. The microwave power applied via a waveguide can be directly injected into the reaction vessel using a coupling rod clamped to a pressured microwave window, giving convenience of scale-up of the reactor volume because a conventional microwave transparent vessel like glass is not need. Microwave-assisted transesterification of triglycerides with potassium hydroxide catalyst achieved an accelerated conversion of 95% in 5 min. The precisely measured microwave energy consumption was only 87% of the calculated heat requirement for both the reactant and the vessel. Computer simulation studies indicated that the cause of the energy efficiency for microwave heating was the relatively low temperature of the vessel due to a reverse temperature gradient, in contrast to those done with conventional hot wall heating.     

Analysis of Energy Consumption in Drying Process of Biomaterials Using a Combined Unsymmetrical Double-Feed Microwave and Vacuum System (CUMV)—Case Study: Tea Leaves

An energy analysis of drying of biomaterials (tea leaves) was conducted on a combined unsymmetrical double-feed microwave and vacuum system (CUMV) to optimize the operating conditions and quality of the products. Tea leaves were dried from an initial moisture content of 172 to 7% (db). An energy consumption model based on the first law of thermodynamics was developed to evaluate energy efficiency. The influences of microwave power, vacuum pressure, and microwave operation modes on energy consumption were investigated in detail. The results showed that energy consumption as well as energy efficiency were strongly dependent on vacuum pressure and microwave power. Energy consumption and color parameters of the tea leaves were compared at different drying conditions. In particular, the experiments were carried out at different microwave powers (800 and 1,600 W) at a frequency of 2,450 MHz and different vacuum pressures (535 and 385 torr) to investigate the effects of these factors on the microwave–vacuum drying.