High-power ultrasound in olive paste pretreatment. Effect on process yield and virgin olive oil characteristics

The effect of high-power ultrasound on olive paste, on laboratory thermo-mixing operations for virgin olive oil extraction, has been studied. Direct sonication by an ultrasound probe horn (105 W cm⁻² and 24 kHz) and indirect sonication with an ultrasound-cleaning bath (150 W and 25 kHz) were applied and their effects compared with the conventional thermal treatment.

A quick-heating of olive paste, from ambient (12–20 °C) to optimal temperature conditions (28–30 °C), and an oil extractability improvement were observed when applying sonication. Better extractability was obtained by direct sonication for high moisture olives (>50%) whereas indirect sonication gave greater extractability for low moisture olive fruits (<50%).

Optimal application of ultrasound was achieved with direct sonication for 4 min at the beginning of paste malaxation and with indirect sonication during the malaxation time.

Effect of high-power ultrasound on oil quality parameters and nutritional and sensory characteristics were studied. Changes in quality parameters (free acidity value, peroxide value, K270 and K232) were not found, however significant effects on the levels of bitterness, polyphenols, tocopherols (vitamin E), chlorophyll and carotenoids were observed. Oils from sonicated pastes showed lower bitterness and higher content of tocopherols, chlorophylls and carotenoids. Related to sensory characteristics, off-flavour volatiles were not detected in oils from sonication treatments. Total peak areas of volatiles and the ratio hexanal/E-2-hexenal, as determined by SPME analysis, were lower than non-sonicated reference oils; sensory evaluation by panel test showed higher intensity of positive attributes and lesser of negative characteristics than those untreated.     

Working towards the development of innovative ultrasound equipment for the extraction of virgin olive oil

Malaxation has been recognized as one of the most critical points in the mechanical extraction process for virgin olive oil (VOO). It is a low and continuous kneading of olive paste at a carefully monitored temperature. Through this essential technological operation the small droplets of the oil formed during the milling merge into large drops that can be easily separated with a decanter centrifuge. During this technological phase, a complex and necessary bioprocess takes place in order to determine the quality and composition of the final product. The malaxer is a heat exchanger characterized by a low overall heat transfer coefficient because the ratio of surface area to volume is disadvantageous, so it is important to find an innovative technology to improve heat-exchange. As matter of fact, the malaxing step is the only discontinuous phase in a continuous extraction process. In the next future, the essential challenge of VOO industrial plant manufacturing sector is to design and build advanced machines in order to transform the discontinuous malaxing step in a continuous phase and improve the working capacity of the industrial plants. In order to reduce the malaxing time enhancing the quality of the product, two ultrasound-assisted virgin olive oil extraction processes were tested against the traditional method. The sonication treatment was applied on olives submerged in a water bath (before the crushing) and on olive paste (after the crushing). The ultrasound technology provides a reduction of the malaxing duration improving VOO yields and its minor compounds content. Better extractibility and higher minor compounds contents were obtained by sonicating the olives submerged in a water bath than olive paste. After experimental trials the results were employed to suggest innovative scaling up solutions of the process and new applications of ultrasounds in the VOO industry.     

Engineering design and prototype development of a full scale ultrasound system for virgin olive oil by means of numerical and experimental analysis

The aim of the virgin olive oil extraction process is mainly to obtain the best quality oil from fruits, by only applying mechanical actions while guaranteeing the highest overall efficiency. Currently, the mechanical methods used to extract virgin oils from olives are basically of two types: the discontinuous system (obsolete) and the continuous one. Anyway the system defined as “continuous” is composed of several steps which are not all completely continuous, due to the presence of the malaxer, a device that works in batch. The aim of the paper was to design, realize and test the first full scale sono-exchanger for the virgin olive oil industry, to be placed immediately after the crusher and before the malaxer. The innovative device is mainly composed of a triple concentric pipe heat exchanger combined with three ultrasound probes. This mechanical solution allows both the cell walls (which release the oil droplets) along with the minor compounds to be destroyed more effectively and the heat exchange between the olive paste and the process water to be accelerated. This strategy represents the first step towards the transformation of the malaxing step from a batch operation into a real continuous process, thus improving the working capacity of the industrial plants. Considering the heterogeneity of the olive paste, which is composed of different tissues, the design of the sono-exchanger required a thorough fluid dynamic analysis. The thermal effects of the sono-exchanger were monitored by measuring the temperature of the product at the inlet and the outlet of the device; in addition, the measurement of the pigments concentration in the product allowed monitoring the mechanical effects of the sono-exchanger. The effects of the innovative process were also evaluated in terms of extra virgin olive oil yields and quality, evaluating the main legal parameters, the polyphenol and tocopherol content. Moreover, the activity of the polyphenol oxidase enzyme in the olive paste was measured.     

Impact of pulsed ultrasound on bacteria reduction of natural waters

There is a limited work on the use of pulsed ultrasound for water disinfection particularly the case of natural water. Hence, pulsed ultrasound disinfection of natural water was thoroughly investigated in this study along with continuous ultrasound as a standard for comparison. Total coliform measurements were applied to evaluate treatment efficiency. Factorial design of 2³ for the tested experimental factors such as power, treatment time and operational mode was applied. Two levels of power with 40% and 70% amplitudes, treatment time of 5 and 15 min and operational modes of continuous and pulsed with On to Off ratio (R) of 0.1:0.6 s were investigated. Results showed that increasing power and treatment time or both increases total coliform reduction, whereas switching from continuous to pulsed mode in combination with power and treatment time has negative effect on total coliform reduction. A regression model for predicting total coliform reduction under different operating conditions was developed and validated. Energy and cost analyses applying electrical and calorimetric powers were conducted to serve as selection guidelines for the choosing optimum parameters of ultrasound disinfection. The outcome of these analyses indicated that low power level, short treatment time, and high R ratios are the most effective operating parameters.     

Effect of ultrasound on the flocculation-sedimentation and thickening of unclassified tailings

In back-fill mining, how to rapidly increase the concentration of tailings is an important problem facing mining engineers. In this paper, the effects of ultrasound frequency (17–25 kHz), power (50–100 W), duration (5–20 min) and start time (3–12 min) on the final underflow concentration (FUC) of unclassified tailings (UTs) were investigated. The flocculation-sedimentation and thickening of tailings were compared with and without ultrasound application. The response surface method was applied to analyze the primary and secondary relationships and interactive relationships between the various ultrasound operating parameters and the FUC, and the optimal conditions were determined. In addition, Environmental Scanning Electron Microscope (E-SEM) was used to analyze the structural changes of underflow aggregates and clearly demonstrated a denser underflow after ultrasound treatment. The results indicated that ultrasound can significantly improve the underflow concentration of the UTs slurry. The frequency and power are the most important influencing factors. The best conditions for ultrasound application are a frequency of 20.4 kHz, power of 90 W, duration of 6.2 min and start time at 15.0 min. The FUC reached 71.75% after several minutes of sonication, which is 4.31% higher than the FUC of free flocculation. The results of E-SEM analysis showed significant differences among the microstructures of settled tailings (STs) after free flocculation and 17 and 20 kHz ultrasound treatment. Ultrasound at a frequency of 20 kHz has a more effective mechanical vibration and cavitation action and can therefore effectively break the polymer flocculant chains into shorter chains and promote the compaction of tailings and the release of water. The size distributions of the flocs before and after sonication also support this conclusion.     

The ultrasound application does not affect to the thermal properties and chemical composition of virgin olive oils

In this work, the effects of high power ultrasound treatment (40 kHz) on virgin olive oil (VOO) for different times (0, 15, 30 min) were studied, in order to verify if extent modifications in their chemical composition and thermal properties. The effects of the different ultrasound treatments on VOOs were determined considering the following parameters: quality index (free acidity, K₂₃₂ and K₂₇₀), lipid profile (fatty acids and triglycerides composition) minor components (phenols, tocopherols, pigments and volatiles) and thermal properties (crystallization and melting) by Differential Scanning Calorimetry (DSC).During the ultrasound treatments, bubbles growth was present in the VOO due to the phenomenon of cavitation and a slight increase of the temperature was observed. In general, the ultrasound treatments did not cause alterations on VOO parameters evaluated (oxidation state, lipid profile, minor components and thermal profiles). However, a slight decrease was observed in some volatile compounds.     

Green ultrasound-assisted extraction of carotenoids from pomegranate wastes using vegetable oils

The objective of this work was to develop a new process for pomegranate peels application in food industries based on ultrasound-assisted extraction of carotenoids using different vegetable oils as solvents. In this way, an oil enriched with antioxidants is produced. Sunflower oil and soy oil were used as alternative solvents and the effects of various parameters on extraction yield were studied. Extraction temperature, solid/oil ratio, amplitude level, and extraction time were the factors investigated with respect to extraction yield. Comparative studies between ultrasound-assisted and conventional solvent extraction were carried out in terms of processing procedure and total carotenoids content. The efficient extraction period for achieving maximum yield of pomegranate peel carotenoids was about 30 min. The optimum operating conditions were found to be: extraction temperature, 51.5 °C; peels/solvent ratio, 0.10; amplitude level, 58.8%; solvent, sunflower oil. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters.     

Removal of colloidal precipitation plugging with high-power ultrasound

Petroleum is a continuous and dynamically stable colloidal system. In the process of oil extraction, transportation, and post-treatment, the stability of the petroleum sol system is easily destroyed, resulting in asphaltenes precipitation that can make pore throat, oil wells, and pipelines blocked, thereby damaging the reservoir and reducing oil recovery. In this paper, removing near-well plugging caused by asphaltene deposition with high-power ultrasound is investigated. Six PZT transducers with different parameters were used to carry out the experimental study. Results show that ultrasonic frequency is one important factor for removing colloidal precipitation plugging in cores, it could not be too high nor too low. The optimum ultrasonic frequency is 25 kHz; Selecting transducers with a higher power is an effective way to improve the removal efficiency. The optimum ultrasonic power is 1000 W. With the increase of ultrasonic treatment time, the recovery rate reaches the maximum and tends to be stable. ultrasonic processing time should be controlled within 120 min. Besides, three methods — ultrasonic treatment alone, chemical injection alone, and ultrasound-chemical method — for removing colloidal precipitation plugging are compared. Results indicate that the ultrasound-assisted chemical method is better than chemical injection alone or ultrasonic treatment alone to remove colloidal sediment in the core. Finally, the mechanism of the ultrasonic deplugging technique is analyzed from three aspects: cavitation effect, the thermal effect, and mechanical vibration.     

Influence of bleaching by ultrasound on fatty acids and minor compounds of olive oil. Qualitative and quantitative analysis of volatile compounds (by SPME coupled to GC/MS)

The effects of bleaching using high power ultrasound (20 kHz) on the quality of olive oil were considered in this study, in order to verify the modifications that can occur in fatty acid composition and minor compounds. During the treatment of olive oil under ultrasonic waves, a rancid odour has been detected. Treated olive oils show no significant changes in their chemical composition but the presence of some volatile compounds, due to ultrasonic treatment. Some off-flavour compounds (hexanal, hept-2-enal and 2(E),4(E)-decadienal) resulting from the sonodegradation of olive oil have been identified. A wide variety of analytical techniques (GLC, HPLC and GC/MS) were used to follow the quality of bleached olive oils with ultrasonic waves by the determination of the amounts of certain minor compounds such as sterols and tocopherols. Steradienes, resulting from the dehydration of sterols, were detected with small quantities especially in severe conditions of sonication. Solid phase micro-extraction (SPME) coupled to gas chromatography was known to be a sensitive technique to follow changes in the oxidative state of vegetable oils by measuring the amount of volatile materials produced during the refining process.     

Advances in ultrasonic production units for enhanced oil recovery in China

With the development of oil recovery technology, ultrasonic technology has been involved in oil production and oilfield development. The mechanism of ultrasonic wave plugging in near well is different from the conventional oil recovery technology. Ultrasonic oil production technique is an effective method to enhance oil production with low cost, good applicability, and no environmental pollution. The core part of ultrasonic oil production equipment for Enhanced Oil Recovery is a high-power ultrasonic transducer. The continuous high-power ultrasound is used to treat the reservoir, which changes the pore structure, the physical property and the state of the fluid, thus improving the permeability and flows conditions of the reservoir, and increasing the oil yield and oil recovery. Ultrasonic oil recovery equipment includes the generation of high-power ultrasonic signals, long-distance transmission and the conversion of electrical energy to acoustic energy. In this paper, state-of-the-art on the development of ultrasonic oil production devices for Enhanced Oil Recovery in China is introduced. The purpose of this paper is to provide a reference for the development of high-power ultrasonic oil extraction equipment and its promotion in tertiary oil recovery technology.     

Ultrasound assisted enzyme catalyzed hydrolysis of waste cooking oil under solvent free condition

The present work demonstrates the hydrolysis of waste cooking oil (WCO) under solvent free condition using commercial available immobilized lipase (Novozyme 435) under the influence of ultrasound irradiation. The process parameters were optimized using a sequence of experimental protocol to evaluate the effects of temperature, molar ratios of substrates, enzyme loading, duty cycle and ultrasound intensity. It has been observed that ultrasound-assisted lipase-catalyzed hydrolysis of WCO would be a promising alternative for conventional methods. A maximum conversion of 75.19% was obtained at mild operating parameters: molar ratio of oil to water (buffer pH 7) 3:1, catalyst loading of 1.25% (w/w), lower ultrasound power 100 W (ultrasound intensity – 7356.68 W m⁻²), duty cycle 50% and temperature (50 °C) in a relatively short reaction time (2 h). The activation energy and thermodynamic study shows that the hydrolysis reaction is more feasible when ultrasound is combined with mechanical agitation as compared with the ultrasound alone and simple conventional stirring technique. Application of ultrasound considerably reduced the reaction time as compared to conventional reaction. The successive use of the catalyst for repetitive cycles under the optimum experimental conditions resulted in a loss of enzymatic activity and also minimized the product conversion.     

Intensification of alkaline delignification of sugarcane bagasse using ultrasound assisted approach

Ultrasound-assisted approach has been investigated for delignification so as to develop green and sustainable technology. Combination of NaOH with ultrasound has been applied with detailed study into effect of various parameters such as time (operating range of 15–90 min), alkali concentration (0.25 M−2.5 M), solvent loading (1:15–1:30 w/v), temperature (50–90 ˚C), power (40–140 W) and duty cycle (40–70 %) at fixed frequency of 20 kHz. The optimized operating conditions established for the ultrasonic horn were 1 M as the NaOH concentration, 1 h as treatment time, 70˚C as the operating temperature, 1:20 as the biomass loading ratio, 100 W as the ultrasonic power and 70% duty cycle yielding 67.30% as the delignification extent. Comparative study performed using conventional and ultrasonic bath assisted alkaline treatment revealed lower delignification as 48.09% and 61.55% respectively. The biomass samples were characterized by SEM, XRD, FTIR and BET techniques to establish the role of ultrasound during the treatment. The morphological changes based on the ultrasound treatment demonstrated by SEM were favorable for enhanced delignification and also the crystallinity index was more in the case of ultrasound treated material than that obtained by conventional method. Specific surface area and pore size determinations based on BET analysis also confirmed beneficial role of ultrasound. The overall results clearly demonstrated the intensification obtained due to the use of ultrasonic reactors.     

Ultrasound pretreatment of wheat dried distiller’s grain (DDG) for extraction of phenolic compounds

Wheat Dried distiller’s grain (DDG), a coproduct from the ethanol production process, is rich in potentially health-promoting phenolic compounds. In the extraction of phenolic compounds from DDG, the DDG cell wall is an important barrier for mass transfer from the inside to the outside of the cell. The effect of high-power ultrasound pretreatment on destruction of DDG cell walls and extraction yield and rate was investigated. Direct sonication by an ultrasound probe horn at 24 kHz was applied and factors such as ultrasound power and treatment time were investigated. The method of nitrogen (N₂) adsorption at 77 K was used as a means to determine and compare the changes in physical properties (specific surface area, pore volume and pore size) of the treated samples at different levels of ultrasound power and treatment time. Increasing specific surface area, pore volume and pore size caused by ultrasonic treatment implied development of new or larger pores and damaged cell walls. Also, it was observed that the ultrasound pretreatment of DDG particles increased the extraction yield and rate of phenolic compounds from DDG by 14.29%. Among tested ultrasound conditions, 100% ultrasound power for 30 s was evaluated as the best pretreatment condition.     

Synthesis of biodiesel from waste cooking oil using sonochemical reactors

Investigation into newer routes of biodiesel synthesis is a key research area especially due to the fluctuations in the conventional fuel prices and the environmental advantages of biodiesel. The present work illustrates the use of sonochemical reactors for the synthesis of biodiesel from waste cooking oil. Transesterification of used frying oil with methanol, in the presence of potassium hydroxide as a catalyst has been investigated using low frequency ultrasonic reactor (20 kHz). Effect of different operating parameters such as alcohol–oil molar ratio, catalyst concentration, temperature, power, pulse and horn position on the extent of conversion of oil have been investigated. The optimum conditions for the transesterification process have been obtained as molar ratio of alcohol to oil as 6:1, catalyst concentration of 1 wt.%, temperature as 45 °C and ultrasound power as 200 W with an irradiation time of 40 min. The efficacy of using ultrasound has been compared with the conventional stirring approach based on the use of a six blade turbine with diameter of 1.5 cm operating at 1000 rpm. Also the purification aspects of the final product have been investigated.     

Sonoelectrochemical hydrogenation of safrole: A reactor design,statistical analysis and computational fluid dynamic approach

In this work, ultrasound-assisted electrocatalytic hydrogenation (US-ECHSA) of safrole was carried out in water medium, using sacrificial anode of nickel. The ultrasonic irradiation was carried out at frequency of 20 kHz ± 500 Hz with a titanium cylindrical horn (MS 73 microtip; Ti-6AI-4V alloy; 3.0 mm diameter). The optimal conditions were analyzed by statistical experimental design (fractional factorial). The influence of the sonoelectrochemical reactor design was also investigated by using computational fluid dynamics as simulation tool. Among the five parameters studied: catalyst type, use of β-cyclodextrin as inverse phase transfer catalyst, sonoelectrochemical reactor design, ultrasound mode and the temperature of the solution, only the last three were significant. The hydrogenation product, dihydrosafrole, reached 94% yield, depending on the experimental conditions applied. Data of computational fluid dynamics showed that a wing shape tube added to the sonoelectrochemical reactor can work as a cooling apparatus, during the electrochemical process. The reactional solution temperature diminishes 14 °C when compared to the four-way-type reactor. Cooper cathode, absence of β-cyclodextrin, four-way-type reactor, ultrasound continuous mode (14 W) and absence of temperature control were the most effective reaction parameters for the safrole hydrogenation using US-ECHSA method. The proposed approach represents an important contribution for understanding the hydrodynamic behavior of sonoelectrochemical reactors designs and, consequently, for the reducing of the experimental costs inherent to the sonoelectrochemical process.     

The promise of low-intensity ultrasound: A review on sonosensitizers and sonocatalysts by ultrasonic activation for bacterial killing

Antimicrobial resistance has become one of the main public health issues in modern society. Ultrasonic antimicrobial treatment (UAT) is expected to solve the problem of antimicrobial resistance since ultrasonic treatment does not cause drug resistance during inactivation. However, the ultrasonic application is hindered due to the high energy cost. To cast more lights on the ultrasound in tandem with catalysts as a superior strategy for bacterial inactivation, the present review focuses on the UAT with the assistant of continuous development of organic sonosensitizer and inorganic sonocatalyst. With the application of these nanomaterials, the ultrasonic parameters changed from low-frequency and high-power ultrasound to high-frequency and low-power ultrasound. The review also presents the composition of sonosensitizers/sonocatalysts including organic and inorganic nanoparticles and discusses the ultrasonic activation mechanisms triggered by these catalysts. Based on the synergistic effect of ultrasound and catalysts, we discuss the importance of extracellular oxidation and intracellular oxidation in the process of bacterial inactivation. Overall, UAT combined with catalysts appears to be an effective treatment strategy that can be successfully applied in the field of medicine, environmental treatment, and food industry.     

Enzymatic catalyzed palm oil hydrolysis under ultrasound irradiation: Diacylglycerol synthesis

Diacylglycerol (DAG) rich oils have an organoleptic property like that of regular edible oils, but these oils do not tend to be accumulated as fat. Palm oil ranks first in the world in terms of edible oil production owing to its low cost. The aim of this study was to propose a new methodology to produce diacylglycerol by hydrolysis of palm oil using Lipozyme RM IM commercial lipase as a catalyst under ultrasound irradiation. The reactions were carried out at 55 °C with two different methods. First, the reaction system was exposed to ultrasonic waves for the whole reaction time, which led to enzymatic inactivation and water evaporation. Ultrasound was then used to promote emulsification of the water/oil system before the hydrolysis reaction, avoiding contact between the probe and the enzymes. An experimental design was used to optimize the ultrasound-related parameters and maximize the hydrolysis rate, and in these conditions, with a change in equilibrium, DAG production was evaluated.Better reaction conditions were achieved for the second method: 11.20 wt.% (water + oil mass) water content, 1.36 wt.% (water + oil mass) enzyme load, 12 h of reaction time, 1.2 min and 200 W of exposure to ultrasound. In these conditions diacylglycerol yield was 34.17 wt.%.     

Intensified sonochemical degradation of 2-Picoline in combination with advanced oxidizing agents

2-picoline is a very important pyridine derivative with significant applications though it is also poisonous and harmful having considerable adverse influence on aquatic life, environment and organisms. The need for developing effective treatment methodologies for 2-Picoline directed the current work focusing on degradation of 2-Picoline using the combination of ultrasound and advanced oxidants such as hydrogen peroxide (H₂O₂), potassium persulphate (KPS), Fenton’s reagent, and Peroxymonosulphate (PMS) along with the use of Titanium oxide (TiO₂) as catalyst. Ultrasonic bath having 8 L capacity and operating frequency of 40 ± 2 kHz has been used. The effect of parameters like power, initial pH, temperature, time and initial concentration of 2-Picoline were studied to establish best operating conditions which were further used in the combination treatment approaches of ultrasound with oxidising agents. The chemical oxygen demand (COD) reduction for the optimized approaches of ultrasound in combination with oxidizing agents was also determined. Degradation experiments were performed using oxidising agents also in absence of ultrasound to investigate the individual treatment capacity of the oxidants and also the synergetic index for the combination. Kinetic study demonstrated that second order model suited for all the treatment approaches except US/Fenton where first order model fitted better. Ultrasound in combination with Fenton reagent demonstrated a substantial synergy for the degradation of 2-Picoline compared to other treatment approaches showing highest degradation of 97.6 %, synergetic index as 5.71, cavitational yield of 1.82 × 10⁻⁵ mg/J and COD removal of 82.4 %.     

Role of H2O2 in the fluctuating patterns of COD (chemical oxygen demand) during the treatment of palm oil mill effluent (POME) using pilot scale triple frequency ultrasound cavitation reactor

Palm oil mill effluent (POME) is a highly contaminating wastewater due to its high chemical oxygen demand (COD) and biochemical oxygen demand (BOD). Conventional treatment methods require longer residence time (10–15 days) and higher operating cost. Owing to this, finding a suitable and efficient method for the treatment of POME is crucial. In this investigation, ultrasound cavitation technology has been used as an alternative technique to treat POME. Cavitation is the phenomenon of formation, growth and collapse of bubbles in a liquid. The end process of collapse leads to intense conditions of temperature and pressure and shock waves which assist various physical and chemical transformations. Two different ultrasound systems i.e. ultrasonic bath (37 kHz) and a hexagonal triple frequency ultrasonic reactor (28, 40 and 70 kHz) of 15 L have been used. The results showed a fluctuating COD pattern (in between 45,000 and 60,000 mg/L) while using ultrasound bath alone, whereas a non-fluctuating COD pattern with a final COD of 27,000 mg/L was achieved when hydrogen peroxide was introduced. Similarly for the triple frequency ultrasound reactor, coupling all the three frequencies resulted into a final COD of 41,300 mg/L compared to any other individual or combination of two frequencies. With the possibility of larger and continuous ultrasonic cavitational reactors, it is believed that this could be a promising and a fruitful green process engineering technique for the treatment of POME.