Fast, easy ethanomethanolysis of Jatropha curcus oil for biodiesel production due to the better solubility of oil with ethanol in reaction mixture assisted by ultrasonication

Biodiesel was obtained by transesterification of Jatropha curcus oil with anhydrous methanol, ethanol, and various mixtures of methanol/ethanol system. The present research work ultrasonic assisted transesterification of J. curcus oil was carried out in the presence of various mixtures of methanol/ethanol system and potassium hydroxide (KOH) as a catalyst, keeping the molar ratio of oil to alcohol 1:6. The methodology allows for the reaction to be run under atmospheric conditions. The ethanomethanolysis and ultrasonic mixing promote the rate of transesterification reaction due to the better solubility of oil with ethanol in reaction mixture and obtained methyl esters as well as ethyl esters.     

Fast,easy ethanolysis of coconut oil for biodiesel production assisted by ultrasonication

Biodiesel is a renewable fuel, consistituting an alternative to petroleum-based diesel fuel. It is non-toxic and biodegradable and has a low emission profile, is better from environmentally sensitive areas. Research study on alternative fuels is essential for increased energy security. Presently, biodiesel is produced mainly is batch reactor. In this process the required energy is given by heating accompanied by mechanical stirring which has several disadvantages because of time consuming high labour cost. Being methanol is a toxic chemical; the objective of this work is to produce coconut oil ethyl ester by using ultrasonic irradiation. The advantages of ethanol are non-toxic domestic all available, having higher carbon atoms which provide higher heat content. The optical conditions for biodiesel production is the molar ratio oil to ethanol 1:6, KOH catalyst 0.75 wt.% of oil and 7 min reaction time. The reaction time reduced 15–40 times comparing to the conventional batch processes and found ?98% biodiesel yield.     

Time reducing process for biofuel production from non edible oil assisted by ultrasonication

Limited resources of conventional fuels such as petrodiesel have led to the search for alternative fuels. Various convention batch/continuous processes for the biodiesel production have been developed before the recent year. All processes are time consuming with high labor cost. Thus, we need a new process for biodiesel production which reduces the reaction time and production cost as well as save the energy. In this work, ultrasonic assisted transesterification of Jatropha curcas oil is carried out in the presence of methanol and potassium hydroxide (KOH) as catalyst, keeping the molar ratio of oil to alcohol 1:5, catalyst concentration 0.75 wt% of oil, ultrasonic amplitude 50% and pulse 0.3 cycle, 7 min reaction time under atmospheric condition. Ultrasonic mixing has increased the rate of transesterification reaction as compare to the mechanical mixing.     

Ultrasonic-assisted transesterification of Jatropha curcus oil using solid catalyst,Na/SiO2

The production of biodiesel from non-edible vegetable oil using ultrasonication, calls for an efficient solid catalyst to make the process fully ecologically and economically friendly. The methodology allows for the reaction to be run under atmospheric conditions. Solid catalyst and ultrasonication reduced the reaction time comparing to the conventional batch processes and we found 98.53% biodiesel yield. The optimal conditions for biodiesel production is the molar ratio oil to methanol 1:9, Catalyst conc. 3 wt.% of oil and 15 min reaction time.     

Ultrasound assisted enzyme catalyzed transesterification of waste cooking oil with dimethyl carbonate

This work reports the production of biodiesel with waste cooking oil and dimethyl carbonate in solvent free system through transesterification by immobilized enzyme (Novozym 435) under the influence of ultrasound irradiation. The experiments were conducted in an ultrasonic water bath under three different conditions i.e. ultrasonic irradiation (UI) without stirring, UI coupled with stirring and only stirring to compare their overall effects on fatty acid methyl esters (FAME) conversion. As compared with the conventional stirring method, where FAME conversion was 38.69% at 4 h, the UI without stirring significantly enhanced the conversion of enzymatic transesterification to 57.68% for the same reaction time. However the reaction rate was further increased under the condition of ultrasonication coupled with stirring and resulted into higher conversion of 86.61% for the same reaction time. Effects of reaction parameters, such as temperature, ratio of DMC/oil, speed of agitation and enzyme loading on the conversion were investigated. Furthermore, repeated use of Novozym 435 showed gradual decline in both conversion as well as enzyme activity.     

Ultrasonic biodiesel synthesis from crude Jatropha curcas oil with heterogeneous base catalyst: Mechanistic insight and statistical optimization

This paper reports studies in ultrasound-assisted heterogeneous solid catalyzed (CaO) synthesis of biodiesel from crude Jatropha curcas oil. The synthesis has been carried out in two stages, viz. esterification and trans-esterification. The esterification process is not influenced by ultrasound. The transesterification process, however, shows marked enhancement with ultrasound. A statistical experimental design has been used to optimize the process conditions for the synthesis. XRD analysis confirms formation of Ca(OMe)₂, which is the active catalyst for transesterification reaction. The optimum values of parameters for the highest yield of transesterification have been determined as follows: alcohol to oil molar ratio ≈ 11, catalyst concentration ≈ 5.5 wt.%, and temperature ≈ 64 °C. The activation energy of the reaction is calculated as 133.5 kJ/mol. The heterogeneity of the system increases mass transfer constraints resulting in approx. 4× increase in activation energy as compared to homogeneous alkali catalyzed system. It is also revealed that intense micro-convection induced by ultrasound enhances the mass transfer characteristics of the system with ∼20% reduction in activation energy, as compared to mechanically agitated systems. Influence of catalyst concentration and alcohol to oil molar ratio on the transesterification yield is inter-linked through formation of methoxy ions and their diffusion to the oil–alcohol interface, which in turn is determined by the volume fractions of the two phases in the reaction mixture. As a result, the highest transesterification yield is obtained at the moderate values of catalyst concentration and alcohol to oil molar ratio.     

Ultrasonically driven continuous process for vegetable oil transesterification

A bench scale continuous process for the manufacture of biodiesel from neat vegetable oils under high power low frequency ultrasonic irradiation was investigated. The experimental studies explored variations in alcohol-oil stoichiometry and type of oil. Important parameters such as residence time and reaction volume were considered. The highest conversion was achieved when short residence time was employed. The transesterification under ultrasonic irradiation is mainly influenced by the residence time in the reactor and alcohol-oil molar ratio.     

Aspects of ultrasonically assisted transesterification of various vegetable oils with methanol

The batch transesterification of vegetable oil with methanol, in the presence of potassium hydroxide as catalyst, by means of low frequency ultrasound (40 kHz) was studied with the aim of gaining more knowledge on intimate reaction mechanism. The concentration of fatty acid methyl esters, of mono-, di- and triglycerides of the actual reaction mixture were determined at short reaction time by HPLC. The effect of ultrasounds on the lipids transesterification correlated with triglyceride structures is discussed. It was found that under ultrasonic activation the rate-determining reaction switches from DG-->MG (classical mechanic agitation) to MG+ROH-->Gly+ME (ultrasonically driven transesterification).     

电感耦合等离子体串联质谱法分析麻疯树油中的多元素

工业化和现代化进程的加快消耗了大量能源,对能源的高度依赖性导致了全球化石能源需求的快速增长,随着非再生化石能源的日渐枯竭,迫切需要大力发展可再生能源以调整现有能源结构。作为国际上研究最多的生物柴油,麻疯树油是国内外公认的最有可能替代化石能源的再生能源,具有极大的开发潜力。麻疯树油中的微量元素在燃烧过程中会影响发动机的性能,并在尾气排放过程中决定了对环境所造成的污染程度。本文以获得麻疯树油中多元素的含量为目的,建立应用电感耦合等离子体串联质谱(ICP-MS/MS)法准确测定麻疯树油中低水平Na,Si,P,S,Cl,K,Ti,V,As含量的分析方法。采用微波密闭消解系统,依次向麻疯树油样品中加入硝酸和双氧水进行消解。详细地研究了各待测元素在不同分析模式下检出限(DL)和背景等效浓度(BEC)的变化情况,在MS/MS模式下,通过向碰撞/反应池(CRC)中加入反应气可以完全消除质谱干扰。选择O₂为反应气,P+,S+,Ti+,V+,As+与O₂的反应均为放热过程,能发生质量转移自发生成PO+,SO+,TiO+,VO+,AsO+,利用O₂质量转移法消除质谱干扰;选择H₂为反应气,Cl+与H₂反应能自发生成ClH+₂,利用H₂质量转移法消除质谱干扰,而Na+,Si+,K+均不能与H₂发生质量转移反应,利用H₂原位质量法消除质谱干扰。选择Sc为内标元素校正了分析过程中的基体效应。通过考察不同反应气流速下各元素的BEC变化,优化了反应气流速,O₂的最佳流速为0.45 mL·min-1,H₂的最佳流速为7.5 mL·min-1。在优化的实验条件下获得Na,Si,P,S,Cl,K,Ti,V,As的检出限分别为6.41,37.3,24.6,118,530,7.96,7.61,0.34,3.20 ng·L-1,各元素在0～50 μg·L-1范围内的线性相关系数(R2)≥0.999 8,方法具有良好的线性关系。采用三水平加标回收实验来验证方法的准确性和精密度,所有元素的加标回收率在91.2%～108%之间,相对标准偏差(RSD)为1.9%～4.6%,表明所建立的方法准确性好,精密度高。通过对来自中国不同地区的4个麻疯树油样品进行测定,结果显示,4个麻疯树油样品中P含量≤164 ng·g-1,S含量≤2310 ng·g-1,碱(Na+K)含量≤1 690 ng·g-1,三项指标均达到了中国生物柴油调和燃料国家标准,欧Ⅳ生物柴油标准,德国生物柴油标准和美国生物柴油标准。这项研究为麻疯树油中多种微量元素的准确分析提供了一种方便可行的新方法,为麻疯树油的质量控制和安全应用提供了科学的理论依据。     

Fish oil based vitamin D nanoencapsulation by ultrasonication and bioaccessibility analysis in simulated gastro-intestinal tract

Recently, nanoemulsions have been employed for different applications including food and drug industries for efficient nutrient delivery system. In this study, vitamin D (a lipophilic molecule) was encapsulated in fish oil for higher oral bioavailability. The oil-in-water nanoemulsion was formulated by ultrasonication technique with a droplet size range of 300–450 nm and a shelf life of more than 90 days. The influence of oil, water and surfactant concentration was investigated by phase diagram. The formulated nanoemulsion had encapsulation efficiency in the range of 95.7–98.2%. Further, nanoemulsion passed through simulated gastro-intestinal tract revealed an increased bioavailability than non-encapsulated vitamin. Thus, the formulation can be used as a drug delivery vehicle for various lipophilic compounds. Till date, no one have fabricated an efficient nano-vehicle for the delivery of vitamin D as well as analyzed the efficient delivery system in simulated GI-tract, this is first of its kind study in this regard. This can be scaled up further after analyzing the safety aspects.     

Ultrasound-assisted lipase-catalyzed transesterification of soybean oil in organic solvent system

This work reports the transesterification of soybean oil with ethanol using two commercial immobilized lipases under the influence of ultrasound irradiation. The experiments were performed in an ultrasonic water bath, following a sequence of experimental designs to assess the effects of temperature, enzyme and water concentrations, oil to ethanol molar ratio and output irradiation power on the reaction yield. Results show that ultrasound-assisted lipase-catalyzed transesterification of soybean oil with ethanol might be a potential alternative route to conventional alkali-catalyzed method, as high reaction yields (∼90 wt.%) were obtained at mild irradiation power supply (∼100 W), and temperature (60 °C) in a relatively short reaction time, 4 h, using Lipozyme RM IM as catalyst. The repeated use of the catalyst under the optimum experimental condition resulted in a decay in both enzyme activity and product conversion after two cycles. The use of Novozym 435 led to lower conversions (about 57%) but the enzyme activity was stable after eight cycles of use, showing, however, a reduction in product conversion after the forth cycle.     

Water Deficit and Salt Stress Diagnosis Through LED Induced Chlorophyll Fluorescence Analysis in Jatropha curcas L.

LED induced chlorophyll fluorescence analysis is employed to investigate the effect of water deficit and salt stress upon the growth process of Jatropha curcas L.. Red(Fr) and far-red(FFr) chlorophyll fluorescence around 685 nm and 735 nm, respectively, were observed and examined as a function of the stress intensity(salt concentration and water deficit). The fluorescence ratio Fr/FFr which is a valuable nondestructive and nonintrusive indicator of the chlorophyll content of leaves was exploited to monitor the jatropha plants under stress. The data indicated that salinity plays a minor role in the chlorophyll concentration of leaves for NaCl concentrations in the 25 to 200 mM range. The fluorescence ratio also permitted the detection of damage caused by water deficit in the early stages of the plants growing process. A significant variation of the Fr/FFr ratio was observed in the first 10 days of the experiment, and before signs of visual stress became apparent. The results suggest that the Fr/FFr ratio is an early-warning indicator of water deficit stress     

Preparation of magnetite–dextran microspheres by ultrasonication

An improved method of preparing magnetite–dextran microspheres by ultrasonication is proposed. Several parameters were evaluated and the characteristics of the microspheres investigated by scanning electron microscope (SEM), atomic force microscope (AFM), particle size analyzer and magnetometer. The results show that the initial Fe/dextran ratio is the most effective parameter for both the size and the magnetic properties.     

The effects of organoclay on the morphology and mechanical properties of PAI/clay nanocomposites coatings prepared by the ultrasonication assisted process

In this research, solvent based polyamide – imide (PAI)/clay nanocomposites were prepared successfully using the solution dispersion technique. With the assistance of the ultrasonic wave, the effect of the ultrasonic wave time on the microstructure of 3 wt% PAI/C20A nanocomposite (NC) was investigated. Then, the best ultrasonic parameters were selected and the effects of the concentration of Cloisite 20A (C20A) (1, 3 and 5 wt% C20A) on the microstructure and mechanical properties (adhesion, hardness, flexibility, wear and impact) of NCs were investigated. The PAI, C20A and nanocomposites (NC)s were characterized by Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray analysis (EDX), and Wide-angle X-ray diffraction (WAXD). The results showed that the sample with 1 and 3 wt% C20A had better mechanical properties, as compared to the pure PAI and the 5 wt% NC.     

Pulsed ultrasound assisted dehydration of waste oil

A method to aid the separation of the oil phase from waste oil emulsion of refineries had been developed by using a pulsed ultrasonic irradiation technology. Compared with conventional continuous ultrasonic irradiation, it is found that pulsed ultrasonic irradiation is much better to make water drop coalescence and hence dehydration of waste oil. The effects of ultrasonic irradiation parameters on waste oil dehydration are further discussed. The orthogonal experiment is also designed to investigate the degrees of influence of ultrasonic parameters and the optimal technological conditions. Under the optimal experimental conditions, the water content of waste oil is decreased from 65% to 8%, which thereby satisfies the requirements of refineries on the water content of waste oil after treatment (<10%).     

Biodiesel production from non-edible Silybum marianum oil using heterogeneous solid base catalyst under ultrasonication

The aim of this study is to investigate modified TiO₂ doped with C₄H₄O₆HK as heterogeneous solid base catalyst for transesterification of non-edible, Silybum marianum oil to biodiesel using methanol under ultrasonication. Upon screening the catalytic performance of modified TiO₂ doped with different K-compounds, 0.7 C₄H₄O₆HK doped on TiO₂ was selected. The preparation of the catalyst was done using incipient wetness impregnation method. Having doped modified TiO₂ with C₄H₄O₆HK, followed by impregnation, drying and calcination at 600 °C for 6 h, the catalyst was characterized by XRD, FTIR, SEM, BET, TGA, UV and the Hammett indicators. The yield of the biodiesel was proportional to the catalyst basicity. The catalyst had granular and porous structures with high basicity and superior performance. Combined conditions of 16:1 molar ratio of methanol to oil, 5 wt.% catalyst amount, 60 °C reaction temperature and 30 min reaction time was enough for maximum yield of 90.1%. The catalyst maintained sustained activity after five cycles of use. The oxidative stability which was the main problem of the biodiesel was improved from 2.0 h to 3.2 h after 30 days using ascorbic acid as antioxidant. The other properties including the flash point, cetane number and the cold flow ones were however, comparable to international standards. The study indicated that Ti-0.7-600-6 is an efficient, economical and environmentally, friendly catalyst under ultrasonication for producing biodiesel from S. marianum oil with a substantial yield.     

Ultrasound-assisted solid Lewis acid-catalyzed transesterification of Lesquerella fendleri oil for biodiesel synthesis

Biodiesel, a mixture of fatty acid methyl esters (FAME), is bio-renewable, non-toxic, biodegradable, and is an attractive alternative to petroleum diesel. This work studied the sonochemical transesterification of Lesquerella fendleri oil (LFO) using inexpensive solid Lewis acid (LA) catalysts with an aim to reduce environmental pollution and dependance on non-renewable fuel sources. Due to the presence of hydroxy fatty acid methyl esters (HFAME) in LFO (∼60%), in addition to producing biofuel it can also be used to generate chemically important estolides and cyclic lactones. AlCl₃, SnCl₂, and Sn(CH₃COO)₂ showed catalytic activity using direct immersion ultrasound (DI-US) among a list of LA catalysts investigated, with AlCl₃ being the best catalyst. Ultrasound increased the reaction rate by facilitating carbocation formation of glyceridic carbons. Experiments were carried out at room temperature in a solvent range from 3:1 to 18:1 methanol-to-oil molar ratio and catalyst loading from 1 wt% to 6 wt% over 10 to 60 min sonication time at 48% ultrasound amplitude (roughly 17 W/cm²). Complete conversion (>99%) was achieved in 40 min with 5 wt% AlCl₃ catalyst. A statistical regression analysis with STATA 14.0 software was performed to optimize process parameters. Chemical characterizations of the compounds were performed with nuclear magnetic resonance (NMR) spectroscopy (¹H NMR & ¹³C NMR), and % conversion of FAMEs was calculated from the ¹H NMR spectra. The fatty acid profile was determined by GC-FID and GC–MS analysis. FT-IR spectroscopic analysis and thermogravimetric analysis (TGA) were performed to investigate the infrared absorption pattern of the compound and the volatility difference between Lesquerella fendleri biodiesel and oil under nitrogen atmosphere. Results indicate that this is a fast, green, energy-efficient, sustainable, and industrially applicable method for biodiesel production from LFO.     

Ultrasound assisted enzymatic degumming of crude soybean oil

The present work deals with ultrasound assisted enzymatic degumming (UAED) of crude soybean oil quantifying the extent of degumming (EOD), cavitational yield and synergistic index (f) for the combination approaches. The effect of different operating parameters such as enzyme loading, pH, presence of water, temperature and ultrasonic power on the EOD has been investigated. Ultrasound combined with enzyme at loading of 2.0 ml/L resulted in EOD as 92.2% under ambient conditions. Addition of water (5%) in combination with ultrasound and enzyme at 2.0 ml/L loading and pH of 5 resulted in maximum EOD (98.4%) in 120 min of treatment. The extent of phospholipid separation was also observed to be dependent on the power dissipation and maximum phospholipids separation was obtained at 100 W. Scale-up studies were performed at 500 ml and 1 L operating volume under optimized conditions of 2.0 ml/L as the enzyme loading, pH of 5, 5% water addition and ultrasonic power of 100 W where 93.63% and 91.15% phospholipid separation respectively was obtained. The effects of ultrasonic treatment were also quantified in terms of the acid value reduction and oxidative stability for the processed oil. It was demonstrated that suitable reduction in acid value (final value less than 1) and oxidative stability (TOTOX less than 4) is effectively obtained using UAED. Overall the approach of UAED was established to show much higher efficacy for soybean oil processing as compared to only ultrasound or only enzymatic treatment.     

Green synthesis of garlic oil nanoemulsion using ultrasonication technique and its mechanism of antifungal action against Penicillium italicum

Penicillium italicum (P. italicum) can cause significant economic loss of fruits and vegetables. Although garlic oil (GO) is an effective antimicrobial agent, the unstability and hydrophobicity limit its use as an environmentally friendly alternative to the conventional antibiotics against P. italicum. In this study, we focused on the fabrication and characterization of a functional GO nanoemulsion (NE) using ultrasonic technique and revealed the antifungal mechanism of the GO NE on P. italicum based on morphological, structural and molecular analyses. The optimal hydrophilic lipophilic balance (HLB) value determined for GO was 14 through the combination of Tween 80 and Span 80. Then the Box-Benhnken Design (BBD) was applied to produce the GO NE and the effects of different fabrication parameters on the particle size were evaluated. The optimal GO NE was selected with the GO concentration of 5.5%, the Smix concentration of 10%, the ultrasonic time of 5 min and the power of 50%. This GO NE had the smallest particle size of 52.27 nm, the best antifungal effect and the most stability. Furthermore, the antifungal mechanism of the GO NE on P. italicum was evaluated by extracellular conductivity, micro-Raman spectra, fluorescence imaging and scanning electron microscopy (SEM) imaging. The results presented that the GO NE retained the antifungal active ingredients. The fungal cell structure and morphology were malformed after treated with the GO NE and the lipids, nucleic acids and protein of P. italicum were destructed. Finally, the optimal GO NE was applied in vivo and P. italicum in citrus was successfully inhibited. It indicated that the optimal GO NE had the better antifungal activity against P. italicum than the pure GO. Besides, the minimum inhibitory concentration (MIC) of GO after preparing into the NE was changed from 3.7% to 0.01265% with about 300 times improvement of bioavailability. Therefore, the synthetic GO NE which promoted the bioavailability of GO was recommended as a promising alternative to inhibit P. italicum in vegetables and fruits.     

Structuring functional mayonnaise incorporated with Himalayan walnut oil Pickering emulsions by ultrasound assisted emulsification

Nowadays Pickering emulsions have attracted immense attention due to their enhanced stability and numerous food applications. In this context, the present study was aimed to introduce Pickering emulsions stabilized by soy protein isolate (SPI)-maltodextrin (MD)-pectin complex incorporated with Himalayan walnut oil (HWO) for development of novel mayonnaise by ultrasound assisted emulsification. The functional mayonnaise was characterised for its stability, structural, textural, rheological and morphological properties. The rheological and microstructure measurements indicated that use of SPI-pectin HWO emulsions had a viscoelastic solid behaviour (G′ > G″) with highly interconnected gel-like network structure leading to diffused oil droplet distribution. An increase in particle size diameter (1.86–5.09 µm) and hardness values (43.16–69.08 N) was seen with increase in the SPI-pectin wall material concentration. A significant reduction in whiteness (L* value) from 91.12 to 53.52 was noted during storage for encapsulated samples. Mayonnaise formulations containing encapsulated HWO depicted significantly lower peroxide value (2.65 meqO₂/kg) after extended storage period in comparison to free oil (8.33 meqO₂/kg). FTIR analysis of mayonnaise formulations depicted successful complexation of HWO with SPI-MD-pectin matrix. These findings would be of immense importance in designing of Pickering emulsions stabilized by protein-polysaccharide particles with aim of delivering nutraceuticals associated with myriad health benefits.