Extraction of Mn(II) from NaCl solution by NaCl/sodium oleate/n-pentanol/n-heptane microemulsion system

A microemulsion (ME) consisting of sodium oleate, n-pentanol, n-heptane and sodium chloride (NaCl) solution was used for Mn(II) extraction. The cation exchange mechanism of Mn(II) extraction by sodium oleate (NaOL) was confirmed by the analysis of continuous variation of the NaOL concentration and the infrared spectrum. The effect of the extraction time, the cosurfactant type and volume fraction, the volume ratio of aqueous to ME (R), the initial concentration of Mn(II), temperature, pH and the NaCl concentration in aqueous phase on the extraction yield of Mn(II) were investigated. The extraction percentage of Mn(II) was up to 99% when R = 1. Both the extraction and re-extraction had good extraction efficiency. Therefore, the extraction of Mn(II) by NaCl/sodium oleate/n-pentanol/n-heptane ME is an effective approach.     

Extraction of acetyl 11-keto-β-boswellic acids (AKBA) from Boswellia serrata using ultrasound

The present work establishes the application of ultrasund for intensification of extraction of acetyl 11-keto-β-boswellic acid (AKBA), a potent anti-inflammatory agent from Boswellia serrata. Ultrasound-assisted extraction (UAE) yield is also compared with Soxhelt and batch extraction techniques. The optimized batch extraction showed 4.8 ± 0.04 mg/g yield of AKBA with extraction time of 120 min. On the other hand, UAE required only irradiation time of 10 min for obtaining a highest extraction yield of 6.5 ± 0.05 mg/g AKBA under optimized conditions. UAE reduced operation time and enhanced extraction yield of AKBA. Therefore, UAE could be the best alternative to intensify extraction.     

Effect of molecular weight on shape memory behavior in polyurethane films

Understanding the relationship between the number‐average molecular weight (M_n) and the shape memory behavior of polymers is crucial for a complete picture of their thermomechanical properties, and hence for the development of smart materials, and, in particular, in textile technology. We report here on the study of shape memory properties as a function of M_n of polymers. Shape memory polyurethanes (SMPUs) of different M_n were synthesized, with various catalyst contents or molar ratio(r = NCO/OH) in the composition. In particular, two types of SMPU, namely T_m and T_g types according to their switch temperature type, were synthesized to compare the influence of M_n on their shape memory behavior. X‐ray diffraction, differential scanning calorimetry, dynamic mechanical analysis, and shape memory behavior results for the SMPUs are presented. The results indicate that the melting temperature (T_m), the glass transition temperature (T_g), the crystallinity, and the crystallizability of the soft segment in SMPUs are influenced significantly by M_n, before reaching a critical limit around 200 000 g mol^?1. Characterization of the shape memory effect in PU films suggests that the T_m‐type films generally show higher shape fixities than the T_g‐type films. In addition, this shape fixity decreases with increasing M_n in the T_g‐type SMPU, but the shape recovery increases with M_n in both types of SMPU. The shape recovery temperature, in contrast, decreases with M_n as suggested by the result of their thermal strain recovery. It is concluded that a higher molecular weight (M_n > 200 000 g mol^?1) is a prerequisite for SMPUs to exhibit higher shape recovery at a particular temperature. Copyright © 2007 Society of Chemical Industry     

INFLUENCE OF SOLVENT POLARITY ON INTERFACIAL MECHANISM AND EFFICIENCY OF SUCCINIC ACID REACTIVE EXTRACTION WITH TRI-n-OCTYLAMINE

This article presents the results of a comparative study of reactive extraction of succinic acid with tri-n-octylamine (TOA) dissolved in solvents with different dielectric constants (dichloromethane, n-butyl acetate, and n-heptane), with and without octan-1-ol addition as phase modifier. The positive effect of octan-1-ol on extraction efficiency was quantified by means of amplification factors. For all studied systems, the addition of octan-1-ol into the solvent phase led to an increase of extraction efficiency, the most important effect being recorded for the solvent with the lowest polarity, namely n-heptane. The maximum value of amplification factor was reached for pH = 6 and indicated an increase of reactive extraction yield of about 1.26 times for dichloromethane, 1.55 times for n-butyl acetate, and 2.88 times for n-heptane.     

Studies on Third Phase Formation in the Extraction of Th(NO3)4 by Tri-iso-amyl Phosphate in n-alkane Diluents

Third phase formation in the extraction of Th(NO₃)₄ from its solution with near-zero free acidity by 1.1 M solutions of tri-iso-amyl phosphate (TiAP) in n-dodecane, n-tetradecane, n-hexadecane, and n-octadecane has been investigated as a function of equilibrium aqueous phase Th(IV) concentration at 303 K. Distribution of Th(NO₃)₄ between organic and aqueous phases as well as the variation of densities of organic phases in biphasic and triphasic regions for its extraction by the above-mentioned solvents have been investigated with respect to equilibrium aqueous phase Th(IV) concentration under the above experimental conditions. Data on the ratio of volume of the diluent-rich phase to that of third phase for various TiAP/n-alkane-Th(NO₃)₄-303 K systems have also been generated in the present study. The results obtained are compared with literature data available for tri-n-butyl phosphate (TBP) and tri-n-amyl phosphate (TAP) systems which were experimented under identical conditions.     

Prediction of long-term ABS relaxation behavior

The applicability of time–temperature superposition to tensile stress relaxation of ABS plastics has been verified at strains from 0.5 to 5% for temperatures in the range of 10–50°C. Master curves have been compiled to predict the long-term stress relaxation at 23°C. and a stress–strain–reduced time surface has been constructed. A comparison of relaxation times and activation energies has confirmed that a strain increase facilitates stress relaxation up to yield. The decay of relaxation modulus at linear viscoelastic strains was shown to be equivalent to that of tensile creep modulus. By normalizing the master curves to originate at yield stress and then converting them into multiaxial from the strain which gives the best data fit with long-term hydrostatic pipe-burst strength was shown to be at yield or beyond. The ABS yield-strain master curves at 23°C. were shown to match satisfactorily the long-term pipe-rupture data. Activation energies for ABS relaxation have been compared below and above the rigid matrix T_g, to assess the degree of stiffening of the polymer in the solid state.     

Intensification of 1‐phenylethanol production by periodical membrane extraction of the product from fermentation broth

BACKGROUND: Enantioselective bioreduction of acetophenone to S‐(?)‐1‐phenylethanol by Saccharomyces cerevisiae under non‐growth conditions is inhibited by the product created. This study investigated the possibility of intensification and mathematical simulation of 1‐phenylethanol production using periodic product removal carried out by membrane extraction in a hollow fiber membrane module. RESULTS: The highest reaction rate was observed at the beginning of the biotransformation. With increased product concentration in the reaction medium, the reaction rate gradually decreased by about 50% after 20 h of biotransformation. The low concentration of product maintained in the reaction medium using membrane extraction had positive influence on the 1‐phenylethanol production with a high yield (96%) and mean reaction rate of 0.226 mg h^?1g^?1, 35% higher than biotransformation without product removal. The equilibrium change and membrane fouling caused by biomass were not significant. It was possible to mathematically simulate the whole course of the extractive biotransformation with good agreement with experimental data. CONCLUSION: Bioreductive production of 1‐phenylethanol is more effective when using periodic membrane extraction of the product from the fermentation broth, which gives higher reaction rate, higher yield and simpler downstream process than biotransformation without product removal. Copyright © 2012 Society of Chemical Industry     

Mathematical model of supercritical extraction applied to oil seed extraction by CO2+saturated alcohol — I. Desorption model

Supercritical fluid extraction of solutes from solid matrix is represented by the extraction curve, where cumulated extracted oil is plotted versus time. Experimental data obtained in laboratory scale and pilot plant is adjusted with different extraction models; in order to predict extraction curves for full-scale extractors. Sometimes, a shortcut method is useful to adjust experimental data; these correlations are typical in most of engineering processes. In this paper, three shortcut methods are reviewed. First, a model based on flux models considering residence time distribution curves for serially interconnected perfectly mixed tanks and plug flow in series or in parallel with them. It could be used to analyze extractor behavior taking into account bed distribution (preferential ways, dispersion). Second, fast adjusting or ‘t^n’ model considers a differential mass balance where mass transfer coefficient is an ‘nth^’ potential function of time; analytical solution gives an explicit equation. Third, it is presented a linear shortcut method by intervals based on Sovovà model; it predicts considering four extraction periods: delay, rapid extraction, slow extraction and depletion; delay time and solubility are evaluated using the ‘t^n’ model. This model gives a process transfer function (Laplace domain). Supercritical fluid extraction of sunflower seed oil with carbon dioxide was performed in a pilot plant at 30.0 MPa and 40°C, using different amounts of methanol, ethanol, butanol and hexanol as cosolvents. Experimental data are fitted with proposed shortcut methods. Fitting error is less than 5% except in linear shortcut method by intervals which is higher.     

Advances in characterization of triacylglycerols: Expansion of materials used in Joint JOCS/AOCS Official Method Ch 3a-19

Joint JOCS/AOCS Official Method Ch 3a-19 was an improvement over triacylglycerol characterization methods based on hydrolysis with pancreatic lipase. In this study we developed three further improvements and applied them to the analysis of the fatty acid distribution in triacylglycerols from trout. First, the liquid–liquid extraction of lipid by chloroform and methanol from fish meat was replaced with a single extraction step using pre-packed columns. This allowed the extraction time to be reduced from 30 min/sample to 5 min/sample with ca. 10% higher yield using half the volume of the extraction solvent, chloroform. Both extraction methods gave similar FA composition of the extracted oil. Furthermore, an alternative CALB lipase and an alternative normal-phase solid phase extraction column were shown to reliably duplicate the results obtained with the Official Method Ch 3a-19. In addition, the SPE columns could be used at least 5 times without loss of separation and without carryover.     

Thermodynamic Properties of Aqueous Solutions of Alkanes under Supercritical Conditions

P–V–T–X relationships for the water–methane, water–n-pentane, water–n-hexane, water–n-heptane, and water–n-octane systems are derived by piezometry at a constant volume in the vicinity of the critical point of water (647.096 K) and up to 673.15 K at pressures up to 40 MPa and alkane mole fractions of 0–1.0. Conditions are determined under which real mixtures behave as an ideal gas or have a constant compressibility factor. It is demonstrated that the concentration dependence of the partial molar volumes of alkanes in the range of small concentrations is asymptotic if the isothermal isobar of the solvent is critical. The molecular parameters of the equation of state that is based on perturbed-hard-chain theory are determined and used in the calculation of thermodynamic parameters for this class of solutions.     

Process-intensified extraction of phycocyanin followed by β-carotene from Spirulina platensis using ultrasound-assisted extraction

ABSTRACT

The development of sustainable technology for the extraction of value-added products from the ecological feedstock is gaining importance. The present work focuses on the intensification of extraction of different metabolites such as phycocyanin and β carotene from microalgae (Spirulina platensis) and also presents the optimum extraction parameters using an ultrasound-assisted approach. Initially, phycocyanin was extracted from lyophilized biomass of Spirulina platensis using an ultrasound-assisted approach, and then the extract was centrifuged and the supernatant was treated by using the sugaring-out method to separate phycocyanin from chlorophyll. The remaining biomass was further used for the extraction of β-carotene using the same ultrasound-assisted approach. Various operating parameters such as amplitude, duty cycle, sonication time, and depth of horn immersed into the solution have been investigated for intensified extraction. Moreover, Taguchi design of experiments was used to evaluate the yield of β-carotene using the L₉ orthogonal array based on the effect of probe length, amplitude, duty cycle, and sonication time. On the basis of results and signal-to-noise (S/N) ratio analysis, a ranking of the parameters was performed. It can be noted here that the order of ranking was amplitude > sonication time > duty cycle > depth of horn immersing into the solution. Overall, it has been observed that maximum extraction of phycocyanin and β-carotene was 67 mg/g of dry biomass and 4.66 mg/g of dry weight, which was obtained at optimal amplitudes of 80% and 66% of the duty cycle and 0.5 cm depth of horn immersing into the solution in 4 min and 10 min, respectively. The present study clearly demonstrated that significant intensification benefits can be obtained in terms of the extraction of metabolites at optimal conditions using the ultrasound-assisted approach.     

Extraction and Fermentation‐Based Purification of Saponins from Sapindus mukorossi Gaertn.

In the present study, the extraction and purification of saponins from Sapindus mukorossi Gaertn. were examined for effective utilization of the saponin resource. Saponins were extracted from S. mukorossi Gaertn. using water. The conditions of the water extraction process, including extraction temperature, extraction time, number of times of extraction, and solvent‐material ratio were optimized. The yield of total Sapindus saponins (TSS) from the pericarp was 33.41 % and its purity in the extract was 45.71 %. The saponin solution was further concentrated to 1/6–1/7 of its original volume, and dried yeast BV818 that adapted to the concentrated Sapindus saponins solution (SW) was screened. The activation conditions, inoculum amount, fermentation temperature, and fermentation period were optimized. By using the dried yeast under optimized conditions, the purity was increased to 75.50 %. The yield of the byproduct ethanol was 5.33 % (w/v), while the content of TSS in the final product decreased from 18.29 to 15.30 % (w/v). These results could contribute to the development of industrial‐scale production of Sapindus saponins.     

The Effect of the Structure of Trialkyl Phosphates on their Physicochemical Properties and Extraction Behavior

The density of various trialkyl phosphates (TalP) such as tri‐n‐butyl phosphate (TBP), tri‐iso‐butyl phosphate (TiBP), tri‐sec‐butyl phosphate (TsBP), tri‐n‐amyl phosphate (TAP), tri‐2‐methylbutyl phosphate (T2MBP), tri‐iso‐amyl phosphate (tri‐3‐methylbutyl phosphate, TiAP), tri‐sec‐amyl phosphate (tri‐2‐amyl phosphate, TsAP), tri‐cyclo‐amyl phosphate (TcyAP), tri‐n‐hexyl phosphate (THP), and 1.1 M solutions of some of these phosphates in various diluents, solubility of water in trialkyl phosphates, and the aqueous solubility of trialkyl phosphates have been measured. Extraction of nitric acid, Th(IV), and U(VI) by trialkyl phosphates has also been studied by the batch extraction method. Metal‐solvate stoichiometry in the extraction of Th(IV) and U(VI) by some of the phosphates has been evaluated. Data on the extraction of U(VI) by various trialkyl phosphates as a function of equilibrium aqueous‐phase nitric acid concentration at 303 K are presented in this paper. Data on the extraction of Th(IV) and U(VI) from 1 M and 5 M HNO₃ by trialkyl phosphates as a function of equilibrium aqueous‐phase metal concentration at 303 K are also presented in this paper. The effects of the structure of trialkyl phosphates on their physicochemical properties and extraction behavior are described in this paper.     

Influences of phase composition and thermomechanical conditions on shape memory properties of segmented polyurethanes with amorphous reversible phase

We synthesized series of shape memory polyurethanes with amorphous reversible phase (T_g‐SMPUs) and systematically studied their microphase structure and shape memory properties. The T_g‐SMPUs having no or less hard phase showed lower shape recovery. When the volume fraction of hard phase was in the range of 20–30%, the T_g‐SMPUs exhibited the highest shape recovery. As the fraction of hard phase increased further the shape recovery decreased, because more polymer components with higher glass transition temperatures (T_gs) would participate in strain storage. For the T_g‐SMPUs having similar T_gs, those polymers having higher volume fraction of hard phase exhibited higher shape fixity, broader shape recovery region, and larger recovery stress. Increasing deformation strain could raise shape fixity and recovery stress but broaden shape recovery region. The highest recovery stress of a material could be achieved when the deformation occurred at its glass transition temperature below which decreasing deformation temperature could not increase recovery stress further. POLYM. ENG. SCI., 2012. © 2011 Society of Plastics Engineers     

Parameters Influencing Third‐Phase Formation in the Extraction of Th(NO3)4 by some Trialkyl Phosphates

Third‐phase formation in the extraction of Th(IV) by trialkyl phosphates (TalP) such as tri‐n‐butyl phosphate (TBP), tri‐iso‐butyl phosphate (TiBP), tri‐sec‐butyl phosphate (TsBP), tri‐n‐amyl phosphate (TAP), tri‐2‐methylbutyl phosphate (T2MBP), tri‐iso‐amyl phosphate (TiAP), tri‐sec‐amyl phosphate (TsAP), and tri‐cyclo‐amyl phosphate (TcyAP) has been investigated under various conditions. Formation of a third phase in the extraction of Th(IV) by TBP/n‐dodecane as a function of TBP concentration at 303 K was studied. Measurements were also carried out on the extraction of Th(IV) from its solution with near‐zero free acidity by various phosphate/diluent binary solutions (1.1 M) as a function of temperature. Third‐phase formation in the extraction of Th(IV) by 1.1 M TalP in various diluents from nitric acid media has also been studied as a function of equilibrium aqueous‐phase acidity at 303 K. Empirical equations to predict limiting organic concentration with respect to various parameters for third‐phase formation in the extraction of Th(IV) by TBP and TAP from nitric acid media have been derived. Some of the above phosphates have been investigated for the distribution of Th(NO₃)₄ between the “diluent‐rich phase” (DP) and “third‐phase” (TP) in the extraction of Th(IV) by 1.1 M TalP in various diluents from its saturated solution with near‐zero free acidity at 303 K. Results of the above studies are presented in this paper. Based on these studies, the effects of extractant concentration, the temperature, the nature of the diluent, the equilibrium aqueous‐phase acidity, and the structure of the extractant on third‐phase formation behavior of trialkyl phosphates are described in this paper.     

Thermal degradation of cellulose and cellulose esters

Cellulose, cellulose diacetate (CDA), cellulose triacetate (CTA), cellulose nitrate (CN), and cellulose phosphate (CP) were subjected to dynamic thermogravimetry in nitrogen and air. The thermostability of the cellulose and its esters was estimated, taking into account the values of initial thermal degradation temperature T_d, the temperature at the maximum degradation rate T_dm, and char yield at 400°C. The results show that these polymers may be arranged in the following order of increasing thermostability: CN < CP < regenerated cellulose < filter cotton < CDA < CTA. The activation energy (E), order (n), and frequency factor (Z) of their degradation reactions were obtained following the Friedman, Chang, Coats–Redfern, Freeman–Carroll, and Kissinger methods. The dependence of T_d, T_dm, E, n, Ln Z, and char yield at 400°C on molecular weight and test atmosphere is also discussed. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 68:293–304, 1998     

乙醇提取-丙酮沉淀法提取分离茶皂素的工艺研究

以油茶饼粕为原料，采用乙醇提取-丙酮沉淀法对茶皂素进行提取分离。以茶皂素纯度和得率为考察指标，对乙醇体积分数、液料比、提取温度、提取时间、提取次数、提取液浓缩程度和丙酮用量等工艺参数进行了单因素优化。结果表明：体积分数95%的乙醇为提取溶剂，乙醇与预处理过的油茶饼粕液料比为9：1（mL：g），提取温度为70℃，提取时间为4 h，提取次数为2次，提取液浓缩至刚好有固体析出，丙酮用量为4倍浓缩液体积量时提取分离效果较佳，得到的茶皂素纯度为85.17%，得率为9.82%。不同溶剂打浆对产品纯化效果的比较发现：丙酮、乙酸乙酯、无水乙醇、体积分数95%的乙醇作为打浆纯化溶剂用于提高茶皂素纯度效果均不明显。     

Response surface analysis of microwave‐assisted extraction of polysaccharides from cultured Cordyceps militaris

BACKGROUND: Microwave‐assisted extraction was employed to extract polysaccharides from cultured Cordyceps militaris. The optimal conditions for polysaccharide extraction were determined by response surface methodology. Box–Behnken design was applied to evaluate the effects of three independent variables (microwave power, extraction time and ratio of solution to solid) on the polysaccharide yield of C. militaris. RESULTS: Correlation analysis of the mathematical‐regression model indicated that a quadratic polynomial model could be employed to optimize the microwave‐assisted extraction of polysaccharide. Response surface plots showed that microwave power, extraction time and ratio of solution to solid exhibited independent and interactive effects on the extraction of polysaccharide. The optimal conditions to obtain the highest polysaccharide yield of C. militaris were a microwave power of 744.8 W, an extraction time of 4.2 min and a ratio of solution to solid of 31.1 mL g^?1. CONCLUSION: Under these optimal conditions, the experimental values agreed with the predicted values, using analysis of variance, indicating the goodness of fit of the model used and the success of response surface methodology for optimizing microwave‐assisted extraction of polysaccharide from C. militaris. Copyright © 2009 Society of Chemical Industry     

Synthesis of new polyesters with chelating subunits by solution and interfacial polycondensation

New polyesters have been prepared by solution and interfacial polycondensation of acid chlorides obtained from bis‐α,ω‐polymethylene‐[(2‐methoxy)phenoxy]acetic acids, acid‐ether siderophores AE _n (n being the number of methylene units), and diols including bisphenol A, ethylene glycol and propanediol. For interfacial polycondensation, average molecular weights range from 1000 to 4500 g mol^?1; at higher temperature the molecular weights increase but the yield is smaller. Differential scanning calorimetry shows T_g ranging from ?5 to + 110 °C. Polyesters are crystalline with n = 6 and amorphous with n = 2 and 4; in addition, increasing n in AE _n increases molecular weights and T_g values. In solution polycondensation, the average molecular weights are around 3000 g mol^?1 and T_g is low. © 2001 Society of Chemical Industry     

Phase behavior,density, and crystallization of polyethylene in n‐pentane and in n‐pentane/CO2 at high pressures

The phase behavior and volumetric properties of polyethylene (PE) in solutions of n‐pentane and n‐pentane/CO₂ were studied in a temperature (T) range of 370–440 K at pressures up to 60 MPa. Measurements were conducted with a variable‐volume view‐cell system equipped with optical sensors to monitor the changes in the transmitted light intensity as the P or the T of the system was changed. Lower‐critical‐solution‐temperature‐type behavior was observed for all of the liquid–liquid (L–L) phase boundaries, which shifted to higher pressures in solutions containing CO₂. The solid–fluid (S–F) phase boundaries were investigated over a P range of 8–54 MPa and took place in a narrow T range, from 374 to 378 K in this P interval. The S–F phase boundary showed a unique feature in that the demixing temperatures showed both increasing and decreasing trends with P depending on the P range. This was observed in both the PE/n‐pentane and PE/n‐pentane/CO₂ mixtures. The density of these solutions were measured as a function of P at selected temperatures or as a function of T at selected pressures that corresponded to the paths followed in approaching the phase boundaries (S–F or L–L) starting from a homogeneous one‐phase condition. The data showed a smooth variation of the overall mixture density along these paths. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 2201–2209, 2003