Separation Of Ethyl Acetate Research Articles

Separation of Ethyl Acetate and Ethanol Azeotropic System by Acetate-Based Ionic Liquid

Separation of Ethyl Acetate and Ethanol Azeotropic System by Acetate-Based Ionic Liquid

Exploration of different water content on the performance of reactive-extractive distillation for separating the ternary azeotropic mixture

Reactive-extractive distillation (RED) has gained significant attention as an innovative approach for separating azeotropic mixtures. Although many studies have reported its positive benefits, no studies have explored the impact of varying water content on RED performance, a domain that has seen exhaustive exploration in conventional extractive distillation. In this study, we investigate how water content affects RED performance using the separation of ethyl acetate (EA), 1,4-dioxane (DIO), and water as a case study. We design diverse configurations tailored for feed compositions ranging from 0.35 to 0.8 water mole fractions using a double column reactive-extractive distillation (DCRED). These configurations are globally optimized and the performance is compared against the triple-column conventional extractive distillation (TCCED) based on economic, environmental, and thermodynamic efficiency considerations. The TAC and CO2 emission of TCCED schemes exhibit the linear decreases, reaching its lowest point at 50 mol.% water content. Beyond this threshold, both indicators increase significantly, even surpassing the reference case (20 mol.% water) at 80 mol.% water content. The thermodynamic efficiency of TCCED behaves inversely due to the intrinsic exergy destructions. Interestingly, the DCRED schemes show almost linear decreases in the trends of both economic and environmental indicators, and the notable deviations are then observed at 65 mol.% water content, accompanied with a slight decrease up to 80 mol.%. The thermodynamic efficiency of DCRED scheme gives an inverse trend, identical to those observed in TCRED. Overall, TCCED performs best at 50 mol.%, in which DCRED excels at 80 mol.% water content. This comprehensive study bridges a significant knowledge gap, offering insights into optimizing RED processes for varying water content, an unexplored topic despite widespread application of RED.

Separation of ethyl acetate and ethanol by imidazole ionic liquids based on mechanism analysis and liquid–liquid equilibrium experiment

Azeotrope of ethyl acetate (EAC) and ethanol (EA) generated in the synthesis of ethyl acetate (EAC), was difficult to separate by general distillation. Liquid-liquid extraction using ionic liquids (ILs) as extractants is a green and efficient method for separating azeotropes. To select the suitable ILs, the σ-profiles of EAC, EA, and different anions of imidazole ILs were obtained through the COSMO-SAC model. Then, the extraction mechanism of ILs in the EAC-EA system was discussed from the micro perspective, the interaction between ILs and EA was analyzed graphically by the interaction region indicator (IRI) using the Multiwfn and VMD, the interaction energy between ILs and EA/EAC were calculated by Gaussian 09. Finally, we selected 1-ethyl-3-methyl-imidazolium dihydrogen phosphate ([EMIm][H2PO4]), 1-butyl-3-methyl-imidazolium dihydrogen phosphate ([BMIim][H2PO4]), 1-ethyl-3- methyl-imidazolium hydrogen sulfate ([EMIm][HSO4]), and 1-butyl-3-methyl- imidazolium hydrogen sulfate ([BMIm][HSO4]) as the extractants based on the mechanism analysis. The Liquid-liquid equilibrium(LLE) data of EAC-EA-ILs were measured at 298.15 K under atmospheric pressure; the effects of ILs with different alkyl chain lengths of cations on the extraction efficiency were investigated, and the influence of ILs with different anions was also verified through experiments. Meanwhile, we adopted the NRTL activity coefficient equation to regress the experiment data, and the interaction parameters were optimized by the least square method using Matlab 2014.

Tailoring Nanoporous-Engineered Sponge Fiber Molecular Sieves with Ternary-Nested Architecture for Precise Molecular Separation.

Polymeric fiber molecular sieves (PFMs) with ultrahigh surface areas, well-defined Murray's-law hierarchical nanoporous structures, and superior self-standing properties are of great interest for molecular-level separation applications. However, creating such PFMs has been proven extremely challenging. Herein, we report a cross-scale pore-forming strategy to create intriguing sponge fiber molecular sieves with hierarchical, tailorable, and molecularly defined nanoporosity by nanospace-confined chain-packing modulation at the molecular level. Robust secondary ultramicropores (<7 Å) and micropores (<2 nm) are in situ constructed in the macro/mesoporous skeletons of sponge fibers to realize a tunable pore size distribution. The resultant PFMs exhibit the integrated properties of ultrahigh surface area (860 m2 g-1), large pore volume (0.6 cm3 g-1), self-standing properties, and excellent molecular sieving performance and are widely applied in acetophenone/phenyl ethanol separation, hydrogen peroxide purification, ethyl acetate separation, and CO2 adsorption fields. The fabrication of such PFMs provides a feasible way for the design and development of polymeric fibrous sieves for molecular separation in large-scale chemical, energy, and environmental operation processes.

Column chromatography for separation and fractionation of flavor-active esters on hydrophobic resins and simulation of breakthrough behavior

For simulating an adsorption/elution step for separation and recovery of flavor-active esters in beer in the presence of ethanol at various temperatures, and validating the predicted breakthrough behavior, equilibrium data on concentration of each ester is required. This work evaluates the application of frontal analysis method (FA) for prediction of breakthrough behavior for adsorption of ethyl acetate, and determination of equilibrium concentrations and binding capacity for competitive adsorption of four major flavor-active esters in beer (i.e. ethyl acetate, isopentyl acetate, ethyl 4-methylpentanoate, and ethyl hexanoate), together with improvement of the obtained results, through fraction collection, and offline analysis, on columns packed with hydrophobic resins, Amberlite XAD16N and Sepabeads SP20SS. Single-component adsorption of ethyl acetate reveals a shorter breakthrough time, and higher slope of breakthrough curve for adsorption on SP20SS, due to smaller particle size, (50–100 µm), and enhanced mass transfer characteristics of this resin. Competitive frontal analysis tests, neatly demonstrate that increase in temperature is not favorable for adsorption but aids the elution step, 63–100% recovery of flavors at 333.15 K in comparison to 40–80% recovery at 298.15 K. Lower binding capacity of esters and shorter adsorption/elution cycle time is achieved at higher ethanol concentration and cyclic operation simulated under non-isothermal condition, exhibit higher accuracy between predicted and experimental breakthrough curves for XAD16N. A cyclic operation is simulated, for a larger scale column, for two scenarios, separation of ethyl acetate and complete separation of all flavor-active esters in the mixture. For more detailed prediction of breakthrough behavior, the influence of other components present in process streams needs to be investigated on competitive adsorption of esters.

Mixed matrix membrane of ZSM-5/poly (ether-block-amide)/polyethersulfone for pervaporation separation of ethyl acetate from aqueous solution

The ZSM-5/poly (ether-block-amide) (PEBA)/polyethersulfone (PES) dual layer mixed matrix membranes (MMMs) were prepared for pervaporation (PV) separation of ethyl acetate (EAc) from aqueous solutions. The ZSM-5 zeolite nanoparticles were synthesized by the conventional hydrothermal method and characterized using the XRD, XRF and FESEM analysis. The effect of top layer thickness, PEBA concentration, zeolite loading concentration, feed concentration and temperature on the separation performance of the prepared membranes was investigated. The FTIR, SEM, contact angle and swelling tests were used to characterize the fabricated MMMs. The results indicated that loading ZSM-5 zeolite nanoparticles into the PEBA matrix had a significant influence on the separation performance of the prepared membranes. The ZSM-5/PEBA/PES membrane containing 7.5 wt% ZSM-5 with a top layer thickness of 20 μm, showed the highest separation factor. The total flux was decreased by loading ZSM-5 into the membranes up to 7.5 wt% and further enhancement in the zeolite loading content resulted in increasing the total permeation flux. The best separation factor and total flux of the ZSM-5/PEBA/PES-07.5 membrane were found to be 108.52 and 1895 g m−2h−1, respectively for a feed concentration of 5 wt% EAc and temperature of 50 °C.

Separation of ethyl acetate and ethanol azeotrope mixture using dialkylphosphates-based ionic liquids as entrainers

Isobaric vapor-liquid equilibrium (VLE) data for the ternary systems of ethyl acetate + ethanol + 1-ethyl-3-methylimidazolium diethylphosphate ([EMIM][DEP]), ethyl acetate + ethanol + 1-butyl-3-methylimidazolium diethylphosphate ([BMIM][DEP]) and ethyl acetate + ethanol + 1-butyl-3-methylimidazolium dibutylphosphate ([BMIM][DBP]) were measured at 101.3 kPa. The results showed that all the three ionic liquids (ILs) produced remarkable salting-out effect, leading to the increase of the relative volatility of ethyl acetate to ethanol. Hence, the azeotropic point of ethyl acetate and ethanol could be eliminated with the addition of a certain content of ILs. The separation effect of the three ILs follows the order of [EMIM][DEP] > [BMIM][DEP] > [BMIM][DBP]. Then, the experimental VLE data were well correlated with the nonrandom two-liquid (NRTL) model. Finally, the σ-Profiles of solvents and ILs were used to analysis the micro-mechanism of the different separation performance of the three investigated ILs.

Kuersetin dari Daun Erythrina poeppigiana (leguminosae)

Erythrina plants known plants “dadap” is a higher plant that grows in tropical and subtropical regions. E. poeppigiana plants was a source of secondary metabolites, which contain flavonoids. This study aims to isolate the flavonoid compounds from the leaves of E. poeppigiana through the stages of extraction, fraction, separation and purification. E. poeppigiana leaves powder (2.5 kg) was extracted with methanol and partitioned with n-hexane and ethyl acetate. Furthermore, the separation of ethyl acetate of E. poeppigiana leaves fraction using a combination of column chromatographic was obtained pure compound (5 mg) in the form of a yellow amorphous solid. The chemical structure of pure compound was based on the data spectroscopy (MS, UV, IR, 1H-NMR and 13C-NMR) and identified as the compound 3,3 ‘, 4’, 5,7-pentahidroksiflavon or known as quercetin.

Microwave-assisted continuous reactive distillation process for preparation of ethyl acetate

AbstractAs a novel process intensification technology, microwave-assisted continuous reaction distillation (MRD) was proposed for the esterification reaction and separation of ethyl acetate (EtOAc). The effects of reflux ratio, mole ratio of acetic acid (HOAc) to ethanol (EtOH), reboiler duty, microwave power on EtOH conversions, EtOAc purity and mass ratio of distillate to feed (D/F) were explored. In comparison with conventional heating, the experimental results revealed that the EtOAc purity in the distillate under microwave conditions (MC) was improved. Computer simulations for conventional and MRD systems were performed using the Aspen Plus non-equilibrium stage model to substantiate the experimental results. The model predictions are in good agreement with the experimental data, revealing the accuracy and reliability of the non-equilibrium model. This new MRD process can be an effective and productive method of ester production.

Preparation of jujube-cake structure membranes through in situ polymerization of hyperbranched polysiloxane in ethylene-vinyl acetate matrix for separation of ethyl acetate from water

The addition of hyperbranched polysiloxane (HPSiO) could improve the hydrophobic of the membranes which is helpful to recover EA from water.

Separation of ethyl acetate (EA)/water by tubular silylated MCM-48 membranes grafted with different alkyl chains

The MCM-48 type materials and membranes had been successfully silylated with different alkyl chains (methyl, propyl and n-octyl). The silylated MCM-48 membranes prepared on supports with pore size of 1 μm had a good effect on separation of the ethyl acetate (EA)/water mixture. The materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), IR spectroscopy, pervaporation. These results showed that the silylated MCM-48 type materials could adsorb large amount of EA, about 145 mg/g for C 8H 17-MCM-48 at 7 kPa at the room temperature, which was ten times of the Si-MCM-48′. Besides this, the C 8H 17-MCM-48 membranes had EA/H 2O separation factor of 251 at room temperature and 123 at 50 °C with the total flux 4.3 and 6.6 kg/(m 2 h), respectively. The long-chain alkyl groups grafted in the membrane pore could enhance temperature tolerance of the membrane for separating EA/H 2O. Under the same conditions, the CH 3- and C 3H 7-MCM-48 membranes had lower separation factor and larger total flux. The phenomenon in the separation experiments was controlled by the solution-diffusion mechanism. EA molecules were firstly adsorbed in the silylated pores selectively and made up a compact hydrophobic membrane, which could prevent the penetration of the water, resulting in the high EA selectivity.

Separation of Ethyl Acetate−Ethanol Azeotropic Mixture Using Hydrophilic Ionic Liquids

The separation of ethyl acetate and ethanol (EtOH) is important but difficult due to their close boiling points and formation of an azeotropic mixture. The separation of the azeotropic mixture of ethyl acetate and EtOH using the hydrophilic ionic liquids (ILs) 1-alkyl-3-methylimidazolium chloride (alkyl = butyl, hexyl, and octyl) ([Cnmim]Cl, n = 4, 6, 8) and 1-allyl-3-methylimidazolium chloride and bromide ([Amim]Cl and [Amim]Br) has been investigated. Triangle phase diagrams of five ILs with ethyl acetate and EtOH were constructed, and the biphasic regions were found as follows: [Amim]Cl > [Amim]Br > [C4mim]Cl > [C6mim]Cl > [C8mim]Cl. The mechanisms of the ILs including cation, anion, and polarity effect were discussed. The results showed that the hydrophilic ILs [Cnmim]Cl (n = 4, 6, 8), [Amim]Br, and [Amim]Cl could remove EtOH effectively from the azeotropic mixture of ethyl acetate and EtOH. Moreover, it was found that [Amim]Cl had the highest extraction efficiency, and the purity of ethyl acetate cou...

Separation of Ethyl Acetate and Ethanol by Room Temperature Ionic Liquids with the Tetrafluoroborate Anion

Liquid–liquid equilibrium data are presented for mixtures of 1-ethyl-3-methylimidazolium tetrafluoroborate ([emim]BF4) or 1-(2-hydroxyethyl)-3-methylimidazolium tetrafluoroborate ([C2OHmim]BF4) or 1-ethyl-2,3-dimethylimidazolium tetrafluoroborate ([edmim]BF4) or 1-(2-hydroxyethyl)-2,3-dimethylimidazolium tetrafluoroborate ([C2OHdmim]BF4) + ethanol + ethyl acetate at 298.15 K. The distribution ratio and selectivity values, derived from the tie line data, show that [C2OHmim]BF4 has better extraction capacity than other studied ionic liquids and that a hydroxyl group on the cation and a CH3 group at the 2-position can obviously affect the interaction between the ionic liquid and ethanol. The experimental results show that [C2OHmim]BF4 is potentially a candidate to separate ethyl acetate and ethanol by liquid–liquid extraction. The experimental tie lines were correlated with the NRTL equation.

Enhancement of Solubility and Mass Transfer Coefficient Through Hydrotropy

This paper presents a comprehensive study on the effect of hydrotropes on the solubil- ity and mass transfer coefficient of ethyl acetate in water. The solubility and mass transfer studies were performed using hydrotropes such as tri-sodium citrate, urea, sodium benzoate, and sodium salicylate under a wide range of concentrations (0 to 3.0 mol/L) and system temperatures (303 to 333 K). The performance of the hydrotropes was measured in terms of the Setschenow constant (Ks). It was found that the solubility of ethyl acetate increases with increase in hydrotrope con- centration and also with system temperature. A Minimum Hydrotrope Concentration (MHC) in the aqueous phase was found required to initiate significant solubilization of ethyl acetate. Con- sequent to the increase in solubilization of ethyl acetate, the mass transfer coefficient was also found to increase with increase in hydrotrope concentration. All hydrotropes used in this work showed an enhancement in the solubility and mass transfer coefficient to different degrees. The maximum enhancement factor, which is the ratio of the value in presence and absence of a hy- drotrope, has been determined for both solubility and mass transfer coefficient. These character- istics would be much useful in increasing the rate of output of the desired product made from ethyl acetate. In addition, the separation of ethyl acetate from any liquid mixture which is found to be difficult can be carried out effectively using this technique.

Pervaporation of flavors with hydrophobic membrane

Using a pervaporation process, a surface-modified hydrophobic membrane was used for recovery of esters which are volatile organic flavor compounds; ethyl acetate (EA), propyl acetate (PA), and butyl acetate (BA). A surface-modified tube-type membrane was used to evaluate the effects of the feed concentration (0.15–0.60 wt%) and feed temperature (30–50 °C) on the separation of EA, PA, and BA from dilute aqueous solutions. The permeation flux increased with the increasing feed ester concentration and operating temperature. EA, PA, and BA in the permeate were concentrated up to 9.13–32.26, 11.44–34.95, and 14.96–36.37 wt%, respectively. The enrichment factors for the 0.15–0.60 wt% feed solution of EA and BA were in the range of 48.5-62.8 and 97.7-101.5, respectively. Phase separation occurred in the permeate stream because the ester concentration in the permeate was above the saturation limit. This meant that selectivity of the membrane was high enough for the recovery of esters from dilute aqueous solution, even though the enrichment factor of the membrane was lower than that of non-porous PDMS membrane. The fluxes of EA, PA, and BA at 0.60 wt% (6,000 ppm) feed concentration and 40 °C were 254, 296, and 318 g/m2.hr, which are much higher than those obtained with polymer membranes. In the case of non-porous PDMS at feed concentrations of 90-4,800 ppm and at 45 °C, it was reported that the permeate flux of EA was 1.1–5.8 g/m2.h. Compared to non-porous PDMS, the surface-modified membrane investigated in this study showed a much higher flux and enough selectivity of esters.

Recovery of Volatile Organic Flavor Compounds by Pervaporation

Esters of volatile organic flavor compounds were recovered from dilute aqueous solutions by pervaporation; ethyl acetate (EA), propyl acetate (PA), and butyl acetate (BA). A surface-modified tube-type alumina membrane was used to evaluate the effects of the feed concentration (0.15–0.60 wt%) and feed temperature (30–50°C) on the separation of EA, PA, and BA from dilute aqueous solutions. The permeation flux increased with the increasing feed ester concentration and operating temperature. The separation factors for the 0.15–0.60 wt% feed solutions of EA, PA, and BA at 40°C were in the range of 66.9–78.9, 86.0–89.0, and 117.1–94.7, respectively. EA, PA, BA in the permeate were concentrated up to 9.13–32.26, 11.44–34.95, and 14.96–36.37 wt%, respectively. Due to the high selectivity, phase separation occurred in the permeate stream because the ester concentration in the permeate was above the saturation limit. The fluxes of EA, PA, and BA at 0.60 wt% feed concentration and 40°C were 254, 296, and 318 g/m2·h, which are much higher than those obtained with polymer membranes. In the case of PDMS at feed concentrations of 90–4800 pp, and at 45°C, it was reported that the permeate flux of EA was 1.1–58 g/m2·h. Compared to PDMS, the surface-modified membrane investigated in this study showed a much higher flux of esters.

Vapor permeation of ethyl acetate, propyl acetate, and butyl acetate with hydrophobic inorganic membrane

Abstract This study is focused on the permeation characteristics of ester compounds from aqueous solutions through hydrophobic membrane; ethyl acetate (EA), propyl acetate (PA) and butyl acetate (BA). A surface-modified tube-type alumina membrane (Al 2 O 3 ) was used for ester compounds recovery by vapor permeation. Experiments were performed to evaluate the effects of the feed concentration (0.15–0.60 wt.%) and feed temperature (30–50 °C) on the separation of EA, PA, and BA from dilute aqueous solutions. It was found that the permeation flux increased with increasing feed ester concentration and operating temperature. The fluxes of EA, PA, and BA at 0.60 wt.% feed concentration and 40 °C were 282, 526, 661 g/m 2 h, which were much higher than those of polymer membranes. The separation factors for the 0.15–0.60 wt.% feed solution of EA, PA, and BA at 40 °C were in the range of 28.1–93.9, 83.6–129.4, and 190.7–209.9, respectively. The membrane tested showed high flux and high selectivity.

Improved hydrophobic zeolites to fill silicone membranes for ethyl acetate extraction from water by pervaporation

Two types of hydrophobic zeolites Y were prepared by treating the NaY-type zeolite with SiCl4, with or without subsequent hydrothermal treatment. X-ray diffraction analysis showed that the framework of the two modified zeolites Y are more perfect than that of the NaY one, and the Si/Al ratio is greatly enhanced by hydrothermal treatment. The determined sorption isotherms indicate an improvement of the ester-to-water sorption ratio with the increase in Si/Al ratio. When the zeolite-filled silicone membranes are used in separation of ethyl acetate - water mixture by pervaporation, both the total permeation flux and the selectivity to the ester are improved by the use of the hydrophobic zeolite Y as the filler in the membrane. The stronger the hydrophobicity of the zeolite Y, the higher the filled membrane selectivity.Key words: hydrophobic zeolites Y, silicone-filled membranes, ethyl acetate - water mixture, sorption, pervaporation.

Extraction of organics from aqueous solutions by pervaporation. A novel method for membrane characterization and process design in ethyl acetate separation

The separation characteristics of the GFT silicone composite membrane for the extraction of ethyl acetate from water were determined by vacuum pervaporation. Batch-type pervaporation of aqueous solutions of ethyl acetate was performed and the process was modelled. Parameters such as initial mass of the aqueous solution, membrane area, change in the membrane properties with the composition and temperature of the liquid mixture can be taken into account to predict the production capacity. The membrane time-area duality is theoretically shown by the established unique model for both batch and continuous operations enables the calculation of the parameters for a given separation. A new method for the rapid determination of membrane characteristics is proposed. It is based on a computer analysis of the depletion curves and permits the determination of the pervaporation flux and selectivity at different compositions with only one experiment, provided that the sorption at the membrane upstream face during the pervaporation experiment is fast enough compared with the diffusion through the membrane phase.