Liquid–liquid extraction of levulinic acid from aqueous solutions using hydrophobic tri-n-octylamine/alcohol-based deep eutectic solvent

Levulinic acid(LA)is one of the top-12 most promising biomass-based platform chemicals,which has a wide range of applications in a variety of fields.However,separation and purification of LA from aqueous solution or actual hydrolysate continues to be a challenge.Among various downstream separation technologies,liquid-liquid extraction is a low-cost,effective,and simple process to separate LA.The key breakthrough lies in the development of extractants with high extraction efficiency,good hydrophobicity,and low cost.In this work,three hydrophobic deep eutectic solvents(DESs)based on tri-n-octylamine(TOA)as hydrogen bond acceptor(HBA)and alcohols(butanol,2-octanol,and menthol)as hydrogen bond donors(HBDs)were developed to extract LA from aqueous solution.The molar ratios of HBD and HBA,extraction temperature,contact time,solution pH,and initial LA concentration,DES/water volume ratios were systematically investigated.Compared with 2-octanol-TOA and menthol-TOA DES,the butanol-TOA DES exhibited the superior extraction performance for LA,with a maximum extraction efficiency of 95.79±1.4%.Moreover,the solution pH had a great impact on the LA extraction efficiency of butanol-TOA(molar ratio=3:1).It is worth noting that the extraction equilibrium time was less than 0.5 h.More importantly,the butanol-TOA(3:1)DES possesses good extraction abilities for low,medium,and high concentrations of LA.

Preparation and characterization of alumina nanoparticles in non-aqueous solution

Nanometer Al2O3powder is prepared by sol-gel method.Trans mission electron microscope(TEM),X-ray diffrac-tion(XRD),ther mal analysis,IR and the grain-testing instructure are used to characterize the particle shape and phase,chemical bonds of hydrous cassiterite andsize distribution after being heated.XRDand TEMshowthat the powder is fibrous γ-Al2O3at800 ℃andsphericalα-Al2O3at1 200℃.The grain-testinginstructure shows that the average particle diameter of γ-Al2O3is36.2nm while that ofα-Al2O3is125.6nm.The IRshows that aluminumstearate is synthesizedin the process of sol-gel.

Synergistic extraction of zinc from ammoniacal solutions using β-diketone mixed with CYANEX923 or LIX84I

The extraction behaviors of zinc from ammoniacal solutions were investigated using β-diketone （HA） and their mixtures with CYANEX923 or LIX84I. The effects of pH, total ammonia concentration, extractant concentration, anion species and temperature on zinc extraction were examined. The synergistic mechanism was discussed with regard to the structure of extractant and the extracted zinc complexes. It is found that the increase of total ammonia concentration and pH inhibits zinc extraction for all extraction systems due to the formation of zinc ammine complexes in aqueous phase. This effect of HA with CYANEX923 is evidently smaller than that of HA with LIX84I or HA alone system. Effect of anion species on the zinc extraction by HA with CYANEX923 can be neglected, but this effect of HA alone and the mixture of HA with LIX84I decreases in the order of （NH4）2SO4 〉 NH4NO3 〉 NH4Cl.

Solvent extraction of vanadium from sulfuric acid solution

The behaviour of vanadium（V） extracted from sulfuric acid solution was investigated using Cyanex 923 as an extractant. The effects of the concentration of Cyanex 923 and the pH of the solution were studied. The extraction of vanadium（V） increases with the increase of Cyanex 923 concentration and shaking time. Cyanex 923 can extract vanadium（V） from sulfuric acid solution at low pH conditions, and the best pH conditions for extraction of vanadium（V） are at pH 1.0-2.0. The species extracted into the organic phase is VO2HSO4 with one molecule of Cyanex 923. Equilibrium studies were used to assess the extraction efficiency of vanadium（V） recovery from the sulfuric acid solution.

COSMO-RS prediction and experimental verification of 1,5-pentanediamine extraction from aqueous solution by ionic liquids

1,5-Pentanediamine(PDA)produced by biological fermentation becomes popular,but the separation of PDA from the broth is a typical difficult problem.In this work,the performance of 200 ionic liquids(ILs),formed by combining 25 cations and 8 anions,in the extraction of PDA from aqueous solution were evaluated using COSMO-RS model.The extraction mechanism was investigated with the help ofσ-profile and interaction energy analyses.Both the cation and anion have impacts on the extraction efficiency,where cation mainly influences the interaction of IL with PDA and anion affects the hydrophobicity of IL.The IL composed of long alkyl-chain in cation and the anion of[PF6]-or[TF2 N]-,which has theσ-profile more likely distributed in the nonpolar region but less distributed in the polar region,is favorable for extraction.The experimental liquid-liquid equilibrium demonstrated the effects of cation and anion on extraction performance,which validated the reliability of COSMO-RS model in IL screening for PDA extraction.The IL[IM-1,8][PF6]could serve as a promising extractant for the downstream separation process of the biological production of PDA.

Study on Gold (Ⅰ) Solvent Extraction from Alkaline Cyanide Solution by TBP with Addition of Surfactant

The new solvent extraction system for gold() from alkaline cyanide solution by TBP with addition of surfactant in aqueous phase was studied. The effect of various factors, such as equilibrium pH, constitution of organic phase, molar ratio of CPBAu(CN)2-, extraction time, aqueous/organic phase ratio, different initial gold concentration, equilibrium temperature, different diluent, different types of extractants and surfactants etc., was inspected. The results show that gold() can be extracted quantitatively by controlling the quantity of surfactant (CPB); both the equilibrium pH and diluent hardly influence percent extraction. Gold() percent extraction reaches more than 98% under the optimal experimental conditions. 30% vol TBP diluted by sulphonating kerosene can load gold() to rather high levels. Loading capacity is in excess of 38 g/L. The extraction mechanism is discussed and the overall extraction reaction is deduced.

Synergistic Extraction of Gallium from Sulfate Solution

A novel extractant mixture, di-2-ethylhexyl phosphate (DEHPA) plusHX, was proposed and tested for recovering gallium from sulfatesolution. It was found that the extraction capacity of DEPHA forgallium from sulfate solution could be enhanced significantly due tothe synergistic effect of acidic extractant HX. Gallium extraction isnegligible below pH 0 and highly sensitive to pH of aqueous phase inthe range from 0 to 1, and satisfactory extraction can be gained atpH＞1. More than 96/100 Ga Extraction was obtained using 15/100 DEHPAplus 2/100 HX.

Enhanced extraction of scandium and inhibiting of iron from acid leaching solution of red mud by D2EHPA and sodium chloride

D2EHPA(P204),tri-butyl-phosphate(TBP)and sodium chloride(NaCl)were attractive for selective extraction of scandium from acid leaching solution of red mud.The extraction parameters of P204 concentration(X_(P204)),NaCl concentration(C_(NaCl)),pH value,reaction time,stirring speed and O/A were investigated to extract scandium and separate iron from the acid leaching solution.The extraction mechanism was analyzed by Fourier transform infrared spectroscopy(FT-IR)and thermodynamic theory.The single-stage extraction efficiency of scandium,iron andβ(Sc/Fe)were 99.1%,9.4%and 1061.2,respectively,with C_(NaCl) of 75 g/L and XP204 of 0.75 at solution pH value of 1.2 and stirring speed of 200 r/min for 6 min,in which a good separation effect of scandium and iron was obtained.The vibration absorption peak Sc─O was contributed to the extraction of scandium with P204.The complex[FeCln]^(3−n) existed in the solution with adding NaCl into the acid leaching solution.The value of n was higher and the valence state of the complex[FeCln]^(3−n) was lower with an increase of chloride concentration,which restricts the extraction efficiency of iron with P204.The extraction of three stages in the counter-current simulation experiments was carried out according to the McCabe-Thiele diagram.Gibbs free energy change(ΔG)of−5.93 kJ/mol,enthalpy change(ΔH)of 23.45 kJ/mol and entropy change(ΔH)of 98.54 J/(mol·K)were obtained in the solvent extraction proces,which indicate that the extraction reaction is easily spontaneous and endothermic and a proper increase of temperature is conducive to the extraction of scandium.

Alkaline extraction characteristics of steelmaking slag batch in NH_4Cl solution under environmental pressure

In order to obtain better carbonation effect, extraction behavior of slag batch is necessary to study. Relevant parameters like selective extraction yield were originally discussed. The relationship between selective extraction yield and conversion ratio was systemically focused on. The results show that alkaline earth metal conversion ratio is changed with leaching time and NH4CI concentration by first order exponential, and the maximum conversion for calcium keeps about 68% at 120 min in 0.4 mol/L NH4C1 solution, while leaching temperature and particle size have a linear effect on conversion ratio. Selective extraction yield of calcium is more than 93%, and the value of Mg is less than 5%. Apparent layer bands of silicon and calcium appear in the surface area through morphology detection of slag after leaching, and the case for 38-75 μm slag batch is more obvious than 75 150 μm slag and slag with larger particle size when leaching in 0.4 mol/L NH4Cl solution for 90 rain at 60 ℃.

Kinetic Mass Transfer Between Non-aqueous Phase Liquid and Gas During Soil Vapor Extraction

The mass transfer between non-aqueous phase liquid(NAPL) phase and soil gas phase in soil vapor extraction(SVE) process has been investigated by one-dimensional venting experiments. During quasi-steady volatilization of three single-component NAPLs in a sandy soil, constant initial lumped mass transfer coefficient (λgN,0) canbe obtained if the relative saturation (ξ) between NAPL phase and gas phase is higher than a critical value (ξc), andthe lumped mass transfer coefficient decreases with ξ when ξ＜ξc. It is also shown that the lumped mass transfercoefficient can be increased by blending porous micro-particles into the sandy soil because of the increasing of theinterfacial area.

Solvent extraction of zinc from zinc sulfate solution

The extraction of zinc from zinc sulfate solution was investigated, using 20% saponified D2EHPA as an extractam and 260^# sulfonate kerosene as a diluent. The solution was stirred for 8 min at phase ratio （Vσ/Va） of 1.0：1.0, initial pH of 2.0 and stirring speed of 200 r/min. The results show that 75% zinc can be extracted from the zinc sulfate solution when the concentration of zinc is 18.7 g/L after being settled for 10 min. 88.60% zinc can be stripped by 196 g/L sulfuric acid, and zinc ion can be separated from ferric ion.

Solvent extraction of copper and ammonia from ammoniacal solutions using sterically hindered β-diketone

Extraction of copper and ammonia from Cu2+-NH3-Cl--H2O solution using laboratorialy synthesized sterically hindered β-diketone(4,4-dimethyl-1-(4-dodecylphenyl)-1,3-pentanedione) was studied.The effects of the copper concentration,the total ammonia concentration,the initial pH in the aqueous phase,the phase ratio,and the temperature on copper extraction ratio and ammonia extraction in loaded organic phase were investigated using this sterically hindered β-diketone.Under the conditions of temperature 25℃,contact time of two phases 30 min,phase ratio 1-1,concentration of copper 3 g/L,concentration of total ammonia 3 mol/L,aqueous pH 8.43,and the concentration of β-diketone in organic phase 20%(volume fraction),ammonia in aqueous phase is much lower to be extracted by organic phase(just 14.5 mg/L),while the extraction rate of copper is 95.09%.

Comparative Study on the AUergenicity of DifferentLitopenaeus vannamei Extract Solutions

Allergen extracts are widely used for allergy diagnosis and treatment. The application of shrimp extract is hampered dueto the low protein concentration and the inconsistent allergenicity. Extracting solutions are considered to be the primary limitingfactor of protein extraction from crustaceans. This study aimed to select an optimal solution for shrimp protein extraction by com-paring the allergenicity of different shrimp extracts. The effect of 7 existing or modified extracting solutions were evaluated, includ-ing the glycerol-NaC1 solution, the glycerol Cocaine＇s solution, the buffered saline solution, the Cocaine＇s solution, the Glucoseleaching solution, 1 mol L-1 KC1 solution, and 0.01 mol L-1 phosphate buffered saline solution with and without dithiothreitolor （DTT）.The quantitative （protein concentration） and qualitative parameters （SDS-PAGE protein patterns and immuno-reactivity） were deter-mined using the sodium dodecyl sulfate polyacrylamide gel electrophoresis, enzyme linked immunosorbent assay and immunoblottingassay. Results showed that the 1 molL-1 KC1 solution with DTT was optimal for shrimp protein extraction, which yielded high con-centrafion and allergenicity in the protein extract, including major and minor allergens. The 1 tool L-l KC1 solution with DDT is pro-posed for preparation of shrimp extract and associated allergy diagnosis, as well as potential applications for other crustaceans.

Liquid-liquid extraction of phosphorus from sulfuric acid solution using benzyl dimethyl amine

This study addresses the liquid-liquid extraction behavior of phosphorus from a sulfuric acid solution using benzyl dimethyl amine(BDMA)in kerosene.The extraction equilibria investigated with varied BDMA concentrations could reveal the formation of 3[BDMA]·[H_(3)PO_(4)]^(-)complex in the organic phase.The thermodynamic properties determined at various temperatures indicated that the process was exothermic with a calculated enthalpy(△H^(Θ))of−24.0 kJ·mol^(−1).The organic-to-aqueous phase(O/A)volume ratio was varied to elucidate the quantitative extraction of phosphorus.The McCabe-Thiele diagram plotted for the extraction isotherm was validated for the requirement of three counter-current stages in the extraction at an O/A volume ratio of 2.0/3.5.The back-extraction of phosphorus from the loaded organic phase was quantitatively achieved by contacting 4.0 mol·L−1 H2SO4 solution in three stages of counter-current contact at an O/A volume ratio of 3/2.This study can be applied to remove phosphorus from the sulfuric acid leach solutions of monazite processing,and many other solutions.

Crude Extract of Detergent⁃Like Gleditsia sinensis lam Exhibiting Self⁃Organization for Protection of Mild Steel in Harsh Hydrochloric Acid Solution:How to Seek Crude Natural Plant Extracts as Green Corrosion Inhibitors

This study proposes a thought to employ detergent⁃like renewable low⁃cost crude extract of Gleditsia sinensis lam(GSL)as green corrosion inhibitor for mild steel in HCl solution.Crude Gleditsia sinensis lam extract(GSLE)was gained at mild conditions by simply refluxing in ethanol with a Soxhlet extractor.The target GSLE extract exhibited regular self⁃organization in mixed solvents of organic solvents/H2O such as ethanol/H2 O(v/v,50/50)at room temperature,which was evidenced by different means including scanning electron microscopy,transmission electron microscopy,and dynamic light scattering.The study demonstrates that the yielded assemblies of the crude extract of GSLE displayed chemical adsorption on the studied mild steel sample surfaces.Furthermore,the formed stable crude extract assemblies of GSL presented outstanding anti⁃corrosion capability in 1.0 mol/L HCl aqueous solution based on electrochemical measurements including polarization curves and impedance spectroscopy.It is discovered that the maximal corrosion inhibition efficiency could reach approximate 95%.The molecular modeling was performed to acquire the nature of frontier orbitals of the main representative chemical components of crude GSLE for deep understanding of chemical interactions with iron.The results presented herein would guide us to seek sustainable environmentally friendly low⁃cost detergent⁃like plant crude extracts for corrosion inhibition of various metals in aggressive acid environments.

Extraction of copper from bacterial leach solution using LIX98

Extraction of copper from bacterial leach solution using Lix984 had been performed. It was found that the main factors influencing extraction yield of copper are the phase ratio and the concentration of extractant, following the pH of solution and extraction time and the order of factors influencing the separation rate is the pH of solution, the concentration of extractant, the extraction time and the phase ratio. The best conditions obtained by the orthogonal tests are as follows: the extractant concentration 4%, extraction time 3 min, phase ratio 1∶1, pH of solution 2.

Precursor solution prepared by evaporation deamination complex method for solvent separation of Mo and W by H_2O_2-complexation

An novel method on preparation of precursor solution for solvent separation of molybdenum （Mo） and tungsten （W） by hydrogen peroxide （H2O2）-complexation from the ammonium tungstate solution containing high Mo was studied. The precursor solution was obtained via evaporation deamination and H202-complex transformation processes. Then it was extracted with a mixture extractant of tri-alkyl phosphine oxide （TRPO） and tributyl phosphate （TBP） to separate Mo and W. The results indicated that the evaporation deamination complex method reduced the acid consumption by more than 90% in comparison with the traditional directly acid regulation complex method. The transformation rates of W and Mo were higher than 95% and the decomposition rate of H202 was less than 15% at a 1.8-1.9 times H202 dosage, 45-50 ℃, initial pH of 1.80-1.90, and transformation volume ratio of 100% for 60 min in the H2O2-complexation transformation process. The minimum extraction rate of W was 2%, the maximum extraction rate of Mo was 82.6% and the highest separation coefficient was 76.7 in a single-stage extraction.

Solvent extraction of scandium from leaching solution of red mud roasted with ammonium sulfate using D2EHPA/TBP

Red mud is an important secondary resource for scandium production.The red mud leaching solution containing scandium in this study was derived from environmentally friendly ammonium sulfate roasting and water leaching process.A synergistic extraction with a mixture of di(2-ethylhexyl)phosphate acid(D2EHPA)and tributyl phosphate(TBP)for recovery of scandium from red mud leaching solution is proposed.The effects of D2EHPA concentration,H_(2)SO_(4)concentration,rare earth elements,dosage of TBP,phase ratio(A/O),contact time and H_(2)O_(2)concentration on scandium extraction were investigated.The results show that more than 99%scandium is extracted under the optimal conditions while Fe,Al,Ti,Ca and rare earth elements(Ce,Y,La,Nd,Er,etc.)are hardly extracted.The stripping efficiency of Sc reaches above 92.37%under the optimal stripping conditions of 5 mol/L NaOH with an A/O of 1 at 90℃for 30 min.The proposed technology could provide an effective method for extraction of scandium from red mud leaching solution.

Optimization of separation processing of copper and iron of dump bioleaching solution by Lix 984N in Dexing Copper Mine

The effects of the concentration of Lix 984N,phase ratio,initial pH value of aqueous phase and extraction time on the extraction of copper and iron under the condition of low Cu2+ /Fe3+ ratio in dump bioleaching solution of Dexing Copper Mine were explored.The optimal conditions of extraction are as follows: the concentration of Lix 984N 10%; the phase ratio (O/A) 1:1; the initial pH value of aqueous phase 1.5 and the mixing time 2 min.The stripping experiments show that H2SO4 solution could efficiently recover copper from the organic phase under the optimal conditions.

Research on the quality control technology for the Astragalus membranaceus extraction solution in cosmetics

Calycosin-7-glucoside,which is the target ingredient of the Astragalus membranaceus extraction solution,was studied by the high-performance liquid chromatography-diode array detector method(HPLC-DAD),and a high-performance liquid chromatography-electrospray ionization detector method(HPLC-CAD)was also established for fingerprint chromatogram analysis.Meanwhile,the heavy metal content was tested to build a quality control standard for Astragalus membranaceus extraction solution.Result shows a good linearity in 4-80μg/mL mass concentration range with the correlation coefficient r=0.999,RSD=2.4%,and the recovery rate is between 99.2%-102.7%.The fingerprint chromatogram analysis features with 14 specific peaks,including 5 identified components.The similarity is between 0.485 to 0.995.Content of heavy metals such as lead,mercury,and cadmium are below the detection limit,and the content of arsenic is less than 2 mg/kg.This research results can serve as process optimization basis and quality control standards for Astragalus membranaceus extraction solution,and provide reference to quality control and research guideline for other cosmetics using herbal extracts as raw materials.