Deep eutectic solvents for separation and purification applications in critical metal metallurgy:Recent advances and perspectives

Solvent extraction,a separation and purification technology,is crucial in critical metal metallurgy.Organic solvents commonly used in solvent extraction exhibit disadvantages,such as high volatility,high toxicity,and flammability,causing a spectrum of hazards to human health and environmental safety.Neoteric solvents have been recognized as potential alternatives to these harmful organic solvents.In the past two decades,several neoteric solvents have been proposed,including ionic liquids(ILs)and deep eutectic solvents(DESs).DESs have gradually become the focus of green solvents owing to several advantages,namely,low toxicity,degradability,and low cost.In this critical review,their classification,formation mechanisms,preparation methods,characterization technologies,and special physicochemical properties based on the most recent advancements in research have been systematically described.Subsequently,the major separation and purification applications of DESs in critical metal metallurgy were comprehensively summarized.Finally,future opportunities and challenges of DESs were explored in the current research area.In conclusion,this review provides valuable insights for improving our overall understanding of DESs,and it holds important potential for expanding separation and purification applications in critical metal metallurgy.

Optimization of Preparative Separation and Purification of Total Flavonoids from Radix Puerariae by Macroporous Resin Method

Aim To screen the optimum macroporous resin and conditions for the isolation and purification of flavonoids from Radix Puerariae. Methods The static and dynamic adsorption/desorption methods were used, and the separation and purification process was evaluated by measuring the concentration of total flavonoid in the fractions with UV spectrophotometer. Results The SP70 macroporous resin was the most effective compared with other macroporous resins. The optimum conditions were screened, which were 0.5 g· mL^- 1 corresponding to crude drug for concentration of extract, pH 5 - 6, and appended 60 times the volume of the resin bed （BV） with the adsorption speed 2 BV·h^-1, and the volume of aq. 70% （V/V） ethanol as eluant was 5 BV with desorption speed 2 BV·h^-1. By this method, the final contents of total flavonoids exceeded 80%. Conclusion The SP70 macroporous resin is the most effective one for large-scale isolation and purification of flavonoids from Radix Pueraria, which meets industrial needs.

Separation and Purification of Recombinant Hirudin Variant 3 from Bacillus subtilis

[ Objective] The research aimed to get the optimized separation and purification conditions of the hirudin produced from Bacillus subtilis DB403 （pUBH5）. [Method] Through the systemic pretreatment, preliminary chromatography and fine chromatography. [Result]The optimized separation and purification conditions were that： Supernatant was treated by trichloroacetic acid, then by ultrafiltration desalt and anion exchange chromatography. Strong anion Q F. F. was better than weak anion DEAE F.F. The proper balanced solution was Tris-HCI （ pH 8.0）. The proper conductivity was 6 ms/cm. The maximum applied sample was 240 ATU/ml to matrix of strong anion Q F. F. This optimized procedure was magnified in strong anion exchange HiPrep 16/10Q with the 90% recovery and 70.2% purity. The purification of gel filtration of Sephacryl S-100 to hirudin was not relative to flow rate within certain scope. The application size of sample was 10 ml. The purity checked by HPLC was 95.1%, and the recovery was 93%, and the band of SDS-PAGE was single. [ Conclusion] The research provided the reference of the further industrialization separation and purification of hiruin.

Separation and recovery of Cu and As during purification of copper electrolyte

Cu, As, Sb and Bi in copper electrolyte could be efficiently removed by reducing with SO2 followed by evaporative crystallization. As2O3 and CuSO4·5H2O were obtained after crystallized product was treated by dissolution, oxidation, neutralization, sedimentation, filtration and evaporative crystallization. The removal rates of Cu, As, Sb and Bi are 87.1%, 83.9%, 21.0% and 84.7%, respectively, when As （Ⅴ） in copper electrolyte is fully reduced to As （Ⅲ） by SO2, and the H2SO4 in concentrated copper electrolyte is 645 g/L. The removal rate of As is 92.81% when 65 g crystallized product is dissolved in 200 mL water at 30 ℃. The CuSO4·5H2O content is 98.8% when the filtrate is purified under the conditions that n（Fe）：n（As） is 1.2, the dosage of H2O2 is 19 times the stoichiometric needed, temperature is 45 ℃, time is 40 min, pH is 3.7, and then is evaporation crystallized.

Separation and Purification of Antioxidant Endophytic Fungi from Stevia Leaves

[Objective] The aim was to separate and purify antioxidant endophytic fun- gi from Stevia leaves. [Method] Stevia leaves were used as materials for endophytic fungi screening and purification. Then, liquid culture was conducted to test fermented supernatant abilities of antioxidant, DPPH free radical clearing and chemilumines- cence inhibition. [Result] Forty two endophytic fungi were separated from F01 to F42. F41 was proved to be the strongest in antioxidant aspect; F37 was the strongest in DPPH clearing; F02, F07, F20, F25, F37, and F416 stood out in a comprehensive comparison of the above aspects. Flow injection chemiluminescenct method was used to test the above six fermentation liquors, and the results showed that antioxidant abilities of the six were quite strong for all of chemiluminescence rates were over 70%. Through preliminary morphological identification, bacterial colony was found white or yellowy and only F02 was of dissepiment. [Conclusion] Fungi with high-antioxidation activities were separated, which paved the way for future research.

Studies on Oxygen Characteristics of YBa_2Cu_3O_(7-x) and Its Applications to Air Separation and Gas Purification

Oxygen diffusion and oxygen selective adsorption properties of rare earths material YBa_2Cu_3O_(7-x) (YBCO) were investigated by thermogravimetric, oxygen static adsorption and selectivity adsorption experiments. The results show that YBCO is a very good deoxidizing material. The oxygen desorption of YBCO begins remarkably at about 400 ℃, mass loss can arrive at 1.2% of its original quantity at 800 ℃. Oxygen can be completely absorbed back into the sample again when temperature descends to 400 ℃. The oxygen adsorption selectivity, reproducibility and oxygen adsorption under very low oxygen partial pressure make the material desirable for air separation and gas purification. High purity nitrogen gas was produced with the YBCO molecular sieves in the air separation and gas purification experiments. 0.017 m^3 of high purity nitrogen (>99.9999%) can be obtained with 1 kg YBCO molecular sieve in one cycle. As a deoxidant, an obvious advantage of YBCO is that no hydrogen is needed in its applications.

Separation and purification of deoxynivalenol(DON) mycotoxin from wheat culture using a simple two-step silica gel column chromatography

Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo and in vitro. In this work, wheat culture was inoculated with a Fusarium graminearum PH-1 strain for DON production. The solvent system for crude extraction was acetonitrile-water（84：16, v/v）. A simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography（preparative HPLC） to purify the compound. The solvent system for the second silica gel column chromatography was methylene chloride-methanol（17：1, v/v）, which provided a good elution effect selected on thin layer chromatography（TLC）. The target compound was identified by HPLC, and the chemical structure was confirmed by mass spectrometry（MS） and ~1H and ^（13）C nuclear magnetic resonance（NMR） spectroscopy. A total of 433 mg of purified DON was obtained from 1 kg of wheat culture, with a purity of 99.01%. The study had provided an easy-operating and cost-effective method to isolate an expensive compound in a simple way.

Advancement in separation materials for blood purification therapy

Blood purification refers to the extra corporeal therapies of removing potentially toxic substances, in which blood is circulated through an adsorption system loading separation materials. High-efficient inexpensive separation materials are critical to success. In this review, separation materials such as polymers and nanomaterials are summarized and compared. Combining the advantages of the adsorptive membranes and nanomaterials, organic–inorganic hybrid/blend membranes have been developed explosively. These hybrid/blend membranes have both the characteristics of high permeability, easy fabrication, good biocompatibility of adsorptive membranes, and characteristics of fast adsorption rate and high adsorption capacity of nanomaterials. The preparation and modification methodology of the separation materials is reviewed. For affinity separation materials, the relationship of ligand chemistry, ligand density and pores of the matrix is discussed. This paper also summarizes some interesting applications in separation materials for removal of bilirubin, endotoxin, toxic metal ions, cytokine, etc.

Review of Alloy Membranes/Films for Hydrogen Separation or Purification

Hydrogen separation and purification are two important chemical processes in the extensive application of hydrogen energy. Membrane technology has opened up a potential solution to the problems of separation and purification in an energy effective way. Membranes of adequate hydrogen permeability, good thermal and mechanical stability are the key to successful application of membrane technology in hydrogen separation and purification. In this paper, the relative parameters concerning hydrogen permeability, the development of different types of membranes namely: palladium composite membranes; V-based alloy membranes, specific functionality embraced alloy membranes, metal hydride (MH) thin films and fabrications, were reviewed and discussed. Pd-free membranes are found to be the ideal alternatives. Suitable MH thin films with mono- or multi-layer microstructures produced by novel fabrication techniques, is likely to be the promising candidates due to possessing properties distinct from those of bulk materials in membrane form.

Separation and Purification of Total Phloroglucinols in Dryopteris crassirhizoma with DM-130 Macroporous Adsorption Resin

To improve the purity of the total phloroglucinols from Dryopteris crassirhizoma extracts, the separation and purification conditions of the total phloroglucinols from Dryopteris crassirhizoma were studied with DM-130 macroporous adsorption resin in this study. Adsorption rate, elution rate and purity of the total phloroglucinols were used as indexes to investigate the adsorption and desorption capacity of the total phloroglucinols with DM-130 macroporous adsorption resin. Through the study, the optimum sample concentration of the total phloroglucinols and maximum sample volume were 1.5 mg·mL^-1 and 7 BV （210 mL）, respectively. The optimum desorption conditions were achieved by using 80% ethanol as desorption solvent at elution flow rate of 1.0 mL·min^-1. The result showed DM-130 macroporous adsorption resin performed effective adsorption and desorption. After purification, the purity of the total phloroglucinols increased by 11.5-fold.

Separation and Purification of Monascus Pigments from Red Yeast Rice

It is difficult to extract beneficial components from Monascus pigments due to their complex composition. The low purity of Monascus pigment preparations limits their further application in research and production. Therefore, this study was conducted to optimize the conditions for extraction and isolation of Monascus pigments from red yeast rice, to improve the purity of Monascus pigment preparations. Three fractions were isolated using column chromatography from red yeast rice, they were red, orange and yellow respectively. Then, the three fractions were analyzed for composition and purity using thin layer chromatography and liquid chromatography-mass spectrometry(LC-MS). The chromatograms revealed that the yellow and orange fractions had complex compositions that were difficult to be separated, while the red fraction consisted of fewer components. Finally, a single component was isolated from the red fraction using a thin layer chromatography plate, identified as monascorubramine according to its molecular mass.

Separation and Purification of Dodecanedioic Acid from Its Homologous Compounds by Falling Film Crystallization

Separation and purification of dodecanedioic acid (DDDA) from its homologous compounds were studied experimentally by falling film crystallization (FFC). The influences of various operation parameters, including crystallizing time, flow rate of melt and temperature of glycerine bath, on purity of DDDA and crystallizing rate were investigated. Over 99% (by mole) DDDA was obtained for a feed composition of 96% (by mole). The main factors affecting the separation efficiency are flow rate of melt and temperature of glycerine bath. The crystallizing layer of DDDA was further purified by sweating and blasting. A set of optimized operation data are provided for better understanding the mechanism of heat and mass transfer in FFC, and for further industrial application of DDDA purification process.

Design and optimization of an integrated process for the purification of propylene oxide and the separation of propylene glycol by-product

It is difficult to separate the methanol and hydrocarbons in the propylene oxide(PO)purification process due to their forming azeotrope.As for this,a novel PO separation process,in that the deionized water is employed as extractant and 1,2-propylene glycol(MPG)that is formed from the PO hydrolysis reaction is recovered,is presented in this work.The salient feature of this process is that both the non-catalyzed reactions of PO hydrolysis to form MPG and dipropylene glycol(DPG)are simultaneously considered and MPG by-product with high purity is obtained in virtue of the deionized water as reflux liquid and side take-off in MPG column.In addition,the ionic liquid(IL)extractant is screened through the conductorlike screening model for segment activity coefficient(COSMO-SAC)and the comparisons of separation efficiency between the IL and normal octane(nC_(8))extractant for the separation of PO and 2-methylpentane are made.With the non-random two-liquid(NRTL)thermodynamic model,the simulation and optimization design for the full flow sheet are performed and the effects of the key operation parameters such as solvent ratio,theoretical stages,feeding stage etc.on separation efficiency are detailedly discussed.The results show that the mass purity and the mass yield of PO can be up to 99.99%and 99.0%,and the condenser duty,reboiler duty and PO loss in the process with IL extractant can be decreased by 69.66%,30.21%and 78.86%compared to ones with nC_(8).The total annual cost(TAC)calculation also suggests that the TAC would be significantly reduced if using IL in replace of nC_(8) for the investigated process.The presented results would provide a useful guide for improving the quality of PO product and the economic efficiency of industrial plant.

Two-dimensional material separation membranes for renewable energy purification, storage, and conversion

The current energy crisis has prompted the development of new energy sources and energy storage/conversion devices. Membranes, as the key component, not only provide enormous separation potential for energy purification but also guarantee stable and high-efficiency operation for rechargeable batteries and fuel cells. Remarkably, two-dimensional(2D) material separation membranes have attracted intense attention on their excellent performance in energy field applications, owing to high mechanical/chemical stability, low mass transport resistance, strict sizeexclusion, and abundant modifiable functional groups. In this review, we concentrate on the recent progress of 2D membrane and introduce 2D membranes based on graphene oxide(GO), MXenes, 2D MOFs, 2D COFs, and 2D zeolite nanosheets, which are applied in membrane separation(H2 collection and biofuel purification) and battery separators(vanadium flow battery, Li–S battery, and fuel cell). The mass transport mechanism, selectivity mechanism, and modification methods of these 2D membranes are stated in brief, mainly focusing on interlayer dominant membranes(GO and MXenes) and pore dominant membranes(MOFs, COFs, and zeolite nanosheets). In conclusion, we highlight the challenges and outlooks of applying 2D membranes in energy fields.

Separation and Purification of Thrombin-like Enzymes by Affinity Adsorbents

An affinity adsorbent, benzamidine Sepharose 4B, was used to separate and purify thrombin like enzymes. The p aminobenzamidine as a specific ligand was coupled to the matrix-Sepharose 4B. The recombinant thrombin like enzyme-defibrase was used as a model in order to evaluate the efficiency of this biospecific affinity adsorbent. The homogeneity of the enzyme preparation was comfirmed as one band on sodium dodecyl sulfate polyacrylamide gel electrophoresis.

Optimization of Preparative Separation and Purification of Total Polyphenols from Sargassum tenerrimum by Column Chromatography

Polyphenols from the ethanol extracts of Sargassum tenerrimum （ST） with potent antiallergic effects were studied to optimize separation process through column chromatography. The adsorption and desorption characteristics of three widely used adsorbents： macroporous resin, silica gel, and polyvinylpolypyrrolidone （PVPP）, were critically evaluated respectively and studied for the optimization of preparative separation of polyphenols. Static operations on these adsorbents showed that macroporous resin had the best adsorption and desorption capability among the three adsorbents. Dynamic adsorption and desorption with macroporous resin packed column were also conducted to optimize the parameters such as： with the optimal values shown in brackets, the concen- tration of extract solution （4 times diluted）, pH value （6-7）, adsorption speed （3BVh-1, bed volumes/per hour）, concentration of ethanol （80%）, elution speed （3 BV ht） and elution volume （7 BV）. The chromatographic process so optimized gave a purity of 62.43% from the crude polyphenols, providing a promising basis for large scale preparation of bioactive polyphenols upon further scaling up tests.

KAOLIN CLAY PURIFICATION BY DRY HIGH GRADIENT MAGNETIC SEPARATION

A new method-dry High Gradient Magnetic Separation （HGMS）-to remove iron from ultrafine kaolin powder is described. A new kind of disperser, which breaks down the particle clusters in the powder by high speed gas flow from an air compressor, is used to completely disperse the powders. The dispersed particles are passed through vibrating HGMS by a vacuum pump to remove the iron. The magnetic and nonmagnetic fractions are separately collected by cloth collectors. Dry HGMS laboratory experiments are carried out. A product containing 0.90％ Fe2O3 was obtained, and the recovery was 70％.

Advances in Researches of Extraction, Separation, and Purification Technologies for Total Saponins of Panax notoginseng

Total saponins of Panax notoginseng have the functions of promoting blood circulation and removing phlegm, thus they have high medicinal value. There are many different extraction methods in the extraction and separation of total saponins of P. notoginseng . The extraction methods of total saponins of P. notoginseng are mainly divided into traditional extraction methods, modern extraction methods and compound extraction methods.

Separation and purification of proteinases from Gastric Mucosa of Northern Sheatfish,Silurus soldatovi

The separation and purification method for pepsin of Northern Sheatfish (Silurus soldatovi) was established by using the combination technology of salting-out,gel chromatography and gel electrophoresis,and the enzymic properties were also analyzed.The experimental results indicated that 28% and 56% (NH4)2SO4 saturation could separate the activated protease from the pepsin extract of gastric mucosa of Sheatfish (Silurus soldatovi) ;compared with the homogenate extraction,the pepsin specific activity of purified extraction by Sephadex G-75 gel chromatography system increased 598 fold,was 5 times higher than that of activated liquid,and the total production rate was 10.1%.The purified pepsin liquor at the conditions of pH3.3 0.01 M alanine-formic acid buffering solution,60 cm chromatography column,and the flowing rate of 0.8 ML/min was analyzed by SDS-PAGE,which indicated that there were two bands and the molecular weight was 34.0 kDa and 40.4 kDa,respectively.There were two peaks in the enzyme activity determination of the separated collecting liquor in gel chromatography,and the SDS-PAGE showed the concentrations of the two proteins was different,which indicated that it existed at least two pepsins in the gastric mucosa of Sheatfish (Silurus soldatovi).

Separation and Purification of Tobacco Peroxidase I from Nicotiana Tobaccum

A new isoenzyme of tobacco peroxidase(TOP) I was purified from tobacco (K326) by using acetone powder, ammonium sulfate precipitation and column chromatography on DEAE-52 cellulose, Sephadex G-75 and DEAE-Sephadex A-50. It is an iron-protein containing haemachrome, whose molecular weight is 21888.5 and the isoelectric point is 3.5. The optimum pH value and temperature of this enzyme is 6.0 and 45℃respectively. The enzyme is stable in the pH range from 3.0 to 10.0 and has a favorable thermostability.