Synthesis and application of nanocomposite Fe3O4@SiO2@CTAB–SiO2 as a novel adsorbent for removal of cyclophosphamide from water samples

ABSTRACT

We present a way of synthesizing nanocomposite Fe₃O₄@SiO₂@CTAB–SiO₂ by employing simple sol–gel technique with selective etching for extreme selectivity adsorption of cyclophosphamide (CP). The transmission electron microscopy (TEM); scanning electron microscopy (SEM); X-ray diffraction (XRD); Fourier transform infrared (FT-IR); vibrating sample magnetometer (VSM); pH_PZC; and Brunauer, Emmett and Teller (BET) techniques were used for nanocomposite characterization. These nanoparticles have an S_BET of 157.8 m² g^?1 and a high saturation magnetization of 67.5 emu g^?1. First, the adsorption system was examined as a function of contact time under various initial CP contents, ionic strength, initial solution pH, adsorbent dose and temperature in batch test. The optimum dose, pH and contact time were obtained to be 0.01 g, 7.0 and 30 min, respectively. Ultimately, experimental isotherm and kinetics data of adsorption of CP onto nanocomposite Fe₃O₄@SiO₂@CTAB–SiO₂ were fitted to classical models. Additionally, it was found that the maximum adsorption process capacity of CP on adsorbent was 342.8 mg g^?1.     

Adsorption of Textile Dye on Zinc Stannate Oxide: Equilibrium,Kinetic and Thermodynamics Studies

Zn₂SnO₄ powder was prepared by hydrothermal process at 200°C for 12 h. The material was characterized by X-ray-diffraction and surface area. The synthesized sample presented a pure phase and a surface area of 48.8 m² · g^?1. It was used as adsorbent to remove the Reactive Red 141 that is a azo textile dye. The adsorption kinetics of the textile dye on Zn₂SnO₄ followed the pseudo-second-order model. The adsorption process was found to be controlled by both external mass transfer and intraparticle diffusion. The equilibrium data were in good agreement with both Langmuir and Freundlich isotherms. Thermodynamic parameters were calculated, and the results revealed that the adsorption process is endothermic in nature, with weak forces of the Van der Walls acting.     

Adsorptive removal of cationic dye from aqueous solutions by ZnO/ZnMn2O4 nanocomposite

The ZnO/ZnMn₂O₄ nanocomposite (ZnMn) was used as adsorbent for the removal of cationic dye Basic Yellow 28 (BY28) from aqueous solutions. The adsorbent was characterized by X-ray diffraction, scanning electron microscope, TEM, Fourier transform infrared ray, BET, particle size distribution and zeta potential measurements. The adsorption parameters, such as temperature, pH and initial dye concentration, were studied. Kinetic adsorption data were analyzed using the pseudo-first-order, pseudo-second-order and intraparticle diffusion kinetic models. The Langmuir and Freundlich isotherm models were applied to fit the equilibrium data. The maximum adsorption capacity of BY28 was 48.8 mg g^?1. Various thermodynamic parameters, such as ΔG°, ΔH° and ΔS°, were calculated.     

Hydrothermal preparation of Zn2SnO4 nanocrystals and photocatalytic degradation of a leather dye

Zinc stannate (Zn₂SnO₄) powder was prepared by a hydrothermal process at 200 °C for 12 h. The material was characterized by X-ray-diffraction (XRD) and N₂ adsorption–desorption isotherms. The synthesized sample presented a pure phase, an average nanocrystal size of about 19 nm, a surface area (BET) of about 41.8 m² g^?1 and total pore volume of about 0.19 cm³ g^?1. Its photocatalytic activity was tested by the degradation of the leather azo-dye, Direct Black 38, in aqueous solution under UV irradiation. Adsorption kinetic data showed that the pseudo-second-order model was the most appropriate for the dye studied. Adsorption onto the Zn₂SnO₄ surface followed the Langmuir isotherm. The catalyst showed highly photocatalytic activity towards degradation of the dye, almost equal to that of the TiO₂-P25 Degussa photocatalyst. The results indicate that Zn₂SnO₄ could be employed for the removal of dyes from wastewaters.     

Cerium dioxide nanoparticles decorated on CuFe2O4 nanofibers as an effective adsorbent for removal of estrogenic contaminants (bisphenol A and 17-α ethinylestradiol) from water

CeO₂/CuFe₂O₄ nanofibers with high adsorption selectivity for bisphenol A (BPA) and 17-α ethinylestradiol (EE2) were synthesized by support of CeO₂ on the CuFe₂O₄ nanofibers. The characteristics of nanocomposite were investigated via using XRD analysis, FT-IR, SEM, pH_pzc, and Brunauer, Emmett, and Teller methods. The results showed that the maximum adsorption capacities of adsorbent for BPA and EE2 were 226.9 and 179 mg g^?1, respectively. Moreover, the regeneration experiments illustrated that synthesized adsorbent could be recovered, and it showed good recycling ability after being used for six cycles. The isotherm analysis indicated that the equilibrium data could be represented by the Langmuir–Freundlich model. The thermodynamic study showed that the adsorption processes were spontaneous and endothermic under studied conditions.     

SO2 abatement over nanocrystalline MgAl2O4 spinel-supported catalysts

Thermally stable magnesium-rich MgAl₂O₄ spinel with mesoporous nanostructures and high surface area has been prepared by co-precipitation and post hydrothermal treatment, using glucose as organic template. Physical and chemical properties were characterized by XRD, N₂ sorption, TG, FTIR, SEM, and TEM. The synthesized MgAl₂O₄ showed a surface area of 324 m² g^?1 and centralized mesopore distribution (ca. 3.3 nm pore width) after calcination at 700 °C for 3 h. The prepared MgAl₂O₄ were impregnated with metal oxides as sulfur transfer catalysts for high-temperature SO₂ adsorption reaction. The results showed that ferric doped MgAl₂O₄ had the highest SO₂ pick-up capacity up to 58 % and best regeneration up to 81 %. These results showed that thermally stable nanostructured MgAl₂O₄ are a promising candidate as catalyst for desulfurization in fluid catalytic cracking process.     

ADSORPTION OF A LEATHER DYE ON MESOPOROUS STRUVITE OBTAINED FROM SWINE WASTEWATER

Struvite powder obtained from swine wastewater was used as adsorbent to remove an azo leather dye from aqueous solution. The material was characterized by X-ray diffraction, surface area, and atomic force microscopy. The sample presented a single phase having a mesoporous structure and surface area of 35.63 m² g^?1. Langmuir and Freundlich isotherm models were fitted to the adsorption data and both satisfactorily represented the process. The maximum adsorption capacity was 38.14 mg g^?1. From the analysis of thermodynamic parameters such as free energy of adsorption (ΔG°), enthalpy (ΔH°), and entropy (ΔS°) it was verified that the adsorption process is very fast, spontaneous, and exothermic in nature, with weak forces acting.     

Microwave assisted hydrothermal synthesis of MnO2·0.5H2O ion-sieve for lithium ion selective adsorption

Li_1.6Mn_1.6O₄ (LMO) synthesized by microwave assisted hydrothermal method were used to obtain MnO₂·0.5H₂O ion sieves (HMO) after acid treatment. The HMO-1 prepared with a Li/Mn molar ratio of 4, at 100ºC for 1 h under microwave irradiation, exhibits an effective Li⁺ adsorption capacity of 5.6 mmol·g^?1 and a high selectivity to Li⁺ with an equilibrium distribution coefficient of 12366.44 mL·g^?1. Moreover, it shows almost saturated ion-exchange capacity (> 95%) for Li⁺ extracted/inserted process. Thus HMO ion-sieves with high adsorption capacity and selectivity to Li⁺ are expected to be a promising application for Li⁺ selective adsorption from brine, seawater, and aqueous lithium generated in industries.     

Waterborne polyurethane-silanized CoFe2O4-acrylate magnetic pressure-sensitive adhesive

A novel waterborne polyurethane-silanized CoFe₂O-acrylate magnetic pressure-sensitive adhesive was prepared. With the increase of PU content, gel content, swelling capability, and SAFT increased, and fracture energy increased first, then decreased. The T-peeling strength increased from 8.93 to 19.07 N · m^?1, tack force increased from No.3 to No.10, while shear resistance increased from 35 to 72 h, and then they decreased. Two empirical models: W_A = 90.46 + 125.04[PU]-319.96[PU]² and T = 9.09 + 96.07[PU]-235.11[PU]², were obtained. With the increase of CoFe₂O₄ content, the saturation magnetization increased from 5.5 to 14.2 emu · g^?1, and remanence increased from 1.7 to 3.7 emu · g^?1, while coercivity decreased from 875 to 763 Oe.     

Adsorption of Cu(II) from Aqueous Solution by Porous Mn3[Co(CN)6]2 · nH2O Nanospheres

Prussian blue analogue of porous Mn₃[Co(CN)₆]₂ · nH₂O nanospheres with a large surface area were prepared by simple mixing K₃[Co(CN)₆]₂ and manganous nitrate solution at room temperature. The morphology and structure of the prepared products were characterized by XRD, FE-SEM, TEM, and BET. The results indicated that the product was composed of nanospheres with the diameter of ～250 nm, which was of porous structure with the pore diameter in the 2.5–4 nm range. The adsorption behavior of Cu(II) ions from aqueous solution onto porous nanospheres was investigated as a function of parameters, such as the equilibrium time, the pH, the initial concentration, and the temperature. A maximum adsorption capacity of 140.85 mg g^?1 of Cu(II) was achieved. Due to the simple synthetic method and its high adsorption capacity, the porous nanospheres had the potential to be utilized as an effective adsorbent for Cu(II) removal.     

Homogeneous precipitation synthesis and thermoelectric properties of Ca2Co2O5 ceramics

Abstract

Homogeneous precipitation method was applied to synthesise Ca₂Co₂O₅ powders using calcium nitrate, cobalt nitrate and urea as raw materials. Uniform plate-like Ca₂Co₂O₅ powders with an average grain size of 1 μm can be obtained by calcining the precursor for 8 h at 1073 K in the air. The Ca₂Co₂O₅ ceramics were gained after sintering for 4 h at 1083 K using uniaxial pressure moulding and then sintering technique. The thermoelectric properties of ceramic samples were measured from 303 to 973 K, and the result shows that the electrical conductivity, Seebeck coefficient, thermal conductivity and figure of merit of the sample are 2236·85 S m^?1, 175·95 μV K^?1, 1·01 W m^?1 K^?1 and 0·69 at 973 K respectively.     

Highly Efficient Removal of Congo red from Wastewater by Nano-Cao

Nano-CaO with high surface area of 120 m² · g^?1 has been used as adsorbents for Congo red adsorption from wastewater. The maximum adsorption capability of Congo red on nano-CaO reached 357.14 mg · g^?1 in 10 min, while the maximum capability on commercial CaO was only 238.66 mg · g^?1 in 30 min. In comparison with commercial CaO, some published metal oxides for Congo red adsorption such as Fe₂O₃, NiO, MgO, and Mn₂O₃, etc., the Nano-CaO exhibited much more favorable adsorptive property. In addition, the effects of pH, salt concentration, and temperature were also investigated, and these factors played significant roles for Congo red adsorption on Nano-CaO.     

Activated carbon from cherry stones by chemical activation: Influence of the impregnation method on porous structure

Cherry stones are utilized as a precursor for the preparation of activated carbons by chemical activation with phosphoric acid (H₃PO₄). The activation process typically consists of successive impregnation, carbonization, and washing stages. Here, several impregnation variables are comprehensively studied, including H₃PO₄ concentration, number of soaking steps, H₃PO₄ recycling, washing of the impregnated material, and previous semi-carbonization. The choice of a suitable impregnation methodology opens up additional possibilities for the preparation of a wide variety of activated carbons with high yields and tailored porous structures. Microporous activated carbons with specific surface areas of ～800 m² g^?1 are produced, in which > 60% of the total pore volume is due to micropores. High surface areas of ～1500 m² g^?1 can be also developed, with micropore volumes being a 26% of the total pore volume. Interestingly, using the same amount of H₃PO₄, either carbons with surface areas of 791 and 337 m² g^?1 or only one carbon with a surface area of 640 m² g^?1 can be prepared. The pore volumes range very widely between 0.07–0.55, 0.01–0.90, and 0.09–0.79 cm³ g^?1 for micropores, mesopores, and macropores, respectively.     

PREPARATION AND THERMAL EXPANSION OF FE2-xYxW3O12 POWDER BY CITRATE SOL-GEL PROCESS

Fe_2-xY_xW₃O₁₂ powder has been synthesized by the citrate sol-gel process. A model was proposed to calculate the concentration of species in a citric solution. The calculated results could provide valuable information for determining the optimal molar ratio of cation to citric acid and pH value of solution for Fe_2-xY_xW₃O₁₂ preparation. The predicted parameters derived from this model are in good agreement with the experimental results. The prepared gel and the Fe_2-xY_xW₃O₁₂ powder were characterized by X-ray diffraction (XRD) and differential thermal analysis-thermogravimetry (DTA-TG). The results show that it is very difficult to obtain pure Fe₂W₃O₁₂ powder by the citrate sol-gel process in the temperature range 500°–1000°C, however, Y₂W₃O₁₂ can easily be prepared even at 500°C. Y₂W₃O₁₂ annealed at 1000°C for 10 h is favorable for absorbing moisture in air to form Y₂W₃O₁₂·3.3H₂O. The thermal expansion coefficients of Y₂W₃O₁₂·3.3H₂O are: α_a = ? 8.01 × 10^?6°C^?1, α_b = ? 2.51 × 10^?7°C^?1, and α_c = ? 5.55 × 10^?6°C^?1 in 473–1173 K.     

Efficiency and Mechanism of Ciprofloxacin Hydrochloride Degradation in Wastewater by Fe3o4/Na2S2O8

ABSTRACT

The nanosized Fe₃O₄ catalyst was synthesized via a modified reverse coprecipitation method and characterized by means of a scanning electron microscope (SEM) and an X-ray diffraction (XRD) analysis instrument. The degradation efficiency and reaction rate of Fe₃O₄ in activating sodium persulfate used to degrade ciprofloxacin were determined from the catalyst dosage, oxidant concentration, and initial pH. The results showed that under the optimum conditions of a catalyst dosage of 2.0 g·L^?1, a sodium persulfate concentration of 1.0 g·L^?1, and an initial pH of 7, the degradation rate of ciprofloxacin was 93.73%, the removal rate of total organic carbon was 78%, and the first-order reaction constant was 0.06907 min^?1 within 40 min. It was also demonstrated that the reactive oxygen species in the Fe₃O₄/sodium persulfate catalytic system were mainly composed of SO₄^– and supplemented by OH· and HO₂· using probe compounds such as ethanol, tertiary butanol, and benzoquinone.     

Microwave-assisted green synthesis of hybrid nanocomposite: removal of Malachite green from waste water

Gum xanthan/psyllium-based nanocomposite was prepared by microwave-assisted synthetic method for the removal of toxic Malachite green (MG) dye from aqueous solutions. The nanocomposite was prepared by in situ incorporation of the K₂Zn₃[Fe(CN)₆]·9H₂O nanoparticles into the semi-IPN matrix in the presence of ammonium persulphate and glutaraldehyde as initiator-crosslinker system. Liquid uptake efficacy of the hybrid superabsorbent was enhanced through the optimization of different reaction conditions, including APS = 0.027 mol L^?1; glutaraldehyde = 0.053 × 10^?3 mol L^?1; solvent = 8.0 mL; acrylic acid = 10.928 mol L^?1; pH 7.0; reaction time = 60 s and microwave power = 100 % and its thermal behavior was evaluated using TGA-DTG-DTA technique. Candidate nanocomposite was characterized by FTIR, SEM, XRD and UV–visible spectroscopic methods. Various optimized parameters for the efficient removal (83 %) of the Malachite green were adsorbent dose of 800 mg, 14 mg L^?1 initial dye concentration and contact time of 28 h. Further, Langmuir and Freundlich adsorption isotherms showed good applicability in adsorption process of MG onto the nanocomposite with maximum adsorption efficiency of 3.21 mg g^?1. However, for Freundlich isotherm, R ² was around 0.9947 and value of 1/n was less than 1 for the synthesized nanocomposite which indicated that the Freundlich isotherm was more favorable than Langmuir isotherm model along with its usability for wide range of dye concentrations. The nanocomposite was found to be a potential product for dye removal from waste water and could prove to be a boon for textile sector.     

Modeling of Adsorptive Filtration of a Leather Dye in a Fixed Bed Column

Abstract

Activated carbons offer an efficient option for the removal of organic and inorganic contaminants from water. However, due to its high costs and difficulty in the regeneration, other low cost adsorbents have been used. In this work, the adsorption capacity of an adsorbent carbon with high iron oxides concentration was compared with that of a commercial activated carbon in the removal of a leather dye from an aqueous solution. The adsorbents were characterized using SEM/EDAX analysis and BET surface area. The capacity of adsorption of the adsorbents was evaluated through the static method at 25°C. The results showed that the color removal was due to the adsorption and precipitation of the dye on the surface of the solids. The adsorption equilibrium was described according to the linear model for the adsorbent carbon and the equilibrium constant was 0.02 L g^?1. The equilibrium of adsorption on activated carbon exhibited a behavior typical of the Langmuir isotherm and the monolayer coverage was 24.33 mg g^?1. A mathematical model was proposed to describe the dynamics of the color removal using a fixed bed considering that the color removal is due to the adsorption and the precipitation of the dye on the adsorbent.     

CO2 adsorption performance of polyethyleneimine-modified ion-exchange resin

A series of solid amine adsorbents were prepared by the template method with ion-exchange resin (D001) as the carrier and polyethyleneimine (PEI) as the modifier. The absorbents were characterized by energy disperse spectroscopy (EDS), scanning electron microscope (SEM), N₂ adsorption–desorption, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA) techniques. The effects of PEI loading, adsorption temperature and influent velocities on CO₂ adsorption capacity in a fixed-bed reactor were investigated. The results show that the solid amine adsorbent prepared by the template method had a better PEI dispersion, stability and CO₂ adsorption capacity. The maximum CO₂ adsorption capacity was 3.98 mmol·g^?1 when PEI loading was 30%, the adsorption temperature was 65°C and the influent velocity was 40 mL·min^?1. The CO₂ adsorption capacity decreased only by 9.50% after 10 cycles of adsorption–desorption tests. The study of kinetics indicates that both chemical adsorption and physical adsorption occurred in the CO₂ adsorption process. The CO₂ adsorption process included fast breakthrough adsorption and gradually approaching equilibrium stage. The particle internal diffusion process was the control step for CO₂ adsorption.     

Soft-templating pathway to create nanostructured Mg–Al spinel as high-temperature absorbent for SO2

Interest in reducing SO₂ emission from the fluid catalytic cracking (FCC) crude oil has been encouraging the development of new materials to achieve such goal. The nanostructured Mg–Al spinel (MgAl₂O₄) was prepared by co-precipitation and post hydrothermal treatment in the presence of glucose and followed by elimination of the organic components by calcination at 700 °C for 3 h. Physical and chemical properties were characterized by XRD, N₂ sorption, TG, FTIR, SEM, and TEM methods. Mesoporous nanostructured MgAl₂O₄ with a high surface area of 324 m² g^?1 were obtained. The organic components contributed to the development of mesoporosity, functioning as a soft template. SO₂ adsorption tests showed that the nanostructured MgAl₂O₄ had a 51.58 % increase of SO₂ sorption capacity than MgAl₂O₄ prepared without glucose. These results showed that the nanostructured MgAl₂O₄ is a promising candidate as catalyst for flue gas desulfurization in FCC process. Three kinetic models were also applied to analyze the SO₂ adsorption kinetics; the pseudo-second order kinetic model fit well with a correlation coefficient (R²) of 0.991 for nanostructured MgAl₂O₄.     

Adsorption of different dyes from aqueous solution using Si-MCM-41 having very high surface area

Adsorption characteristics of four different dyes Safranin O (cationic), Neutral Red (neutral), Congo Red (anionic) and Reactive Red 2 (anionic) on Si-MCM-41 material having very high surface area are reported. The surface morphology of Si-MCM-41 material before and after adsorbing dye molecules are characterised by FTIR, HRXRD, nitrogen adsorption–desorption isotherms, FESEM, and HRTEM. The adsorption capacities of Si-MCM-41 for the dyes followed a decreasing order of NR > SF > CR > RR2. The adsorption kinetics, isotherm and thermodynamic parameters are investigated in detail for these dyes using calcined Si-MCM-41. The kinetics and isotherm data showed that both SF and NR adsorb more rapidly than CR and RR2, in accordance with pseudo-second-order kinetics model as well as intraparticle diffusion kinetics model and Langmuir adsorption isotherm model respectively. The thermodynamic data suggest that the dye uptake process is spontaneous. The high adsorption capacities of dyes on Si-MCM-41 (q_m = 275.5 mg g^?1 for SF, q_m = 288.2 mg g^?1 for NR) is explained on the basis of electrostatic interactions as well as H-bonding interactions between adsorbent and adsorbate molecules. Good regeneration capacity is another important aspect of the material that makes it potent for the uptake of dyes from aqueous solution.