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1.
Chemphyschem ; 25(8): e202300825, 2024 Apr 16.
Artículo en Inglés | MEDLINE | ID: mdl-38296806

RESUMEN

The influence of carbon pore structure on the sorption process of selected cationic dyes has been investigated. The structure and surface of carbonaceous materials have been characterized basing on various techniques: scanning electron microscopy, low temperature nitrogen adsorption-desorption measurements, X-ray photoelectron spectroscopy and thermal analysis combined with identification of gaseous products. The kinetic and equilibrium adsorption measurements of Basic Violet 3, Basic Red 1 and Basic Blue 9 from aqueous media were performed. The studied carbons seem to be promising adsorbents towards dyes, taking into account the easy-to-use uniform spherical form of the granules and a complex type of porosity with micro-, meso- and macropores appropriate for large molecule adsorption.

2.
Chemphyschem ; 25(4): e202300796, 2024 Feb 16.
Artículo en Inglés | MEDLINE | ID: mdl-38100512

RESUMEN

A series of carbon composites were synthesised by carbonisation of resorcinol-formaldehyde resin mixtures with the addition of different amounts of sodium alginate (SA) and compared with a composite prepared using Na2 CO3 as a catalyst for the polymerisation reaction. The effect of operating parameters such as SA concentration and polycondensation time on the structural and morphological properties of resorcinol-formaldehyde resins (RFR) and carbon-derived composites was investigated for further use as adsorbents. The synthesised composites were characterised by FTIR, SEM, Raman spectroscopy and N2 adsorption/desorption techniques. It was found that the morphology, specific surface area (SBET ~347-559 m2 /g), volume and particle size distribution (~0.5-4 µm) and porosity (Vpor =0.178-0.348 cm3 /g) of the composites were influenced by the concentration of SA and the synthesis technique and determined the adsorption properties of the materials. It was found that the surface of the filled chars was found to have an affinity for heavy metals and has the ability to form chemical bonds with cadmium ions. The maximum sorption capacities for Cd(II), i. e. 13.28 mg/g, were observed for the sample synthesised with the highest SA content. This confirms the statement that as-synthesised materials are promising adsorbents for environmental applications.

3.
Phys Chem Chem Phys ; 26(5): 4240-4261, 2024 Jan 31.
Artículo en Inglés | MEDLINE | ID: mdl-38230691

RESUMEN

Entero-vulnerosorbents based on geometrically modified (GM) (mechanical treatment at different times, tMT = 1, 4, and 7 h) fumed nanosilica A300 (NS) and protein molecules (human serum albumin/GM-nanosilica systems) were characterized with a focus on their surface, morphology, topography, and thermal properties. Microscopic, spectroscopic, and analytical techniques, including atomic force microscopy (AFM), optical profilometry (OP), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and elemental analysis (CHN), were used. The differentiation in the surface morphology, micro-nanoroughness, surface chemistry, thermal properties of the silica support, and protein/nanosilica systems were found. AFM, OP, and HRTEM microscopic methods showed that the albumin/silica composite surface is less rough, wavy, and asymmetrical; it is also smoother, flat, and homogeneous because of the formation of a continuous layer of a protein film on the support surface. CHN, XPS, and S/TEM-EDX analysis showed that HSA adsorbed on the unmodified and GM-treated silica carrier led to variations in the physical and chemical features of materials (elemental composition, element concentration, chemical states, chemical bonds between enzyme molecules, and silica surface). Thermal studies were carried out using a thermogravimetric technique linked with a quadrupole mass spectrometer (TG/DTG/DSC-QMS). The degradation of the HSA/nanosilica system is a two-stage process that takes place within the temperature range 160-450-900 °C.


Asunto(s)
Nanoestructuras , Albúmina Sérica Humana , Humanos , Albúmina Sérica Humana/química , Dióxido de Silicio/química , Proteínas
4.
Molecules ; 29(13)2024 Jun 26.
Artículo en Inglés | MEDLINE | ID: mdl-38998985

RESUMEN

This work presents comprehensive studies of the adsorption of neutral and ionic forms of organic adsorbates from aqueous solutions on activated carbon. The influence of pH on the equilibrium and kinetics of the adsorption of methylene blue (MB) and organic acids, benzoic (BA), 2-nitrobenzoic (2-NBA), 3-nitrobenzoic (3-NBA), and 4-nitrobenzoic (4-NBA) acid, was investigated. Experimental adsorption isotherms were analyzed using the generalized Langmuir isotherm equation (R2 = 0.932-0.995). Adsorption rate data were studied using multiple adsorption kinetics equations, of which the multi-exponential equation gave the best fit quality (R2 - 1 = (6.3 × 10-6)-(2.1 × 10-3)). The half-time was also used to represent the effect of pH on adsorption kinetics. Strong dependences of the adsorption efficiency on the solution pH were demonstrated. In the case of organic acid adsorption, the amount and rate of this process increased with a decrease in pH. Moreover, larger adsorbed amounts of methylene blue were recorded in an alkaline environment in a relatively short time. The maximum absorbed amounts were 11.59 mmol/g, 6.57 mmol/g, 9.38 mmol/g, 2.70 mmol/g, and 0.24 mmol/g for BA, 2NBA, 3-NBA, 4-NBA, and MB. The pure activated carbon and the selected samples after adsorption were investigated using thermal analysis and X-ray photoelectron spectroscopy.

5.
Molecules ; 29(9)2024 Apr 28.
Artículo en Inglés | MEDLINE | ID: mdl-38731529

RESUMEN

This work presents a comprehensive analysis of the adsorption of selected aromatic organic compounds on activated carbons. Both the equilibrium and kinetics of adsorption were studied using UV-Vis spectrophotometry. The influence of a number of factors: pH, contact time, presence of an accompanying substance, adsorbate concentration, as well as the mass and size of adsorbent grains, on the adsorption process from aqueous solutions was investigated. Phenol, 2-nitrophenol, 3-nitrophenol, 4-nitrophenol and methylene blue (as an accompanying substance) were selected as adsorbates. GAC 1240W and RIAA activated carbons were used as adsorbents. The equilibrium data were analyzed using the generalized Langmuir isotherm equation (R2 = 0.912-0.996). Adsorption rate data were fitted using a multi-exponential kinetic equation (1 - R2 = (1.0 × 10-6)-(8.2 × 10-4)). As an additional parameter, the half-time was also used to present the influence of selected factors on the adsorption kinetics. An increase in the amount of adsorption was demonstrated with increasing contact time as well as with decreasing solution pH and adsorbent grain size. For selected systems, an increase in the adsorption rate was observed with increasing adsorbate concentration, adsorbent mass and at lower pH values. In some cases, the presence of an accompanying substance also resulted in an increase in adsorption kinetics. In the tested experimental systems, optimal conditions for adsorption were established (T = 298 K, pH = 2, contact time: 7 days, grain diameter: >0.5 mm and the ratio of the mass of the adsorbent to the volume of the adsorbate solution: 1 g/L). Additionally, the acid-base properties (potentiometric titration), morphology (SEM) and structure (TEM) of the used adsorbents were also examined.

6.
Molecules ; 29(9)2024 May 01.
Artículo en Inglés | MEDLINE | ID: mdl-38731578

RESUMEN

In this work, various types of silica materials were used for the synthesis of chitosan-silica composites. The composites were obtained using the chitosan (Ch) immobilization process from an aqueous solution on various silica phases, i.e., amorphous diatomite (ChAD), crystalline diatomite (ChCD), mesoporous silica MCM-41 (ChMCM), and mesoporous silica SBA-15 (ChSBA). Textural, structural, morphological, and surface properties of the materials were determined by using various measurement techniques, i.e., low-temperature adsorption/desorption isotherms of nitrogen, X-ray diffraction (XRD), small-angle X-ray scattering (SAXS), potentiometric titration, high-resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The adsorption properties towards various anionic dyes, i.e., acid red 88 (AR88), acid orange 8 (AO8), and orange G (OG), were evaluated based on kinetic and equilibrium measurements. The ChSBA, ChAD, and ChMCM composites were characterized by relatively high adsorption capacities (am) for AR88, with values equal to 0.78, 0.71, and 0.69 mmol/g, respectively. These composites were also distinguished by the rapid AR88 adsorption rate, with the values of half-time parameter t0.5 equal to 0.35, 2.84, and 1.53 min, respectively. The adsorption equilibrium and kinetic data were analyzed by applying the generalized Langmuir isotherm and the multi-exponential equation (m-exp), respectively. An interaction mechanism between the dyes and the obtained materials was proposed.

7.
Int J Mol Sci ; 24(14)2023 Jul 23.
Artículo en Inglés | MEDLINE | ID: mdl-37511577

RESUMEN

A series of new types of composites (biopolymer-silica materials) are proposed as selective and effective adsorbents. A new procedure for the synthesis of chitosan-nanosilica composites (ChNS) and chitosan-silica gel composites (ChSG) using geometrical modification of silica and mechanosorption of chitosan is applied. The highest adsorption efficiency was achieved at pH = 2, hence the desirability of modifications aimed at stabilizing chitosan in such conditions. The amount of chitosan in the synthesis grew to 1.8 times the adsorption capacity for the nanosilica-supported materials and 1.6 times for the silica gel-based composites. The adsorption kinetics of anionic dyes (acid red AR88) was faster for ChNS than for ChSG, which results from a silica-type effect. The various structural, textural, and physicochemical aspects of the chitosan-silica adsorbents were analyzed via small-angle X-ray scattering, scanning electron microscopy, low-temperature gas (nitrogen) adsorption, and potentiometric titration, as well as their adsorption effectiveness towards selected dyes. This indicates the synergistic effect of the presence of dye-binding groups of the chitosan component, and the developed interfacial surface of the silica component in composites.


Asunto(s)
Quitosano , Contaminantes Químicos del Agua , Dióxido de Silicio/química , Agua , Aguas Residuales , Quitosano/química , Colorantes/química , Adsorción , Gel de Sílice , Contaminantes Químicos del Agua/química , Concentración de Iones de Hidrógeno , Cinética
8.
Molecules ; 28(14)2023 Jul 14.
Artículo en Inglés | MEDLINE | ID: mdl-37513275

RESUMEN

The increasing consumption of phenoxyacetic acid-derived herbicides is becoming a major public health and environmental concern, posing a serious challenge to existing conventional water treatment systems. Among the various physicochemical and biological purification processes, adsorption is considered one of the most efficient and popular techniques due to its high removal efficiency, ease of operation, and cost effectiveness. This review article provides extensive literature information on the adsorption of phenoxyacetic herbicides by various adsorbents. The purpose of this article is to organize the scattered information on the currently used adsorbents for herbicide removal from the water, such as activated carbons, carbon and silica adsorbents, metal oxides, and numerous natural and industrial waste materials known as low-cost adsorbents. The adsorption capacity of these adsorbents was compared for the two most popular phenoxyacetic herbicides, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA). The application of various kinetic models and adsorption isotherms in describing the removal of these herbicides by the adsorbents was also presented and discussed. At the beginning of this review paper, the most important information on phenoxyacetic herbicides has been collected, including their classification, physicochemical properties, and occurrence in the environment.

9.
Molecules ; 28(6)2023 Mar 11.
Artículo en Inglés | MEDLINE | ID: mdl-36985532

RESUMEN

This paper reports the synthesis and structural analysis of mesoporous silica materials with the use of aluminum phyllosilicate clay (bentonite) as an alternative silica source. In the proposed synthesis, bentonite, as natural aluminosilicate, was used instead of commercially available and quite expensive tetraethyl orthosilicate (TEOS) silica source. The objective of the research study was to determine the effect of aluminum loading in the mesoporous silica body for ordering structure, porosity, and potential sorption capacity to thorium ions. The unique direction developed in this procedure is focused on preparing advanced materials from natural sources with their own desired functionality and general availability. The applied procedure based on the classic, one-step synthesis of SBA-15 silicates was modified by gradually increasing the bentonite amount with simultaneous reduction of the TEOS content. The structural and morphological characterization, as well as evaluation of the porous structure of the obtained materials, was performed using powder wide-angle X-ray diffraction (XRD), small-angle scattering (SAXS), transmission and scanning electron microscopy (TEM, SEM), low-temperature nitrogen adsorption-desorption methods and potentiometric titration. The new, cost-effective composites for the removal of Th(IV) ions are proposed. The synergistic effect of expanding the porous surface using bentonite as a silica precursor and the presence of thorium-binding groups (such as Al2O3) is indicated.

10.
Molecules ; 26(8)2021 Apr 20.
Artículo en Inglés | MEDLINE | ID: mdl-33924208

RESUMEN

In this work, organic-inorganic materials with spherical shape consisting of divinylbenzene (DVB) and triethoxyvinylsilane (TEVS) were synthesized and investigated by different complementary techniques. The obtained microspheres may be applied as sorbent systems for the purification of organic compounds from water. The hybrid microspheres combine the properties of the constituents depending on the morphologies and interfacial bonding. In this work, the influence of the molar ratio composition of crosslinked monomer (DVB) and silane coupling agent (TEVS) (DVB:TEVS molar ratios: 1:2, 1:1 and 2:1) on the morphology and quality of organic-inorganic materials have been examined. The materials were analysed using small angle X-ray scattering (SAXS) analysis, low-temperature nitrogen sorption, scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) to provide information on their structural and surface properties. Moreover, thermal analysis was performed to characterize the thermal stability of the studied materials and the adsorbent-adsorbate interactions, while adsorption kinetic studies proved the utility of the synthesized adsorbents for water and wastewater treatment.

11.
Molecules ; 26(8)2021 Apr 09.
Artículo en Inglés | MEDLINE | ID: mdl-33918588

RESUMEN

Mesoporous carbons with differentiated properties were synthesized by using the method of impregnation of mesoporous well-organized silicas. The obtained carbonaceous materials and microporous activated carbon were investigated by applying different methods in order to determine their structural, surface and adsorption properties towards selected dyes from aqueous solutions. In order to verify applicability of adsorbents for removing dyes the equilibrium and kinetic experimental data were measured and analyzed by applying various equations and models. The structural and acid-base properties of the investigated carbons were evaluated by Small-Angle X-ray Scattering (SAXS) technique, adsorption/desorption of nitrogen, potentiometric titration, and Transmission Electron Microscopy (TEM). The results of these techniques are complementary, indicating the type of porosity and structural ordering, e.g., the pore sizes determined from the SAXS data are in good agreement with those obtained from nitrogen sorption data. The SAXS and TEM data confirm the regularity of mesoporous carbon structure. The adsorption experiment, especially kinetic measurements, reveals the utility of mesoporous carbons in dye removing, taking into account not only the adsorption uptake but also the adsorption rate.

12.
Int J Mol Sci ; 21(24)2020 Dec 09.
Artículo en Inglés | MEDLINE | ID: mdl-33317218

RESUMEN

In this work, ultra-small and stable silver nanoparticles (AgNP) on chitosan biopolymer (BP/AgP) were prepared by in situ reduction of the diamminesilver(I) complex ([Ag(NH3)2]+) to create a biostatic membrane system. The small AgNP (3 nm) as a stable source of silver ions, their crystal form, and homogeneous distribution in the whole solid membrane were confirmed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The X-ray photoelectron spectroscopy (XPS) and Auger analysis were applied to investigate the elemental composition, concentration, and chemical state of surface atoms. It was found that ultra-small metallic nanoparticles might form a steady source of silver ions and enhance the biostatic properties of solid membranes. Ultra-small AgNP with disturbed electronic structure and plasmonic properties may generate interaction between amine groups of the biopolymer for improving the homogeneity of the nanometallic layer. In this work, the significant differences between the typical way (deposition of ex-situ-prepared AgNP) and the proposed in-situ synthesis approach were determined. The improved thermal stability (by thermogravimetry and differential scanning calorimetry (TG/DSC) analysis) for BP/AgP was observed and explained by the presence of the protective layer of a low-molecular silver phase. Finally, the antibacterial activity of the BP/AgP nanocomposite was tested using selected bacteria biofilms. The grafted membrane showed clear inhibition properties by destruction and multiple damages of bacteria cells. The possible mechanisms of biocidal activity were discussed, and the investigation of the AgNP influence on the bacteria body was illustrated by AFM measurements. The results obtained concluded that the biopolymer membrane properties were significantly improved by the integration with ultra-small Ag nanoparticles, which added value to its applications as a biostatic membrane system for filtration and separation issues.


Asunto(s)
Quitosano/análogos & derivados , Nanopartículas del Metal/química , Nanocompuestos/química , Plata/química
13.
Int J Mol Sci ; 21(15)2020 Jul 31.
Artículo en Inglés | MEDLINE | ID: mdl-32751874

RESUMEN

The effect of the porous structure of mesocellular silica foams (MCFs) on the lysozyme (LYS) adsorption capacity, as well as the rate, was studied to design the effective sorbent for potential applications as the carriers of biomolecules. The structural (N2 adsorption/desorption isotherms), textural (SEM, TEM), acid-base (potentiometric titration), adsorption properties, and thermal characteristics of the obtained lysozyme/silica composites were studied. The protein adsorption equilibrium and kinetics showed significant dependence on silica pore size. For instance, LYS adsorption uptake on MCF-6.4 support (pore diameter 6.4 nm) was about 0.29 g/g. The equilibrium loading amount of LYS on MCF-14.5 material (pore size 14.5 nm) increased to 0.55 g/g. However, when the pore diameter was larger than 14.5 nm, the LYS adsorption value systematically decreased with increasing pore size (e.g., for MCF-30.1 was only 0.27 g/g). The electrostatic attractive interactions between the positively charged lysozyme (at pH = 7.4) and the negatively charged silica played a significant role in the immobilization process. The differences in protein adsorption and surface morphology for the biocomposites of various pore sizes were found. The thermal behavior of the studied bio/systems was conducted by TG/DSC/FTIR/MS coupled method. It was found that the thermal degradation of lysozyme/silica composites was a double-stage process in the temperature range 165-420-830 °C.


Asunto(s)
Materiales Biocompatibles/química , Enzimas Inmovilizadas/química , Dióxido de Silicio/química , Adsorción , Animales , Pollos , Huevos , Cinética , Muramidasa/química , Porosidad , Propiedades de Superficie
14.
Molecules ; 25(21)2020 Nov 03.
Artículo en Inglés | MEDLINE | ID: mdl-33153177

RESUMEN

Agricultural waste materials (strawberry seeds and pistachio shells) were used for preparation of activated carbons by two various methods. Chemical activation using acetic acid and physical activation with gaseous agents (carbon dioxide and water vapor) were chosen as mild and environmentally friendly methods. The effect of type of raw material, temperature, and activation agent on the porous structure characteristics of the materials was discussed applying various methods of analysis. The best obtained activated carbons were characterized by high values of specific surface area (555-685 m2/g). The Guinier analysis of small-angle X-ray scattering (SAXS) curves showed that a time of activation affects pore size. The samples activated using carbon dioxide were characterized mostly by the spherical morphology of pores. Adsorbents were utilized for removal of the model organic pollutants from the single- and multicomponent systems. The adsorption capacities for the 4-chloro-2-methyphenoxyacetic acid (MCPA) removal were equal to 1.43-1.56 mmol/g; however, for adsorbent from strawberry seeds it was much lower. Slight effect of crystal violet presence on the MCPA adsorption and inversely was noticed as a result of adsorption in different types of pores. For similar herbicides strong competition in capacity and adsorption rate was observed. For analysis of kinetic data various equations were used.


Asunto(s)
Agricultura , Carbón Orgánico/química , Eliminación de Residuos Líquidos , Contaminantes Químicos del Agua/química , Purificación del Agua , Adsorción
15.
Int J Mol Sci ; 21(1)2019 Dec 25.
Artículo en Inglés | MEDLINE | ID: mdl-31881739

RESUMEN

A simple, low-cost, and reproducible method for creating materials with even silver nanoparticles (AgNP) dispersion was established. Chitosan nanofibers with silica phase (CS/silica) were synthesized by an electrospinning technique to obtain highly porous 3D nanofiber scaffolds. Silver nanoparticles in the form of a well-dispersed metallic phase were synthesized in an external preparation step and embedded in the CS/silica nanofibers by deposition for obtaining chitosan nanofibers with silica phase decorated by silver nanoparticles (Ag/CS/silica). The antibacterial activity of investigated materials was tested using Gram-positive and Gram-negative bacteria. The results were compared with the properties of the nanocomposite without silver nanoparticles and a colloidal solution of AgNP. The minimum inhibitory concentration (MIC) of obtained AgNP against Staphylococcus aureus (S. aureus) ATCC25923 and Escherichia coli (E. coli) ATCC25922 was determined. The physicochemical characterization of Ag/CS/silica nanofibers using various analytical techniques, as well as the applicability of these techniques in the characterization of this type of nanocomposite, is presented. The resulting Ag/CS/silica nanocomposites (Ag/CS/silica nanofibers) were characterized by small angle X-ray scattering (SAXS), X-ray diffraction (XRD), and atomic force microscopy (AFM). The morphology of the AgNP in solution, both initial and extracted from composite, the properties of composites, the size, and crystallinity of the nanoparticles, and the characteristics of the chitosan fibers were determined by electron microscopy (SEM and TEM).


Asunto(s)
Antibacterianos/química , Quitosano/química , Nanopartículas del Metal/química , Nanofibras/química , Dióxido de Silicio/química , Plata/química , Antibacterianos/farmacología , Pruebas Antimicrobianas de Difusión por Disco , Bacterias Gramnegativas/efectos de los fármacos , Bacterias Grampositivas/efectos de los fármacos
16.
Langmuir ; 34(6): 2258-2273, 2018 02 13.
Artículo en Inglés | MEDLINE | ID: mdl-29345945

RESUMEN

In this study, the influence of the chitosan immobilization method on the properties of final hybrid materials was performed. Chitosan was immobilized on the surface of mesoporous (ChS2) and fumed silica (ChS3) by physical adsorption and the sol-gel method (ChS1). It was found that physical immobilization of chitosan allows to obtain hybrid composites (ChS) with a homogeneous distribution of polymer on the surface, relatively wide pores, and specific surface area of about 170 m2/g, pHPZC = 5.7 for ChS3 and 356 m2/g and pHPZC = 6.0 for ChS2. The microporous chitosan-silica material with a specific surface area of 600 m2/g and a more negatively charged surface (pHPZC = 4.2) was obtained by the sol-gel reaction. The mechanisms of azo dye adsorption were studied, and the correlation with the composite structure was distinguished. The generalized Langmuir equation and its special cases, that is, Langmuir-Freundlich and Langmuir equations, were applied for the analysis of adsorption isotherm data. The adsorption study showed that physically adsorbed chitosan (ChS1 and ChS2) on a silica surface has a higher sorption capacity, for example, 0.48 mmol/g for the acid red 88 (AR88) dye (ChS2) and 0.23 mmol/g for the acid orange 8 (AO8) dye (ChS1), compared to the composite obtained by the sol-gel method [ChS1, 0.05 mmol/g for the AO8 dye]. For a deeper understanding of the behavior of immobilized chitosan in the adsorption processes, various kinetic equations were applied: first-order, second-order, mixed 1,2-order (MOE), multiexponential, and fractal-like MOE as well as intraparticle and pore diffusion model equations. In the case of AO8 dye, the adsorption rates were differentiated for three composites: for ChS3, 50% of the dye was removed from the solution after merely 5 min and almost 90% after 80 min. The slowest adsorption process controlled by the diffusion rate of dye molecules into the internal space of the pore structure was found for ChS1 (225 min halftime). In the case of ChS2, the rates for various dyes change in the following order: acid orange (AO7) > orange G (OG) > acid red 1 (AR1) > AR88 > AO8 (halftimes: 10.5 < 15.7 < 23.7 < 34.9 < 42.9 min).


Asunto(s)
Compuestos Azo/química , Quitosano/química , Nanocompuestos/química , Dióxido de Silicio/química , Bencenosulfonatos/química
17.
Langmuir ; 33(42): 11203-11216, 2017 10 24.
Artículo en Inglés | MEDLINE | ID: mdl-28851218

RESUMEN

We report an experimental investigation of structural and adhesive properties for Al-containing mesoporous MCM-41 and MCM-41 surfaces. In this work, highly ordered hexagonal mesoporous structures of aluminosilica with two different Si/Al molar ratios equal to 50 and 80 and silica samples were studied; Al was incorporated into the MCM-41 structures using the direct synthesis method, with CTAB as a surfactant. The incorporation of aluminum was evidenced simultaneously without any change in the hexagonal arrangement of cylindrical mesopores. The porous materials were examined by techniques such as low-temperature nitrogen sorption, energy-dispersive spectroscopy, and scanning and transmission electron microscopy. Surface properties were determined through X-ray photoelectron spectroscopy, potentiometric titration, and static contact angle measurements. It was shown that an increase in surface acidity leads to an increase in the wetting energy of the surface. To investigate the influence of acidity on the confinement effects, the melting behavior of water in Al-MCM-41 and MCM-41 with the same pore size was determined by using dielectric relaxation spectroscopy and differential scanning calorimetry methods. We found that the melting-point depression of water in pores is larger in the functionalized pores than in pure silica pores of the same pore diameter.

18.
Materials (Basel) ; 17(17)2024 Aug 27.
Artículo en Inglés | MEDLINE | ID: mdl-39274621

RESUMEN

The aim of this study is to examine the influence of various factors on the precision and repeatability of the experimental determination of herbicide adsorption isotherms. Studies were conducted for the activated carbon RIB as an adsorbent and three herbicides as adsorbates: 2,4-dichlorophenoxyacetic acid (2,4-D), 4-chlorophenoxyacetic acid (4-CPA), and 3-chlorophenoxypropionic acid (3-CPP). The herbicide adsorption process was carried out in single-component and multi-component modes (the herbicide was adsorbed in the presence of an accompanying substance, i.e., 4-nitroaniline (4-NA)). Due to the significant contribution of the competition phenomenon in the adsorption process, which is important, e.g., in multi-component environmental systems, a qualitative and quantitative analysis of herbicide adsorption in the presence of a competing substance was presented. This work presents, among other things, the influence of adsorbent heterogeneity (grain size) on measurement uncertainties. The spread of standard deviations for solutions requiring dilution during spectrophotometric measurements was discussed, indicating that dilutions contribute to increasing measurement uncertainties. The heterogeneity parameters of the Freundlich equation for the studied adsorption systems were analyzed; the 2,4-D/RIB system was indicated as the most energetically heterogeneous. Differentiation of the experimental conditions (pH, temperature) allowed us to assess their impact on the efficiency and mechanism of adsorption. A high repeatability of experimental isotherms was obtained for the multi-component system. The accuracy of quantitative determination of equilibrium concentrations for the tested two-component systems was assessed based on the measured UV-Vis spectra, and the adsorption of herbicides from single- and multi-component systems was compared.

19.
Materials (Basel) ; 17(6)2024 Mar 17.
Artículo en Inglés | MEDLINE | ID: mdl-38541529

RESUMEN

This study presents the results of applying the methods of synthesizing mesoporous carbon and mesoporous polymer materials with an extended porous mesostructure as adsorbents for cationic dye molecules. Both types of adsorbents are synthetic materials. The aim of the presented research was the preparation, characterisation, and utilisation of obtained mesoporous adsorbents. The physicochemical properties, morphology, and porous structure characteristics of the obtained materials were determined using low-temperature nitrogen sorption isotherms, X-ray diffraction (XRD), small angle X-ray scattering (SAXS), and potentiometric titration measurements. The morphology and microstructure were imaged using scanning electron microscopy (SEM). The chemical characterisation of the surface chemistry of the adsorbents, which provides information about the surface-active groups, the elemental composition, and the electronic state of the elements, was carried out using X-ray photoelectron spectroscopy (XPS). The adsorption properties of the mesoporous materials were determined using equilibrium and kinetic adsorption experiments for three selected cationic dyes (derivatives of thiazine (methylene blue) and triarylmethane (malachite green and crystal violet)). The adsorption capacity was analysed to the nanostructural and surface properties of used materials. The Generalized Langmuir equation was applied for the analysis of adsorption isotherm data. The adsorption study showed that the carbon materials have a higher sorption capacity for both methylene blue and crystal violet, e.g., 0.88-1.01 mmol/g and 0.33-0.44 mmol/g, respectively, compared to the polymer materials (e.g., 0.038-0.044 mmol/g and 0.038-0.050 mmol/g, respectively). The kinetics of dyes adsorption was closely correlated with the structural properties of the adsorbents. The kinetic data were analysed using various equations: first-order (FOE), second-order (SOE), mixed 1,2-order (MOE), multi-exponential (m-exp), and fractal-like MOE (f-MOE).

20.
Materials (Basel) ; 17(9)2024 Apr 24.
Artículo en Inglés | MEDLINE | ID: mdl-38730789

RESUMEN

A series of metal- and silica-containing carbon-based nanocomposites were synthesized by pyrolysis of a resorcinol-formaldehyde polymer modified with metal oxide/silica nanocomposites (MxOy/SiO2, where M = Mg, Mn, Ni, Cu and Zn) via the thermal oxidative destruction of metal acetates adsorbed on highly dispersed silica (A380). The concentration of metals was 3.0 mmol/g SiO2. The phase composition and morphological, structural and textural properties of the carbon materials were analyzed by X-ray diffraction, SEM, Raman spectroscopy and low-temperature N2 adsorption. Thermal decomposition under a nitrogen atmosphere and in air was analyzed using TG-FTIR and TG-DTG-DSC techniques to determine the influence of the filler on the decomposition process. The synthesized composites show mesoporous structures with high porosity and narrow pore size distributions. It could be shown that the textural properties and the final composition of the nanocomposites depend on the metal oxide fillers of the precursors. The data obtained show that nickel and copper promote the degree of graphitization and a structural order with the highest porosity and largest specific surface area of the hybrid composites. The good adsorption properties of the obtained materials were shown for the recovery of p-chlorophenol and p-nitrophenol from aqueous solutions.

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