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EN
Improving the selectivity of photocatalysis of LDH pristine (MgAl-LDH) and LDH composite (MgAl-SiW12O40] and MgAl-[PW12O40]) was synthesized and used for degraded malachite green (MG). The effects of the amount of catalyst, pH value, and reaction times on degradation performance were discussed. MG degraded better composites than LDH pristine. The results indicated that MgAl-LDH was successfully synthesized by showing the peak diffractions at angles 10.39°(003), 20.17°(006), and 34.8°(009). Both kinds of attained MgAl-[SiW12O40] and MgAl-[PW12O40] had the typical structure of LDH that proved by appeared diffraction at 2θ angles 7.73°, 28.6°, 35.6° for MgAl-[PW12O40] and at 2θ angles 8.61°, 24.27°, 34.96° and 66.34° for MgAl-[SiW12O40]. The FTIR result indicates materials used for fifth regeneration, which confirmed the LDH composite structure. The photodegradation activity of MG for pristine MgAl LDH (56.1%), composites MgAl-Pw (84.6%) and MgAl-Si (87.8%), respectively. The successful ability of photodegradation process by the percentage of degradation on material LDH-polyoxometalate composite showed the increasing of photodegradation catalytic and the regeneration ability of LDH pristine.
EN
The synthesis and characterization of layered double hydroxide (LDH) and intercalated polyoxometalate were presented.. The growth of polyoxometalate on Ni/Mg layered double hydroxide for degradation procion red (PR) was reported. The degradation parameters and organic dye removal efficiency of Zn/Mg-LDH and both composite LDH-polyoxometalate were determined by considering factors such as pH of dye solution, catalyst dosage, and time as variables of degradation. X-Ray, FTIR, and SEM spectroscopy confirmed the layered double hydroxide structure. XRD and FTIR analysis confirmed the single-phase of the as-made and polyoxometalate intercalated LDH. SEM images show the formation of aggregates of small various sizes. The catalytic activity of the material was evaluated in the degradation of PR as a model pollutant. The result showed that MgAl-SiW12O40 has a good degradation capacity for PR as compared to MgAl-PW12O40, ZnAl-SiW12O40, and ZnAl-PW12O40. The result shows that the LDH composite presents stability and has good photocatalytic activities toward the reduction of methylene blue. The materials utilized for the fifth regeneration are indicated by the FTIR results, which verified the LDH composite structure. The photodegradation process of procion red for immaculate ZnAl-LDH, MgAl-LDH, ZnAl-[PW12O40], ZnAl-[SiW12O40], MgAl-[PW12O40], MgAl-[SiW12O40] amounted to 68%, 70%, 56%, 79%, 74%, and 80%, respectively. The capacity of LDH-polyoxometalate composite material to successfully photodegrade, as measured by the percentage of degradation, revealed an increase in photodegradation catalysis and the ability of LDH to regenerate.
EN
In this work, hydrochar using to modified nickel aluminum layered double hydroxide (hydrochar@NiAl LDH). The collected data by XRD indicate that 2θ of material at 11.38°, 22.90°, 35.20°, and 61.60°. The FTIR spectrum of hydrochar@NiAl LDH at wavenumber 3448, 1650, 1500–1600, 1348, 1056, and 500–800 cm-1. NiAl LDH and hydrochar have surface areas of 3.288 m2/g and 7.366 m2/g, respectively. The precursors enhance the composite’s surface area by 11.879 m2/g. NiAl LDH, hydrochar, and hydrochar@NiAl LDH have optimal pH values of 3, 6, and 6 respectively. The adsorption process is determined by the kinetic model of pseudo-second order and the model of Freundlich isotherm. NiAl LDH, hydrochar, and hydrochar@NiAl LDH had respective maximum adsorption capacities of 25.445, 21.008, and 25.773 mg/g. The increase in regeneration cycles decreases the percentage of adsorbed.
EN
The preparation of the CaAl/HC composite was carried out with a supporting material in the form of hydrochar from duku skin. The success of the preparation was demonstrated by XRD, FT-IR, and BET analysis. The diffractogram of CaAl/HC showed diffraction peaks at 2θ = 10.16° (003), 18.0° (002), 20.15° (006) and 65.4° (110). The diffraction showed similarity to diffraction in CaAl and hydrochar double layer hydroxyl. The FT-IR spectrum of CaAl/HC also showed similarity to the CaAl/HC double layer hydroxyl at 3448, 1635, and 1381 cm-1. The characteristic spectrum of the hydrochar also appeared in CaAl/HC at 20.15. BET analysis showed an increase in the surface area of CaAl/HC before modification of 11.842 m2/g and increased to 22.635 m2/g of CaAl/HC. The ability of CaAl/HC as an adsorbent is determined through several parameters including selectivity, regeneration, isotherm, and thermodynamics. The results of dye selectivity showed that CaAl/HC was more likely to absorb MR dyes in a mixture of dyes (DG, MO, PR, MR, CR, and DR). The regeneration results showed the ability of CaAl/HC which lasted up to 73.26% in the fifth cycle.
EN
Layered double hydroxide (LDH) can be used as an adsorbent to remove pollutants from aqueous solutions, but it drawbacks where the structure is easily damaged so that it cannot be reused in the adsorption process and has a low adsorption capacity. This can be overcome through the development of layered double hydroxide material composited with chitosan support material. In addition to untilizing waste, chitosan is selected as supporting material in the layered double hydroxide modification process, because it is cheap, has high selectivity, and is biodegradable. In this study, the adsorbent was applied in the process of removing Congo Red (CR). The LDH modification process using chitosan was successfully carried out, as seen from XRD analysis which resembled the base material (Mg-Al) and support (CT), the BET analysis which showed an increase in surface area, as well as from the large adsorption capacity value and the regeneration process which tends to be stable after compositing is done.
EN
The development of studies on layered double hydroxide (LDH) material as a photocatalyst for the degradation of dye pollutants continues to increase. LDH is an anionic clay, which is a natural or synthetic mixed metal hydroxide. Pristine LDH is written as M2+/M3+ LDH, (M is metal ion). This study prepared pristine Mg/Al LDH and Zn/Al LDH composited with metal oxide TiO2 and ZnO, respectively. Composite is denoted by M2+/M3+ -metal oxide. The coprecipitation method used was accompanied by calcination of the composite at a temperature 300 °C that was not high. The prepared composites were morphologically characterized by SEM. The materials that had been used until the fifth cycle of regeneration were characterized by XRD and FTIR which still indicated the presence of LDH-metal oxide composite structure. The materials degraded cationic dyes namely rhodamine-B (RhB) and methylene blue (MB). RhB degraded better than MB by pristine LDH and composites. The percent degradation of RhB for pristine Mg/Al LDH, composites Mg/Al-TiO2 and Mg/Al-ZnO were 53.1%, 59.8%, 62.8%, respectively. The percent RhB degradation for pristine Zn/Al LDH, composites Zn/Al-TiO2 and Zn/Al-ZnO were 51.4%, 58.5%, 58.9%, respectively. The percentage of degradation indicates that the LDH-metal oxide composite has succeeded in increasing the photodegradation catalytic ability and the regeneration ability of LDH pristine.
EN
Layered double hydroxide (LDH) Zn/Al and Cu/Al was synthesized by using the coprecipitation method under base condition at pH 10 following with formation of composites based on biochar (BC) to form Zn/Al-BC and Cu/ Al-BC. The materials were characterized by XRD, FTIR, BET, and thermal analyses. Furthermore, materials was applied as adsorbent of Cr(VI) on aqueous solution. The performance of composites as adsorbent was evaluated by reusability of adsorbent toward Cr(VI) adsorption process. The results showed that Cu/Al-BC and Zn/Al-BC can reuse the re-adsorption process with the adsorption ability of more than 60%. The adsorption capacity of Cu/ Al-BC and Zn/Al-BC was higher than that of starting materials and up to 384.615 mg/g for Cu/Al-BC and 666.667 mg/g for Zn/Al-BC. Both composites showed the potential adsorbents to remove Cr(VI) from aqueous solution.
EN
Mg/Cr layered double hydroxide (LDH) has been successfully synthesized by means of the coprecipitation method followed by the intercalation process using oxalate to form Mg/Cr-oxalate. The materials were characterized using XRD, BET, and FTIR and then applied as an adsorbent of anionic dyes i.e. methyl red (MR) and methyl orange (MO). MR and MO adsorption was studied through variations of adsorption time, concentration, temperature, desorption process, and adsorbent regeneration. The XRD characterization results showed an increase in the interlayer distance from 7.62 Å to 11.35 Å after the intercalation process. The increase of interlayer space of Mg/Cr-oxalate is also equal to the BET data, which shows an increase in surface area from 21.511 m2/g to 49.270 m2/g. The kinetics and isotherm parameters of MR and MO adsorption using Mg/Cr LDH and Mg/Cr-oxalate showed the same results following the PFO kinetics model and Langmuir isotherm model with R2 close to one. Mg/Cr LDH has the adsorption capacity for MR and MO up to 61.728 mg/g 54.645 mg/g, respectively. In turn, the highest adsorption capacity is achieved by Mg/Cr-oxalate for MR adsorption at 81.235 mg/g and MO at 71.429 mg/g. The thermodynamic parameters of MR and MO adsorption using Mg/Cr LDH and Mg/Cr-oxalate indicate that the adsorption process is endothermic and spontaneous.
EN
In this study, NiAl-LDH was modified with hydrochar using the NiAl-Hydrochar composite coprecipitation method. Materials were characterized by XRD and FT-IR analysis. XRD diffractogram and FT-IR spectra show that the NiAl-Hydrochar composite material has the characteristics of the precursors. NiAl- Hydrochar composite materials have a large adsorption capacity to adsorb cationic dyes. The adsorption follows the Langmuir adsorption isotherm model with the maximum capacity (Qmax) of the NiAl-Hydrochar composite material reaching 256.410 mg/g for malachite green and the adsorption process takes place spontaneously and endothermically. The regeneration process of NiAl-Hydrochar composites was more stable and the decrease was not significant (>70%). The selectivity of the dye mixture showed that the adsorbent was more selective for malachite green dye compared to methylene blue and rhodamine-B.
EN
Zn/Cr and Zn/Cr layered double hydroxides (LDHs) intercalated with Keggin ion [α-SiW12O40]4-were successfully synthesized at room temperature and pH value of 10. The synthesized materials were characterized by means of the XRD, BET, and FT-IR analyses and used as an adsorbent iron(II). The adsorption process was investigated by studying pH, the kinetics, and thermodynamic properties of the adsorption process. The results showed the interlayer Zn/Cr LDHs was 7.53 Å and increase to 10.26 Å on Zn/Cr LDHs intercalated with Keggin ion [α-SiW12O40]4-. The BET analysis showed that the pore volume of both materials increased from 0.063 cm3 g-1 to 0.163 cm3 g-1. The pH point zero charge measurement for the Zn/Cr LDHs material was 10 while LDHs Zn/Cr intercalated with Keggin ion [α-SiW12O40]4- was 8. Zn/Cr LDHs intercalated with Keggin ion [α-SiW12O40]4- has higher adsorption capacity than Zn/Cr LDHs without intercalation. Desorption of iron (III) was successfully conducted using HCl as reagent showing the involvement of ion exchange in the adsorption.
EN
Magnesium-aluminum-bismuth layered double hydroxides (Mg3Al1-xBix; LDHs) were prepared using both coprecipitation and sol-gel methods. For the preparation of Mg/Al/Bi LDH by the co-precipitation method, the appropriate amounts of dissolved starting materials (Al(NO3)3·9H2O, Mg(NO3)2·6H2O and Bi(NO3)3·5H2O) were mixed with a solution of NaHCO3:NaOH. In the sol-gel processing, the precursor Mg–Al–Bi–O gels were synthesized using the same starting materials and ethylene glycol as complexing agent. The mixed-metal oxides obtained by subsequent heating of Mg–Al–Bi–O gels at 650 °C were reconstructed to Mg3Al1-xBix LDHs in water at 80 °C. All the synthesized products were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and dielectric measurements.
EN
Layered double hydroxides (LDHs) are a class of layered inorganic materials, containing basic layers of metal hydroxides. Between these layers anions and water molecules are accommodated. Interlayer anion can be replaced by wide range of organic and inorganic anions and this key feature of LDH opens new fields of applications. In this study magnesium and aluminum based LDH was modified with linseed compounds using the regeneration method. Modified LDH samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), high resolution transmission electron microscopy (HR-TEM), scanning electron microscopy (SEM) and field emission scanning electron microscopy (FE-SEM). XRD results indicate that anionic spacer has gone inside the gallery space, which is evident from increased interlayer spacing. FT-IR study suggests the presence of spacer moiety in modified LDH. From FE-SEM study, it was observed that the shape and texture of LDH platelets have changed (they were hexagonal and smooth before modification). Unmodified and modified LDH were applied to prepare polyurethane nanocomposites (PUR/LDH and PUR/LLDH, respectively). Nanocomposite PUR/LLDH was characterized by better mechanical and thermal properties in comparison with PUR/LDH and neat polyurethane.
PL
Warstwowe podwójne wodorotlenki (LDH) są klasą warstwowych materiałów nieorganicznych, składających się z podstawowych warstw wodorotlenków metali i umieszczonej pomiędzy nimi warstwy anionów i cząsteczek wody. Aniony warstwy pośredniej mogą być zastąpione przez szereg anionów organicznych i nieorganicznych, co otwiera nowe pola zastosowań modyfikowanych LDH. W ramach tej pracy LDH magnezu i glinu modyfikowano metodą regeneracji związkami z siemienia lnianego. Próbki zmodyfikowanego LDH (oznaczane LLDH) charakteryzowano metodami dyfrakcji rentgenowskiej (XRD), spektroskopii w podczerwieni z transformacją Fouriera (FT-IR), transmisyjnej mikroskopii elektronowej wysokiej rozdzielczości (HR-TEM), skaningowej mikroskopii elektronowej (SEM) i skaningowej mikroskopii elektronowej z emisją polową (FE-SEM). Wyniki badań próbek LLDH metodą XRD wykazały, że warstwa anionowa umieściła się wewnątrz przestrzeni pomiędzy warstwami kationów, o czym świadczyły zwiększone odstępy międzywarstwowe. Badania FT-IR tych próbek dowiodły obecności ugrupowań charakterystycznych dla wprowadzonych na skutek modyfikacji anionów. Rezultaty badań FE-SEM pokazały że kształt i tekstura płytek LDH zmienia się z heksagonalnych i gładkich przed modyfikacją na bardziej nieregularne. Niemodyfikowany i modyfikowany LDH zastosowano do otrzymania nanokompozytów poliuretanowych (odpowiednio PUR/LDH i PUR/LLDH). Nanokompozyty PUR/LLDH charakteryzowały się lepszymi właściwościami mechanicznymi i termicznymi niż PUR/LDH i czysty poliuretan.
EN
Layered Double Hydroxide (LDH) is a class of inorganic clay materials having layered structure in which anions are accommodated between the positively charged metal hydroxide layers. An increasing interest exists, because this class of materials can be used as catalysts, photo catalysts, catalysts supports, anion exchangers and as nanofillers in polymer composites, etc. LDHs with easily exchangeable interlayer ionic species have tremendous potential as novel fillers for polymers composites. Due to a low interlayer space and hydrophilic nature they hardly disperse in polymer matrices. After suitable modification by anions, LDHs can be successfully dispersed at nanoscale in a wide range of polymers. LDHs as a nanofillers improve the flame retardancy and barrier properties of polymer composites. In the present work Mg/Al based LDH was modified by the regeneration method. Modified LDH samples were characterized by XRD, FTIR, HRTEM, SEM and FESEM. XRD results indicate that anionic moiety was introduced into the gallery space and acts as pillar increasing the gallery height, what is evident by increased interlayer spacing. FTIR studies of modified LDH samples corroborated the presence of anionic moiety. From FESEM study it was observed, that after modification of LDH, platelet morphology is completely different from that, which was recorded for pure LDH with hexagonal structure. This modified LDH is well exfoliated in polyurethane polymer matrix with improved mechanical properties.
PL
Dwuwarstwowe hydroksyzwiązki (LDH) stanowią grupę nieorganicznych materiałów mineralnych, w których aniony umiejscowione są pomiędzy dodatnio naładowanymi warstwami wodorotlenków metali. Zainteresowanie tymi związkami ciągle wzrasta, ponieważ mogą być one stosowane jako katalizatory lub ich nośniki, fotokatalizatory, wymienniki jonowe oraz jako nanonapełniacze w kompozytach polimerowych. LDH, ze względu na łatwość wymiany jonów w warstwie pośredniej, ma ogromny potencjał jako nowy napełniacz kompozytów polimerowych. Jednak ze względu na niewielkie odległości między warstwami i hydrofilową naturę trudno jest zdyspergować je w ośrodku polimerowym. Jest to możliwe dopiero po odpowiedniej modyfikacji i wymianie anionów w warstwie pośredniej. LDH jako nanonapełniacze zwiększają odporność kompozytów polimerowych na palenie i poprawiają ich właściwości barierowe. W niniejszym artykule omówiono wyniki modyfikacji LDH, opartego na związkach magnezu i glinu, z wykorzystaniem metody regeneracji. Zmodyfikowane hydroksyzwiązki scharakteryzowano wykorzystując analizę XRD, FTIR, HRTEM, SEM i FESEM. Wyniki dyfrakcji rentgenowskiej (XRD) wskazują, że nastąpiła wymiana anionowych fragmentów struktury, a nowo wprowadzone ugrupowania rozpychają warstwy metaliczne, o czym dowodnie świadczy zwiększenie przestrzeni międzywarstwowej. Analiza widm FTIR potwierdziła obecność nowych ugrupowań. Na podstawie badań FESEM stwierdzono, że po modyfikacji całkowicie zmieniła się morfologia LDH. Modyfikowane hydroksyzwiązki były dobrze eksfoliowane w matrycy poliuretanowej, co skutkowało poprawą właściwości mechanicznych kompozytów.
EN
For an environmental-friendly sustainable society, the global environmental problems should be solved. Here we outline our recent results of environment purification materials with smart functions. For the effective adsorbent for remediation process, zeolite coated with layered double hydroxide (LDH) was prepared by the precipitation of LDH on zeolite-LTA under hydrothermal treatment. This multifunctional material has a possible application for simultaneous uptake of harmful cations and anions, and minimizes environmental pollution during municipal and industrial water management. For novel material for the nuclear waste management, zeolite with hydroxyapatite layers on its surface was obtained by a hydrothermal method on the basis of the cation exchange of Ca2+ in zeolite for NH4+ in solution. The novel nanocomposite is an ideal material for adsorbing and fixing radioactive elements for geological time-scale.
EN
Aseries of Cu,Cr-layered double hydroxides of Cu/Cr ratio equal 2 has been synthesized by co-precipitation at a constant pH, using different preparative conditions. The investigated synthesis parameters included: ageing time, speed of reactants addition, temperature of co-precipitation and pH of synthesis. The dominant product of the synthesis was the nitrate form of Cu,Cr-LDH, containing ca. 10 mol% of carbonate. Modifications of experimental conditions affected chiefly the samples crystallinity. The most obvious effects were associated with changing of pH of the co-precipitation, the most acidic conditions providing a material of the best crystallinity. At the medium synthesis temperature (55°C), a slow addition of the reactants and a long ageing were favourable, but a significant shortening of the ageing time caused only minor deterioration of the sample crystallinity. The latter finding is of practical importance for an upscaling of the process.
EN
A layered organic-inorganic intercalate was prepared by the self-assembly technique using pamoate (PA) as an organic guest in the Zn-Al layered double hydroxide inorganic host (ZAPAN). Various concentrations of PA, ranging from 0.01 to 0.04 M, were used to prepare the intercalated compound with a constant 4:1 ratio of Zn:Al in the mother liquor. The concentration of PA of 0.02 M at pH 7 was found to give a well-ordered nanolayered organic-inorganic hybrid structure. As a result of successful intercalation of PA anion into the Zn-Al inorganic layered double hydroxide (LDH), the expansion of interlayer spacing to 18 A was observed in the PXRD diffractogram of the intercalated compound, compared to 9 A for the Zn-Al LDH with nitrate as the counter anion (ZANIL). FTIR study shows that the intercalated compound resembled the spectra of PA and ZANIL, thus indicating the presence of both functional groups in ZAPAN. It was also found that the BET surface area increased from 6 m2/g to 90 m2/g for ZANIL and ZAPAN, respectively. The pore texture of the resulting materials was also changed as the result of the intercalation and the expansion of the basal spacing together with pore formation between the crystallite during the formation of the resulting layered intercalated compound.
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