Batch cation-exchange experiments were performed on chlorite, using synthetic ground water containing cesium in the concentration range 10−9–10−3 M. The sorption behavior was complex; with increasing Cs concentration, the distribution ratio of Cs decreased at first, but passed through a pronounced maximum at high Cs loadings. The desorption data differed from the sorption data only by a shift towards larger distribution ratios in the region of the maximum. The distribution ratios for isotope exchange were even larger, but varied less with Cs loadings. Similar results were obtained for KCl-treated chlorite; however, grinding or acid-treatment of the chlorite considerably altered its behavior, the absence of the maximum being the most striking change. Most of the effects at higher Cs loadings can be explained by postulating structural changes induced by the sorption of Cs.

Biocompatible drug-delivery materials are important because they provide controlled release of biologically active agents to enhance the effectiveness of medical treatments. Montmorillonite (Mnt) has been utilized in drug-delivery systems for delayed-release application because it can safely encapsulate drug molecules via intercalation reactions. The objective of the present study was to evaluate the delivery characteristics of the drug ciprofloxacin (CIP) from a composite with Mnt (Mnt-CIP) in which the Mnt was first prepared by acid treatment and vibration ball milling. The surfaces of Mnt were modified by reacting the Mnt suspension in 1.0 M HCl acid and by dispersing the powder with a vibration ball mill, then the CIP drug was added at pH 4 and stirred. The goal was to improve the sustained-release performance of the CIP. This Mnt-CIP drug-release system was characterized by X-ray diffraction, X-ray fluorescence analysis, Fourier-transform infrared spectroscopy, surface area measurement using the Brunauer-Emmett-Teller (BET) method, and ultraviolet spectroscopy. The X-ray diffraction results confirmed the intercalation of CIP into the interlayer space of Mnt. The in vitro release properties of the intercalated CIP were investigated using a simulated phosphate-buffered saline solution (pH 7.4) at 36±0.5°C. The CIP drug exhibited a continued release for 3 h. Moreover, Mnt prepared by HCl acid treatment and dispersion in the vibration ball mill delayed the drug dissolution rate. In summary, the Mnt-CIP composite prepared in this study exhibited slow and sustained release characteristics, indicating that Mnt mined from the Gampo-40 mining area in Gyeongju can be used in various drug-delivery applications.

Bentonite from the ‘Bogovina’ coal mine in Serbia, was characterized. The influence of acid treatment on its composition, as well as mathematical descriptions of this influence are reported. The purpose of this work was to correlate the concentration of the acid used for the treatment with the resulting bentonite composition. X-ray diffraction (XRD), infrared spectroscopy and quantitative chemical analysis were employed to define the changes caused by acid treatment.

The contents of all the cations, except Si, decreased exponentially with increasing concentration of the HCl used for the treatment of the bentonite. This approach was tested on previously published data and was shown to be valid.

The basal reflections of smectite decreased gradually and eventually disappeared after intense treatment, while the other reflections remained in the XRD patterns of all the samples, but decreased slightly with increasing acid strength. In addition, the amount of X-ray amorphous matter formed increased rapidly with increasing acid concentration up to 4.5 M. With further increase in the acid strength, the amount of X-ray amorphous matter remained virtually constant.

Bentonite is used as a catalyst in the removal of olefins from aromatic compounds and the present study was designed to investigate how its performance might be improved by various treatments. Bentonite from Semnan mine, Iran, was used in the study following initial characterization. In order to investigate the effect of acid and thermal treatments on the removal of olefins from aromatic compounds, bentonite samples were modified using HNO3 at different concentrations (0.15, 0.3, 0.5, 0.7, 1, and 2 M) and were also at temperatures between 100 and 340°C for 3 h. To examine the catalytic activity of bentonite-based catalysts, the samples were evaluated after running batch and continuous experiments. The optimum catalyst was characterized using thermo-programmed desorption (TPD) of NH3 to examine the acidic sites. Scanning Electron Microscopy (SEM) images, nitrogen adsorption-desorption isotherms (BET analysis), and X-ray diffraction (XRD) patterns were used to study the structural changes of the bentonite produced by the acid and thermal activation. The removal of olefins by the catalysts in batch and continuous systems revealed that the sample modified with 0.3 M Nitric acid at 150°C had superior catalytic activity, with olefin conversion remaining at >50% for up to 20 h. Nitrogen adsorption-desorption isotherms showed that acid treatment can produce a mesoporous structure. On the other hand, the TPD analysis indicated that during weak acid treatment, some cations, such as Al3+ and Fe3+, were leached from octahedral sheets and the interlayers of the clay mineral resulting in weak acid sites being generated. Finally, a novel method was proposed and tested for measuring the Bromine Index (BI) using potentiometric titration.

The potential use of near-infrared (NIR) spectroscopy as a characterization tool for organo-clays would be a great asset but little work has been done in this regard because the application of NIR to clay mineral studies is a relatively new phenomenon. The purpose of this study was to use NIR spectroscopy to investigate the effect of alkylammonium cations on the acid dissolution of a high-charge montmorillonite (SAz-1). Detailed analysis of the spectra of Li+-, TMA+- (tetramethylammonium), and HDTMA+- (hexadecyltrimethylammonium) saturated SAz-1 montmorillonite in the NIR region was achieved by comparing the first overtone (2ν) and combination (ν+δ) bands of XH groups (X = O, C) with the fundamental stretching (ν) and bending (δ) vibrations observed in the mid-infrared (MIR) region. Comprehensive analysis of the vibrational modes of CH3-N, CH3-C, and -CH2-C groups of TMA+ and HDTMA+ cations detected in the MIR and NIR regions was also performed. Both MIR and NIR spectra demonstrated that exchange of Li+ by TMA+ only slightly improved the resistance of SAz-1 layers to dissolution in 6 M HCl at 80°C, while exchange by the larger HDTMA+ cations almost completely protected the montmorillonite layers from acid attack. Use of NIR spectra in reaching these conclusions was crucial. Only in the NIR region could the creation of SiOH groups be monitored, which is an important indicator of the acidification of the montmorillonite surface. The OH-overtone region in the spectra of Li-SAz-1 and TMA-SAz-1 revealed that the SiOH band near 7315 cm−1 increases in intensity with enhanced acid treatment. In contrast, no SiOH groups were identified in the NIR spectra of HDTMA-SAz-1 treated in HCl, indicating that HDTMA+ completely covers the inner and outer surfaces of the montmorillonite and hinders access ofprotons to the Si-O− bonds created upon acid treatment.

Modified kaolinites possess excellent adsorption properties and, therefore, are regarded widely as potential catalytic components. The use of modified kaolinites as a catalytic component for Fischer–Tropsch synthesis (FTS) has remained unexplored, however. In the current study, delaminated and pit-rich nano-kaolinite was prepared via acid treatment of N-methylformamide (NMF)-intercalated kaolinite (intercalation-etching strategy), and was used as a support to prepare a cobalt-based FTS catalyst (denoted as 15%-Co-HNKln). Compared with other FTS catalysts, the supports for which were raw kaolinite or directly acid-treated kaolinite, the 15%-Co-HNKln showed several advantages such as large specific surface area, dispersed Co particles with small particle size, more new active sites, and significant surface acidity. Given the aforementioned advantages, the 15%-Co-HNKln catalyst demonstrated very good FTS performance. Compared with that of the raw kaolinite-supported FTS catalyst, the CO conversion rate and C5–C12 hydrocarbon selectivity of 15%-Co-HNKln increased by 20% and 15%, respectively.

Various approaches have been used for the preparation of heterostructured materials based on clay minerals, with numerous potential applications offered by the resulting functional materials. In this study, a fibrous clay mineral (palygorskite) and a tetraethyl orthosilicate reagent were used to obtain silica–palygorskite heterostructures. The aim was to highlight the influence of two factors during the preparation process: the effect of acid activation pre-treatment of the palygorskite with HCl and the effect of varying the length of the amine chains used – dodecylamine and butylamine – on the formation and development of silica nanoparticles on the surface of the palygorskite fibres. The silica–palygorskite heterostructures were obtained after the removal of the organic templates by calcination at 500°C. The textural and structural properties of the silica–palygorskite heterostructured samples were determined using various experimental characterization techniques, such as X-ray diffraction, transmission electron microscopy, gas adsorption and Fourier-transform infrared spectroscopy. The experimental variables targeted in this study appeared to have a significant effect on the textural properties of the silica–palygorskite heterostructure obtained. The great specific surface area and the mesoporous, microporous and ultramicroporous volumes as determined using nitrogen and/or carbon dioxide gas adsorption confirm the benefit of combining the acid activation pre-treatment of the fibrous clay mineral with the use of a long-chain amine co-surfactant (dodecylamine). The resulting silica–palygorskite heterostucture has a great specific surface area (628 m2 g–1) and a well-developed total pore network (VN2 = 0.24 cm3 g–1; Vultra (CO2) = 0.18 cm3 g–1). This material will be tested for the removal of volatile organic compounds at low concentrations.

Acid-activated clays are inexpensive materials that are used extensively in the removal of unsaturated compounds on an industrial scale. The performance of bentonitic clays in removing these compounds relies heavily on the types of raw clays and acids used in the activation process. In this work, we report on the removal of olefins from aromatic streams by bentonitic clays activated via two different routes. After preliminary tests of four different natural clays, the best clay was selected in terms of it having high swelling index, cation-exchange capacity, specific surface area and suspension stability values. Activation was achieved with hydrochloric acid (HCl) and sulfuric acid (H2SO4), and olefin removal was evaluated after holistic clay characterization by means of X-ray diffraction, X-ray fluorescence, Brunauer–Emmett–Teller (BET) specific surface area analysis, ζ-potential analysis, Fourier-transform infrared (FTIR) spectroscopy after treatment with pyridine, scanning electron microscopy and transmission electron microscopy. The increased basal spacing, replacement of H+ with interlayer cations and retained structural stability of the clay after acid treatment contributed to the improvement of olefin removal for HCl-activated clay. The HCl-activated clay was more efficient in terms of olefin removal than its H2SO4-activated counterpart, removing up to 90% of olefin components after 40 h. Based on pyridine-FTIR spectra and quantitative measurement of the acidic properties of the samples, HCl treatment increased the total number acid sites (Brønsted and Lewis) by approximately ninefold compared to the pristine natural clay and by approximately fourfold compared to the H2SO4-activated clay.

An effective method that combines solvent extraction with ultrasonic irradiation was developed to recycle spent bleaching clay (SBC) from modern oil refinery plants. The principle of ‘waste to treasure’ was used to achieve the regenerated SBC. Various characterization techniques were applied to analyse and compare regenerated SBC and commercial bleaching clay (CBC). The structure of the regenerated SBC did not show any obvious change compared with that of CBC, but the Brunauer–Emmett–Teller-specific surface area (SBET) and pore-volume values of the regenerated SBC increased. At the same time, the parameters of the regenerated SBC reached national standards. In addition, the samples were used as low-cost adsorbents for the adsorption of methylene blue (MB) from water. The regenerated SBC had greater adsorption efficiency and cycle performance for MB than CBC. Hence, the SBC may be treated by ultrasonic radiation combined with extraction, and the regenerated SBC has better properties than CBC. This work opens up a new approach to the regeneration and utilization of SBC and raises the potential of ultrasonic irradiation as an environmentally friendly method to be applied to various regeneration systems.

An ab initio determination of the structure of sepiolite after acid treatment (HCl 0.5 N for 24 h) was carried out using X-ray powder diffraction data. After acid treatment, the sections normal to the a and c axes presented discontinuities, ∼2.25 Å wide, parallel to the (010) plane, with no electronic density maxima, thus suggesting that adjacent planes are joined by van der Waals-like residual links. Partial dissolution was detected on both octahedral and tetrahedral sheets, beginning by breaking the ribbons not along the edges, but in the centre, thus creating a 5.20 x 66.79 Å tunnel along the a axis. By interrupting the tetrahedral sheet, this mechanism changes the phyllosilicate-like nature of the sepiolite to an inosilicate-like structure.