A Thermal Study of Al-Pillared Montmorillonites

2011 ◽  
Vol 187 ◽  
pp. 112-116 ◽  
Author(s):  
Hong Yan Xu ◽  
Xing Tong Chen

Al-pillared montmorillonites (Al-MMT) were synthesized from naturally occurring sodium montmorillonite through exchange of interlamellar ions with hydroxyalumina polycations. Furthermore, Powder X-ray diffraction (XRD), Fourier transformation infra-red spectra (FTIR), Thermogravimetric analysis (TG), and differential scanning calorimetry (DSC) were applied in order to study the themal stability, hydrothermal stability and synthesis mechanisms of pillared materials. The Al-MMT are thermally stable and hydrothermal stability up to700°C. X-ray diffractograms of Al-MMT calcined at 700 0C show a sharp and intense d001 peak, corresponding to a basal spacing of 1.66nm. Until calcinations at 8000C, the pillared clays generally retain their structural ordering as evidenced by a broad basal (001) peak, which is an indication that the layer structure lost some long-range ordering. In a 100% steam flow under atmospheric pressure at 7000C, the characteristic d001 spacing of Al-MMT decreases from 1.83nm to 1.71nm, intensity of basal peak reduced by58%. However, after hydrothermal at 8000C, the basal (001) peak is not observed, indicating a complete structural collapse. Synthesis mechanisms for Al-MMT are established. Some of tetrahedral silicons or aluminums inverse towards gallery to react with pillaring agents and yield Alp-O-AlsⅣ or Alp-O-Sis bridges which would firmly fix the pillars to the host clay.

2010 ◽  
Vol 178 ◽  
pp. 314-317 ◽  
Author(s):  
Hong Yan Xu ◽  
Xing Tong Chen ◽  
Ai Hong Guo

Al-pillared rectorites (Al-REC) were synthesized from naturally occurring rectorite through exchange of interlamellar ions with hydroxyalumina polycations. Furthermore, Powder X-ray diffraction (XRD), Nitrogen adsorption-desorption isotherms, and Transmitting electronic microscopy (TEM) were applied in order to study the themal stability and hydrothermal stability of pillared materials. The Al-REC are thermally stable up to 800 °C. X-ray diffractograms of Al-REC calcined at 800 °C show a sharp and intense d001 peak, corresponding to a basal spacing of 2.75nm. In a 100% steam flow under atmospheric pressure at 800 °C for 20h, the characteristic d001 spacing of Al-REC decreases from 2.74 to 2.52nm, the sharp and intense d001 peak is still observed. And micropore area, mesopore volume and micropore volume retain 62, 33 and 67%, respectively, which affirms that this pillared clay has exceptional hydrothermal stability.


2012 ◽  
Vol 557-559 ◽  
pp. 1629-1632
Author(s):  
Xing Shun Cong ◽  
Min Li

A set of pillared montmorillonite (PILM) catalysts were prepared by exchanging Na+ with iron pillars, chromium pillars, complexes pillars of iron and chromium with different proportion, as well as complexes pillar of silica sol and iron and chromium, respectively. X-ray diffraction (XRD), X-ray fluorescence (XRF), thermogravimetry (TG) and differential thermal analysis (DTA) were used to characterize the catalysts. The XRD results reveal that Fe-Cr complexes pillared montmorillonites (Fe/Cr-PILM) have the basal spacing of about 2.04 nm after calcination at 300 °C for 2 h, while sole metal PILM have that of about 1.0 nm; in particular, the basal spacing of silica sol complexes pillared montmorillonite (Fe-Cr-Si-PILM) are expanded up to 4.33 nm. The TG-DTA results show that both Fe-Cr-PILM and Fe-Cr-Si-PILM have high thermal stability up to 640 °C. Catalytic activity of Fe/Cr-Si-PILM in Longkou lignite (LL) and ShengLi coal residue (SCR) liquefaction was studied, which showed that PILM had a good catalytic performance in coal conversion field.


Minerals ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 45 ◽  
Author(s):  
Bing-Sheng Yu ◽  
Wei-Hsiang Hung ◽  
Jiann-Neng Fang ◽  
Yu-Ting Yu

Smectite is a common clay mineral in nature. Due to its tendency to swell and its strong cation exchange capacity (CEC), smectite is prevalently used in industrial and technological applications. Numerous scholars have explored smectite synthesis, which usually involves autoclaving under high pressure. However, this approach requires an array of expensive equipment, and the process consumes time and energy. This study adopted self-developed equipment to synthesize zinc saponite (Zn-saponite), a type of trioctahedral smectite, using a microwave circulating reflux method under atmospheric pressure. Compared with the conventional hydrothermal methods, the proposed method entails fewer constraints regarding the synthesis environment and can be more easily applied to large-scale synthesis. The phase purity of the synthetic product was examined using X-ray diffraction and the CEC of the product was tested. The results revealed that the microwave circulating reflux method could synthesize Zn-saponite in 16 h under atmospheric pressure, and the CEC of the product reached 120 cmol(+)/kg. In addition, the product exhibited larger basal spacing and a 32% increase in CEC compared with Zn-saponite synthesized using a hot-plate under atmospheric pressure.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.


Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


Processes ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 1238
Author(s):  
Garven M. Huntley ◽  
Rudy L. Luck ◽  
Michael E. Mullins ◽  
Nick K. Newberry

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.


2015 ◽  
Vol 51 (2) ◽  
pp. 255-263
Author(s):  
Rupali Nanasaheb Kadam ◽  
Raosaheb Sopanrao Shendge ◽  
Vishal Vijay Pande

<p>The use of nanotechnology based on the development and fabrication of nanostructures is one approach that has been employed to overcome the challenges involved with conventional drug delivery systems. Formulating Nanoplex is the new trend in nanotechnology. A nanoplex is a complex formed by a drug nanoparticle with an oppositely charged polyelectrolyte. Both cationic and anionic drugs form complexes with oppositely charged polyelectrolytes. Compared with other nanostructures, the yield of Nanoplex is greater and the complexation efficiency is better. Nanoplex are also easier to prepare. Nanoplex formulation is characterized through the production yield, complexation efficiency, drug loading, particle size and zeta potential using scanning electron microscopy, differential scanning calorimetry, X-ray diffraction and dialysis studies. Nanoplex have wide-ranging applications in different fields such as cancer therapy, gene drug delivery, drug delivery to the brain and protein and peptide drug delivery.</p>


Biomolecules ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 220
Author(s):  
Alessio Ausili ◽  
Inés Rodríguez-González ◽  
Alejandro Torrecillas ◽  
José A. Teruel ◽  
Juan C. Gómez-Fernández

The synthetic estrogen diethylstilbestrol (DES) is used to treat metastatic carcinomas and prostate cancer. We studied its interaction with membranes and its localization to understand its mechanism of action and side-effects. We used differential scanning calorimetry (DSC) showing that DES fluidized the membrane and has poor solubility in DMPC (1,2-dimyristoyl-sn-glycero-3-phosphocholine) in the fluid state. Using small-angle X-ray diffraction (SAXD), it was observed that DES increased the thickness of the water layer between phospholipid membranes, indicating effects on the membrane surface. DSC, X-ray diffraction, and 31P-NMR spectroscopy were used to study the effect of DES on the Lα-to-HII phase transition, and it was observed that negative curvature of the membrane is promoted by DES, and this effect may be significant to understand its action on membrane enzymes. Using the 1H-NOESY-NMR-MAS technique, cross-relaxation rates for different protons of DES with POPC (1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine) protons were calculated, suggesting that the most likely location of DES in the membrane is with the main axis parallel to the surface and close to the first carbons of the fatty acyl chains of POPC. Molecular dynamics simulations were in close agreements with the experimental results regarding the location of DES in phospholipids bilayers.


Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.


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