scholarly journals Synthesis of Zn-Saponite Using a Microwave Circulating Reflux Method under Atmospheric Pressure

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.

2021 ◽  
Vol 7 (5) ◽  
pp. 2010-2018
Author(s):  
Olukayode Gideon Oloyede ◽  
◽  
Umar Omeiza Aroke ◽  
Saidat Olanipekun Giwa ◽  
Alexander Asanja Jock ◽  
...  

In this study, Dijah-Monkin bentonite clay was modified with a cationic surfactant hexadecyltrimethylammonium bromide (HDTMA-Br) at the level of twice the cation exchange capacity (CEC). This process results in the development of hydrophobic organoclay with an improved adsorption capacity. The clay obtained from Zing LGA Taraba State, North-East Nigeria, was beneficiated and pulverised to a particle size of 125 µm. The modification was performed without acid activation to prevent damages to the clay’s crystal structure. The organoclay was characterised for chemical composition, functional groups, mineralogical and surface morphology using X-ray fluorescence (XRF), Fourier Transform Infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The XRD showed an increase in the basal spacing from 15.681Å to 17.758 Å, while the XRF revealed a 5.35% concentration of Br on the modified clay, indicating successful intercalation. The FTIR spectra also revealed the appearance of symmetric and asymmetric stretching bands at 2847.7cm-1 and 2914.8cm-1, respectively, as a consequence of the modification, resulting in more sites for adsorption.


Clay Minerals ◽  
2014 ◽  
Vol 49 (5) ◽  
pp. 683-692 ◽  
Author(s):  
F. Kooli

AbstractOrgano-bentonites were prepared using a bentonite and an aqueous cetyltrimethylammonium hydroxide solution. The ratio of the surfactant (in mmoles) to the cation exchange capacity varied from 0.5 to 20, with 20 being the highest ratio ever reported in the literature. At high surfactant to cation exchange capacity ratios, the interlayer spacing increased to 3.75 nm due to the formation of a paraffin-type bilayer of surfactant cations, which was shown to be mainly in gauche conformations using solid state 13C CP/NMR. When the exchange reaction was carried out in a methanol-water mixture, the expansion of the organo-bentonites depended on the concentration of methanol (% by volume). The decomposition temperatures of the organic cations depended on the basal spacing of the organo-bentonites, and in situ X-ray diffraction revealed that the basal spacing of our organo-bentonites was stable up to 210°C. Above this temperature, the basal spacing shrunk to 1.47 nm due to decomposition of the surfactants.


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.


Clay Minerals ◽  
2016 ◽  
Vol 51 (1) ◽  
pp. 39-54 ◽  
Author(s):  
Manoella Silva Cavalcante ◽  
Simone Patrícia Aranha Paz ◽  
Rômulo Simões Angélica ◽  
Edson Noryuki Ito ◽  
Roberto Freitas Neves

AbstractThe use of Mg-montmorillonite in the production of organoclay without sodium activation was investigated. For this purpose, organophilization experiments were carried out by varying the concentration of two surfactants: hexadecyltrimethylammonium (HDTMA+) and dodecyltrimethylammonium (DTMA+) ions. These surfactantswere used at concentrations 0.7, 1.0 and 1.5 times that of the cation exchange capacity (62.6 meq/100 g) of the clay, with a reaction time of 8 h at temperatures of 25 and 80°C. X-ray diffraction (XRD) results confirmed the intercalation for bothin naturaand activated samples. The Fourier-transforminfrared (FTIR) spectroscopy and XRD results showed that the ratio ofgauche/transconformers decreased with increased basal spacing. The results of thermodifferential and thermogravimetric analysis (DTA/DTG) confirmed the thermal stability of the organoclay up to 200°C, permitting the use of suchmaterial in the synthesis of polymer/clay nanocomposites obtained by the melt blending. Thus, Mg-montmorillonite can be intercalated with alkylammonium ions without prior Na-activation to form organoclays. The possibility of using natural (non-activated) Mg-montmorillonite represents a significant difference in terms of processing cost in comparison with existing Ca-montmorillonite in Brazil or even with imported bentonites that require Na-activation during beneficiation.


1990 ◽  
Vol 5 (6) ◽  
pp. 1169-1175 ◽  
Author(s):  
A. D. Berry ◽  
R. T. Holm ◽  
M. Fatemi ◽  
D. K. Gaskill

Films containing the metals copper, yttrium, calcium, strontium, barium, and bismuth were grown by organometallic chemical vapor deposition (OMCVD). Depositions were carried out at atmospheric pressure in an oxygen-rich environment using metal beta-diketonates and triphenylbismuth. The films were characterized by Auger electron spectroscopy, Nomarski and scanning electron microscopy, and x-ray diffraction. The results show that films containing yttrium consisted of Y2O3 with a small amount of carbidic carbon, those with copper and bismuth were mixtures of oxides with no detectable carbon, and those with calcium, strontium, and barium contained carbonates. Use of a partially fluorinated barium beta-diketonate gave films of BaF2 with small amounts of BaCO3.


2013 ◽  
Vol 772 ◽  
pp. 193-199 ◽  
Author(s):  
Carsten Ohms ◽  
Rene V. Martins

Bi-metallic piping welds are frequently used in light water nuclear reactors to connect ferritic steel pressure vessel nozzles to austenitic stainless steel primary cooling piping systems. An important aspect for the integrity of such welds is the presence of residual stresses. Measurement of these residual stresses presents a considerable challenge because of the component size and because of the material heterogeneity in the weld regions. The specimen investigated here was a thin slice cut from a full-scale bi-metallic piping weld mock-up. A similar mock-up had previously been investigated by neutron diffraction within a European research project called ADIMEW. However, at that time, due to the wall thickness of the pipe, stress and spatial resolution of the measurements were severely restricted. One aim of the present investigations by high energy synchrotron radiation and neutrons used on this thin slice was to determine whether such measurements would render a valid representation of the axial strains and stresses in the uncut large-scale structure. The advantage of the small specimen was, apart from the easier manipulation, the fact that measurement times facilitated a high density of measurements across large parts of the test piece in a reasonable time. Furthermore, the recording of complete diffraction patterns within the accessible diffraction angle range by synchrotron X-ray diffraction permitted mapping the texture variations. The strain and stress results obtained are presented and compared for the neutron and synchrotron X-ray diffraction measurements. A strong variation of the texture pole orientations is observed in the weld regions which could be attributed to individual weld torch passes. The effect of specimen rocking on the scatter of the diffraction data in the butt weld region is assessed during the neutron diffraction measurements.


2007 ◽  
Vol 1040 ◽  
Author(s):  
Hiroaki Yokoo ◽  
Naoki Wakiya ◽  
Naonori Sakamoto ◽  
Takato Nakamura ◽  
Hisao Suzuki

AbstractWe have grown indium nitride (InN) films using In buffer layer on an a-plane sapphire substrate under atmospheric pressure by halide CVD (AP-HCVD). Growth was carried out by two steps: deposition In buffer layer at 900 °C and subsequent growth of InN layer at 650 °C. In order to compare, we also grown InN films on an a-plane sapphire. The InN films are investigated on crystal quality, surface morphology and electrical property using high-resolution X-ray diffraction (HR-XRD), X-ray pole figure, scanning electron microscope (SEM), Hall measurement. The results show that the crystal quality, surface morphology and electrical property of InN films are improved by using In buffer layer.


1991 ◽  
Vol 243 ◽  
Author(s):  
A. Greenwald ◽  
M. Horenstein ◽  
M. Ruane ◽  
W. Clouser ◽  
J. Foresi

AbstractSpire Corporation has deposited strontium-barium-niobate by chemical vapor deposition at atmospheric pressure using Ba(TMHD), Sr(TMHD), and Nb ethoxide. Deposition temperature as 550°C in an isothermal furnace. Films were deposited upon silicon (precoated with silica), platinum, sapphire, and quartz. Materials were characterized by RBS, X-ray diffraction, EDS, electron, and optical microscopy. Electrical and optical properties were measured at Boston University.


1971 ◽  
Vol 178 (1051) ◽  
pp. 131-149 ◽  

A previous occasion on which the Croonian lecture was directly concerned with the mechanism of muscular contraction was in 1945, when it was delivered by Professor W. T. Astbury. On that occasion he commented that it was a sign of the times that a physicist should be asked to give the Croonian lecture, and went on to say, and I quote: ‘We are at the dawn of a new era, the era of “molecular biology”, as I like to call it, and there is an urgency about the need for more intensive application of physics and chemistry, and specially structural analysis, to biological problems.’ These were very prophetic words, and, as a physicist just entering biology, I was much interested to read them, and to learn about his experiments. The basic experimental finding which Astbury reported (1947) was that there did not seem to be any important change in the wide angle X-ray diagram from muscle upon contraction; hence it followed that muscles did not contract by any process which simply involved the large-scale disorientation of originally well-ordered polypeptide chains, nor by an alteration in chain configuration in the well-ordered parts of the structure. Astbury suggested instead that there might be ‘specifically active foci’ which one could perhaps paraphrase as ‘larger structural units’ (i.e. larger than individual polypeptide chains) concerned in contraction, which might be studied in the electron microscope or by low angle X-ray diffraction.


2012 ◽  
Vol 14 (1) ◽  
pp. 7
Author(s):  
Syaiful Bahri ◽  
Muhdarina Muhdarina ◽  
Nurhayati Nurhayati ◽  
Fitri Andiyani

Pillared Cengar clay have been synthesized by two methods, first clay suspension is directly mixed into aqueous solution of hydroxy-aluminum polycations (WK) and second by mixing the clay suspension into the solution of sodium acetate and hydroxy-aluminumpolycations (SAK) sequentially. Both clays were calcined in air on atmospheric condition. Diffraction pola, surface morphology and cationexchange capacity of the pillared clays were characterized using X Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) andvisible spectrophotometry methods, respectively. The pillared clays showed increases of basal spacing from 3.57 Å to 4.55 Å and smectiteas a new mineral. Morphology of SAK has more heterogeneous surface with small plates and agglomeration of grains compare with WKwhich small plates. Adsorption of aqueous cation of Cu 2+ were studied on various variables of initial concentration as well as temperatures.As the result, adsorption of cation Cu 2+ on pillared Cengar clay is corresponding to Freundlich isotherm, while the adsorption capacity ofWK on cation Cu 2+ is slightly lower than SAK. The thermodynamic aspect, the WK is reflected possessed exothermic processes withnegative entropy, increased in Gibbs energy and non spontaneous, while the SAK possessed endothermic processes having positive entropy,decreased in Gibbs energy and non spontaneous.


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