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Navegando por Assunto "Organoargila"

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    Adsorção de fenol e benzeno em montmorilonita modificada com brometo de hexadeciltrimetilamônio
    (2014-12) SANTOS, Sheila Silva dos; LEMOS, Vanda Porpino; VILAÇA, A. L. C.; TAVARES, Laís Conceição; QUEIRÓZ, Leandro Santos
    This study evaluates the intercalation of the smectite dioctahedric state of Acre, Brazil, with the quaternary ammonium salt bromide, hexadecyltrimethylammonium (HDTMA) at concentrations ranging from 1 to 5 times the value of the original clay CEC and its application in the adsorption of phenol and benzene in the liquid phase. The materials were characterized by microanalysis X-ray diffraction, scanning electron microscopy /energy dispersive spectroscopy and infrared spectroscopy. The adsorption processes were carried out in simple systems and measurements of the concentrations of phenol and benzene were performed by spectrophotometry in the ultraviolet region. The results indicated that the intercalation of smectite with HDTMA provided approximately 78.8 expansion (range d001: 1.47 nm to 1.91 nm) and sharp decrease of the interlayer positions of elements such as Na, Ca, Mg and K, together by delamination/exfoliation of the clay original. In adsorption processes of phenol and benzene at HDTMA-arg 5 the following results were obtained: qmax = 4.44 and 35.8 mg.g-1; KL= 0.076 and 0.115 L.g-1; ΔGº = -16.85 and -18.38 kJ.mol-1, respectively. These data indicated that the adsorption of benzene and phenol in liquid phase in the organophilic HDTMA-arg 5 were favorable, spontaneous and physical interactions.
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    Síntese e caracterização de materiais híbridos (PCHs e Organoargilas) com aplicabilidade na adsorção de fenol, benzeno e tolueno
    (Universidade Federal do Pará, 2013-12-18) SANTOS, Sheila Silva dos; LEMOS, Vanda Porpino; http://lattes.cnpq.br/1829861620854008
    This study evaluates the use of smectite from Acre/Brazil as a precursor in the synthesis of Porous Clay heterostructure and organofunctionalization with mercaptopropyltrimethoxysilane (MPTS-Arg) and applicability of these materials as adsorbents for phenol, benzene and toluene in the liquid phase. The synthesis of PCH involves the following steps: preparation of organoclay with hexadecyltrimethylammonium (HDTMA-clay); it increases the basal spacing (d001) of organoclay using the co-surfactant octylamine and concomitant addition of a source of Si, such as tetraethylorthosilicate (TEOS) , washing with HCl in ethanol and drying at 60 º C (PCH-60 A and B); calcination at 500 ° C and 700 ° C (PCH 500 A /B and PCH 700) by removing the surfactant / co-surfactant and subsequent replacement of these organic substances by protons that remain on the walls of galleries SiO pillars to new treatment perhaps held at PCH. The material MPTS-Arg was obtained from the intercalation of the original clay with mercaptopropiltrimetoxisilano stirring for 1 h (MPTS Arg-1) and the original clay pre-treated with HCl 1 mol L-1 and stirred for 2 h (Arg-MPOS 2).The materials (clay original HDTMA-Clay, PCH-60, Arg-PCH-500/700 and MPTS) were characterized by X-ray diffraction (XRD), scanning electron microscopy coupled to X-ray spectroscopy and energy dispersive (SEM / EDS), molecular absorption spectroscopy with Fourier transform IR (FTIR), thermal analysis techniques (DTA_TG) and textural analyzes, such as specific surface area measurements (ASE BET, ASELangmuir), total pore volume (TPV) and average pore diameter (APD). Additional characterization by nuclear magnetic resonance in solid coupled to mass spectrometry (NMR-MAS) was conducted for the PCH-500 A. In the experiments adsorption of phenol, benzene and toluene were used aqueous suspensions containing adsorbents of the separately adsorbates. The equilibrium concentrations of phenol, toluene and benzene were measured by molecular absorption spectroscopy in the ultraviolet region, as accepted method is applied in other adsorption studies. We obtained the following results: identification of smectite clay minerals in natural clay with basal spacing of 1.25 nm; intercalation of HDTMA and MPTS with expansion of d (001) to 1.95 nm (HDTMA-Arg 5) and 2.1 nm (MPTS Clay-1h). After modification was observed by EDS analysis a decrease of the concentrations of elements Na, Si and Al (%) and the increase in interlayer positions concentration C. The 29Si MAS NMR spectrum of the PCH A-500 showed signs of chemical center Q3 Si (OSi)3OH and Q4 Si(OSi)4 indicate that the formation of silica in its structure. The PCHs (60 and 500 A) were classified as mesoporous, with ASE BET between 417-446 m2 g-1 and total pore volume (cm-3 g-1) = 0.367 to 0.369. Increasing calcination temperature of 500 to 700º C PCH (PCH 700) provided decrease in SBET (305 m2 g-1) and average pore diameter (0976 nm). It was found from the evaluation of the measures of pore diameter at 700 PCH that 46 % of the measurements correspond to micropores. The adsorption process obtained values for KL (mg L-1) , KF (mg L-1) and qmax (mg g-1) in the following cases : (i) adsorption of phenol (1.40, 2.26 and 3.80) and toluene (145, 18.7 and 135) in the PCH- 500 , (ii) adsorption of benzene (0.33 , 41.49 and 69.81) in PCH 500 B (iii) in toluene adsorption MPTS-Argila 1h (1.06 , 118.9 and 146) and MPTSArgila 2h (2.1 , 92 and 97) , (iv) adsorption of phenol (0.07, 4.44 and 12.48 ) and benzene (12.11, 4.95 and 35.8) in HDTMA-Arg 5, respectively. The data on the characterization of the materials indicated that the formation of PCH caused a large increase in the concentrations of Si and decrease in the concentrations of Al, Fe and other elements due to delamination - exfoliation of smectite original. It was verified that the materials are most suitable for the adsorption of toluene and benzene to phenol.
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