PREPARATION and CHARACTERIZATION of CELLULOSE/HYDROUS NIOBIUM PHOSPHATE HYBRID

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Quantitative microscopy characterization of hydrous niobium phosphate into bleached cellulose

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Sugarcane bagasse cellulose fibres and their hydrous niobium phosphate composites: synthesis and characterization by XPS, XRD and SEM

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Preparation and characterization of cellulose/hydrous niobium oxide hybrid

A composite of cellulose extracted from bagasse with Nb2O5 center dot nH(2)O in three different proportions (16.67, 37.5 and 50.0 wt%) was prepared using the co-precipitation method. The materials were characterized by X-ray diffractometry (XRD), Fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TG/DTG), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). TG data obtained show that the presence of inorganic material influenced slightly the stability of the hybrid material. The precipitation of 16.67 wt.% of oxide was sufficient to inhibit the combustion peaks present in the DSC curve of cellulose. This work will help find new applications for these materials. Published by Elsevier Ltd.

NOVEL CELLULOSE/NbOPO4 center dot nH(2)O HYBRID MATERIAL FROM SUGARCANE BAGASSE

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Novel cellulose/NbOPO 4.nH 2O hybrid material from sugarcane bagasse

In recent years studies concerning the applications of lignocellulosic/ inorganic couples have resulted in the development of an interesting class of functional materials. In this work a cellulose/NbOPO 4.nH 2O hybrid using cellulose from surgacane bagasse was prepared and characterized in order to test for adsorption applications. The preparation process was conducted by carrying out metallic niobium dilution in hydrofluoric acid in the presence of nitric acid, then adding boric acid to form the complex and, finally, the cellulose sugar cane bagasse was added. Concentrated phosphoric acid was also inserted to precipitate hydrous niobium phosphate particles in the cellulose fiber. This material was characterized by X-ray diffractometry (XRD), thermogravimetry (TG/DTG), and scanning electronic microscopy (SEM) connected to an energy dispersive spectrophotometer (EDS). Results by SEM/EDS show that NbOPO 4.nH 2O was present in structure of the cellulose. During the preparation of the material, using boric acid it was observed that the formation of precipitate occurred in a shorter time than the material prepared without boric acid.

Preparação e caracterização de materiais híbridos celulose/NbOPO4.nH2O a partir de celulose branqueada de bagaço de cana-de-açúcar

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Combustion synthesis and properties of the NASICON family of materials

The fine-particle NASICON family of materials, MZr2P3O12(where M = Na, K, ½Ca and ¼Zr) and NbZrP3O12, have been prepared by the combustion of aqueous heterogeneous mixtures of stoichiometric amounts of metal nitrate, zirconyl nitrate, niobium phosphate, diammonium hydrogen phosphate, ammonium perchlorate and carbohydrazide (CH) at 400 °C. The formation of NASICON materials was confirmed by powder X-ray diffraction (XRD), IR, solid-state (31P) NMR spectroscopy and thermal expansion coefficient measurements. The combustion-synthesized NASICON powders have an average agglomerate size of 9�13 µm with a specific surface area varying from 8 to 28 m2 g�1. The powders pelletized and sintered in the range 1100�1200 °C for 5 h achieved 95�97% theoretical density and showed fine-grain microstructure. The coefficient of thermal expansion of a sintered compact was measured up to 500 °C and ranged from �1.5 × 10�6°C�1 to 1.0 × 10�6°C�1 depending on the composition.

Preparação e caracterização de híbridos originados a partir do bagaço de cana-de-açúcar/NbOPO4.nH2O e sua aplicação em membranas como elemento filtrante

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Coupled substitution of niobium and silicon in potassium titanyl phosphate and arsenate (KTiOPO4 and KTiOAsO4. Synthesis and nonlinear optical properties of KTi1-xNbxOX1-xSixO4 (X = P, As)

Coupled substitution of Nb(V) and Si(IV) for Ti(IV) and P(V)/As(V) in KTiOP04 (KTP) and KTiOAsO4 (KTA) giving new series of nonlinear optical materials, KTi1-xNbxOX1-xSixO4 (X=P,As), has been investigated. Substitution up to x = 0.40 readily occurs, the members retaining the orthorhombic (Pna2(1)) structure of KTP. The second harmonic generation (SHG) property of the parent KTP and KTA is not adversely affected by the coupled substitution. SHG intensity of the powder samples of the X = P series shows a slight increase with x up to x = 0.15; for 0.15 < x less-than-or-equal-to 0.40, there is a decrease in SHG intensity as compared to that for KTP. A similar trend in SHG intensity is seen for the arsenic analogs.

Adsorption of phosphate from aqueous solution by hydrous zirconium oxide

Synthetic ZrO2 center dot nH(2)O was used for phosphate removal from aqueous solution. The optimum adsorbent dose obtained for phosphate adsorption on to hydrous zirconium oxide was 0.1 g. The kinetic process was described very well by a pseudo-second-order rate model. The phosphate adsorption tended to increase with the decrease in pH. The adsorption capacity increased from 61 to 66 mg g(-1) when the temperature was increased from 298 to 338 K. A phosphate desorption of approximately 74% was obtained using water at pH 12.