Um novo procedimento de síntese da zeólita A empregando argilas naturais

This work proposes the synthesis of zeolite A by IZA standard proceedures starting from a natural clay. The clay was used in its natural form and after calcination at 900ºC. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and porosity analysis by nitrogen adsorption. Results showed low surface area for Na-A zeolite in sodium form, but a higher one in CaA based on the nitrogen accessibility. The presence of cubic crystals for the A phase was observed in the SEM micrographies. The new procedure starting from natural clay favors the formation of sodalite while that using the calcinated clay gives A.

Estudo da síntese da zeólita MCM-71

A new kind of material, denominated MCM-71, was synthesized and characterized by several complementary techniques: X Ray Diffractometry, textural analysis by nitrogen adsorption, Scanning electronic microscopy and infrared spectroscopy. MCM-71 zeolite was successfully synthesized by hydrothermal synthesis in the presence of triethanolamine. Mordenite phase as impurity was not detected, otherwise quartz was observed. The MCM-71 sample obtained presented a BET surface area of 20 m²/g in the as synthesized form and of 85 m²/g in protonic form. By SEM was observed crystals with rectangular shape with average size of 2 x 0,2 x 0,05 µm and this crystals were agglomerated in spherical particles with average diameter between 14 and 24 µm.

Caracterização de cinza do bagaço de cana-de-açúcar para emprego como pozolana em materiais cimentícios

This work presents the results of morphological and physical-chemical characteristics of a sugar cane bagasse ash material sample produced under controlled burning conditions. The investigation was carried out by analyzing chemical composition, X-ray diffraction, 29Si nuclear magnetic resonance, morphology, thermal analysis, particle size, specific surface, and density. Moreover, the pozzolanic activity of the ash was evaluated by pozzolanic activity index and Chapelle's method. The results suggest that the sugar cane bagasse ash has adequate properties to be used as pozzolan in construction materials.

Síntese e avaliação da atividade fitotóxica de derivados da α-Santonina

Mixtures of α-Santonin and various solvents were irradiated by either high or low pressure mercury lamps. The photochemical reactions afforded lumisantonin (11) (76% in acetonitrile), (3S,3aS,9bS)-3,6,6-trimethyl-3,3a,4,5-tetrahydronafto[1,2-b]furan-2,7(6H,9bH)dione (12) (100% in acetonitrile), 10α-acetoxy-3-oxo-1,7αH,6,11βH-guaia-4-en-6,12-olide (8) (26% in acetic acid), 10α-hydroxy-3-oxo-1,7αH,6,11βH-guaia-4-en-6,12-olide (10) (32%) and (E)-3-((3S,3aS,7aS)-3-methyl-2-oxo-6-(propan-2-ylidene)hexahydrobenzofuran-7-(7aH)-ylidene)propanoic acid (9) (44%) (in water/ acetic acid 1:1, v/v). Lactone 12 was also prepared by irradiation of lumisantonin in diethyl ether. Lactones 8 and 10 were converted, respectively, into the 10α-acetoxy-3β-hydroxy-1,7αH,6,11βH-guaia-4-en-6,12-olide (13) (87%) and 3β,10α-dihydroxy-1,7αH,6,11βH-guaia-4-en-6,12-olide (14) (75%) by sodium borohydride reduction. The effects of the compounds on the development of radicle of Sorghum bicolor and Cucumis sativus were evaluated.

Utilização do D-manitol em síntese orgânica

D-mannitol is used in several fields including food, pharmaceuticals, cosmetics and textiles being an important carbohydrate found widespread in nature. Due to its chirality, it is largely used in organic synthesis with several applications, such as ligands, polymers, chiral pool, for preparation of small chiral building blocks, key intermediates in total synthesis. In this context, the aim of this review is to highlights recent applications of D-mannitol, especially in total synthesis.

Reações de organocatálise com aminas quirais: aspectos mecanísticos e aplicações em síntese orgânica

The philosophy of organocatalysis is based on the utilization of organic compounds to catalyze organic transformations without the intervention of metals. This area has attracted much attention of the synthetic chemistry community on the last years, which can be confirmed by the explosion of published papers dealing with this subject. Phosphorus compounds, urea and thiourea derivatives, alkaloids, guanidine derivatives, for example, have already been used as organocatalysts. In this review we have focused on the use of chiral amines as organocatalyst. We have also chosen some outstanding examples to demonstrate the potentiality of this strategy in the synthesis of natural products and biologically active compounds.

Síntese e estudo de ortossilicatos de zinco luminescentes com aplicação da técnica sol-gel

Usually, the concepts of the Sol-Gel technique are not applied in experimental chemistry courses. This work presents a feasible experiment for chemistry instruction, which involves the synthesis of luminescent materials - Zn2SiO4, with and without Mn2+ as a dopant - by the Sol-Gel technique. The obtained materials were analyzed by scanning electron microscopy, X-Ray diffraction, IR spectroscopy and luminescence measures by UV-vis spectroscopy. The results allow the students to confirm the luminescent properties of the zinc orthosilicate luminophores as well as the structural features expected from literature data.

Síntese e avaliação da atividade antimicrobiana de novas 4-tiazolidinonas obtidas a partir de formilpiridina tiossemicarbazonas

Twelve novel 4-thiazolidinone derivatives (2a-l) have been synthesized by reacting formilpyridine thiosemicarbazones (1a-l) and anhydride maleic in toluene. Their chemical structures were confirmed by IR, ¹H and 13C NMR. The new compounds were submitted to in vitro evaluation against pathogenic Gram-positive, Gram-negative bacteria and yeasts. The findings obtained showed that the compounds 2a, 2d, 2e and 2g were effective against some of the bacterial strains used, whereas the compounds 2d, 2e and 2i exhibited a moderate antifungal activity against the yeast strains evaluated. An initial structure activity relationship (SAR) was established.

Polímeros com capacidade de reconhecimento molecular no controlo da libertação de fármacos. Parte 1: síntese e caracterização

Molecularly imprinted polymers (MIPs) consist of synthetic macromolecular matrix, obtained through molecular imprinting-based methods that show ability to selectively recognize important biological molecules and its application in the drug delivery field is under development. In the present review the main aspects related to the synthesis and characterization of MIPs are studied. The fundamental variables participating in the synthesis process, such as template molecule, functional monomers, cross-linking agents, solvents and imprinting approaches are discussed. Moreover, the main available methods for MIPs chemical and morphological characterization are presented and the importance of the obtained information is discussed.

Síntese e caracterização de nanopartículas de óxido de ferro suportadas em matriz carbonácea: remoção do corante orgânico azul de metileno em água

In this work were prepared composites of iron oxide and carbonaceous materials in two different weight proportions (Carbon/Fe 1/1 and 1/2). The physico-chemical properties of the composites were determined by temperature programmed reduction (TPR), adsorption/dessorption of N2, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and pulse titration H2. The XRD and XPS analysis showed a cubic iron oxide phase, identified as maghemite, formed over the carbon surface. The particle size of maghemite showed to be within 10-30 nm. Carbon/Fe 1/2 was the most active in MB removal kinetics and ESI-MS studies showed that MB removal by both composites leads to oxidized intermediates.

Formulações de atrazina em xerogéis: síntese e caracterização

In this study, controlled release formulations of Atrazine (ATZ) were synthesized by the sol-gel method and characterized by elemental, FTIR, SEM, BET and DSC analyses. The release kinetic of ATZ from the formulations in CaCl2 0.01 mol L-1 medium was monitored by UV/Vis spectroscopy. In all formulations, ATZ was physically dispersed on the Si-polymer, and the dispersion grade decreased with increasing amount of herbicide. The ATZ release kinetics was controlled mainly by dissolution, and the data could be fitted to the Korsmeyer - Pepper model. The ATZ as xerogel presents a lower affinity for soil than as granulated form.

Materiais híbridos à base de sílica obtidos pelo método sol-gel

This review deals with silica based hybrid materials obtained by the sol-gel method. It involves concepts, classifications and important definitions regarding the sol-gel method that allows obtaining materials with organic and inorganic components dispersed in a molecular or nanometric level. We discuss the properties and characteristics of hybrid materials related to experimental synthesis conditions. We devote a special attention to the nanostructured materials, where the self-organization is imposed by the organic component. Finally, we present some important applications of these materials based on their specific properties.

Síntese de β-D-galactopiranosídeos de arila diméricos para avaliação de sua interação com a lectina de Erythrina cristagalli

The synthesis of two new D-galactose-based dimers having a 1,4-butanediamine spacer is reported aiming at the evaluation of their interaction with the Erythrina cristagalli lectin. The title compounds were prepared in four and five steps from 2,3,4,6-tetra-O-acetyl-β-D-galactopyranoside bromide, in 20 % and 15 % overall yield, respectively, using the Doebner modification of the Koenavenagel reaction as the key sep. The lectin-carbohydrate interaction could be evaluated for only one dimer, due to solubility problems. A twofold enhancement of affinity was observed, compared to the corresponding monovalent ligand.

Nanoestruturas em fotocatálise: uma revisão sobre estratégias de síntese de fotocatalisadores em escala nanométrica

Advanced oxidative processes (AOPs) are based on chemical processes that can generate free radicals, such as hydroxyl radicals (.OH) which are strong, non-selective oxidant species that react with the vast majority of organic compounds. Nanostructured semiconductors, especially titanium dioxide (TiO2) in the anatase phase, are well-established photocatalysts for this process, which have proved to be useful in the degradation of dyes, pesticides and other contaminants. Research in different strategies for the synthesis of nanostructured semiconductors, with particular characteristic is currently a topic of interest in many studies. Thus, this paper presents a review about various synthesis strategies of nanostructured photocatalysts.

Síntese enzimática de butirato de isoamila empregando lipases microbianas comerciais

Isoamyl butyrate production was investigated using free and immobilized lipases by esterification of butyric acid with isoamyl alcohol in a solvent-free system and in an organic media. Among the enzymes studied, Lipozyme TL IM was found to be the most active catalyst in n-hexane as a solvent. The effects of different solvents and the amount of water added on conversion rates were studied. A maximum conversion yield of 80% in n-hexano at 48 h was obtained under the following conditions: 3 g L-1 of Lipozyme TL IM, 30 ºC, 180 rpm of agitation, isoamyl alcohol to butyric acid molar ratio of 1:1 and acid substrate concentration of 0.06 M.