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1.
Mater Sci Eng C Mater Biol Appl ; 117: 111263, 2020 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-32919629

RESUMO

Post-synthetic modification of covalent organic frameworks (COFs) is strongly demanded in order to provide additional functionalities to their structures. However, the introduction of functional groups during the synthesis of two dimensional COFs (2D COFs) is highly discouraged, as they can interfere with the π-π stacking forces, compromising framework integrity. Here, we show that direct incorporation of nucleophyllic groups (e.g., primary amines) on pore wall during the synthesis of a 2D-COF (COF-5) is possible by sequential substitution of original monomers. Subsequent bonding of the antitumor drug camptothecin results in a stable hydrophobic drug delivery system. Water adsorption isotherms modelling indicates that the insertion of CPT ligand in the framework promotes a hydrophobic effect that protects a region of COF chain from boronate ester hydrolysis and resulting degradation, which is also proven by stability testing in physiological conditions. Furthermore, this hydrophobic nature favors cell internalization kinetics by promoting interactions with the lipophilic cell membrane. To the best of our knowledge, this is the first case of a stable drug delivery system based on covalently conjugated COFs.

2.
Molecules ; 25(15)2020 Jul 23.
Artigo em Inglês | MEDLINE | ID: mdl-32717782

RESUMO

A combination of hard-templating (HT) and soft-templating (ST) approaches was studied to obtain MWW-type materials with intermediate physicochemical properties. The HT methodology involved the introduction of carbon particles as hard templates during gel synthesis to obtain a layered zeolitic precursor (LZP) with particles possessing a microspherical morphology. The LZP obtained was treated with surfactants as soft templates to expand the layers of the LZP, followed by a pillaring procedure. The materials were characterized by X-ray diffraction, transmission and scanning electron microscopy, elemental analysis and N2 adsorption. The results demonstrate that the obtained material possesses intermediate properties from both approaches, with interparticle mesopores/macropores and pore sizes between 18 and 46 Å. However, the ST procedure causes a partial disruption of some microspheres, forming small crystallite aggregates, and results in a decrease in the number of interparticle mesopores/macropores previously formed by the HT method. All synthesized solids presented catalytic activity, which was evaluated by the cracking of low-density polyethylene (LDPE) as a probe reaction.

3.
Chemistry ; 2020 May 19.
Artigo em Inglês | MEDLINE | ID: mdl-32427389

RESUMO

In this work, an MWW-type zeolite with pillars containing silicon and niobium oxide was synthesized to obtain a hierarchical zeolite. The effect of niobium insertion in the pillaring process was determined by combining a controllable acidity and accessibility in the final material. All pillared materials had niobium occupying framework positions in pillars and extra-framework positions. The pillared material, Pil-Nb-4.5 with 4.5 wt % niobium, did not compromise the mesoporosity formed by pillaring, while the increase of niobium in the structure gradually decreased the mesoporosity and ordering of lamellar stacking. The morphology of the pillared zeolites and the niobium content were found to directly affect the catalytic activity. Specifically, we report on the activity of the MWW-type zeolites with niobium catalyzing the gas-phase oxidation of volatile organic compounds (VOCs), which is an important reaction for clean environmental. All produced MWW-type zeolites with niobium were catalytically active, even at low temperatures and low niobium loading, and provided excellent conversion efficiencies.

4.
Molecules ; 25(4)2020 Feb 24.
Artigo em Inglês | MEDLINE | ID: mdl-32102442

RESUMO

The mixture containing alloy and oxide with iron-based phases has shown interesting properties compared to the isolated species and the synergy between the phases has shown positive effect on dye adsorption. This paper describes the synthesis of Fe2SiO4-Fe7Co3-based nanocomposite dispersed in Santa Barbara Amorphous (SBA)-15 and its application in dye adsorption followed by magnetic separation. Thus, it was studied the variation of reduction temperature and amount of hydrogen used in synthesis and the effect of these parameters on the physicochemical properties of the iron and cobalt based oxide/alloy mixture, as well as the methylene blue adsorption capacity. The XRD and Mössbauer results, along with the temperature-programmed reduction (TPR) profiles, confirmed the formation of Fe2SiO4-Fe7Co3-based nanocomposites. Low-angle XRD, N2 isotherms, and TEM images show the formation of the SBA-15 based mesoporous support with a high surface area (640 m2/g). Adsorption tests confirmed that the material reduced at 700 °C using 2% of H2 presented the highest adsorption capacity (49 mg/g). The nanocomposites can be easily separated from the dispersion by applying an external magnetic field. The interaction between the dye and the nanocomposite occurs mainly by π-π interactions and the mixture of the Fe2SiO4 and Fe7Co3 leads to a synergistic effect, which favor the adsorption.

5.
Molecules ; 24(10)2019 May 23.
Artigo em Inglês | MEDLINE | ID: mdl-31126026

RESUMO

The need for greener procedures is a fact to reduce residues, to decrease industrial costs, and to accomplish the environmental agreements. In an attempt to address this question, we propose the addition of a natural resource, Brazilian diatomite, to an MFI zeolite traditional synthesis. We have characterized the resulting product with different techniques, such as X-ray diffraction, microscopy, and gas sorption, and, afterwards, we evaluate the greenness of the process by the Green Star method. The results were promising: We obtained the desired topology in the form of small crystallites aggregated and a pore diameter of 0.8 nm. In conclusion, the product has the necessary characteristics for an adsorption or catalytic future tests and escalation to industrial production.


Assuntos
Terra de Diatomáceas/química , Zeolitas/síntese química , Brasil , Química Verde , Modelos Moleculares , Propriedades de Superfície , Difração de Raios X , Zeolitas/química
6.
Materials (Basel) ; 12(4)2019 Feb 22.
Artigo em Inglês | MEDLINE | ID: mdl-30813262

RESUMO

Wastewater from the oil industry is a major problem for aqueous environments due to its complexity and estimated volume of approximately 250 million barrels per day. The combination of these petroleum pollutants creates risks to human health, and their removal from the environment is considered a major problem in the world today. Thus, this work has the objective of studying the treatment of this type of effluent through the adsorption method using the following exchange materials: cationic, anionic, their combination by a sequential method, and a composite material. Zeolite A, a layered double hydroxide (LDH), and the new composite material formed by zeolite A and LDH structures were synthesized for this study. All were used for the simultaneous treatment of cations and anions in a complex sample such as water produced from petroleum production. The composite demonstrated an excellent ability to simultaneously remove cations and anions. The results obtained after the different treatment modes of the effluent using different materials varied from 85% to 100% for the removal of cations and from 56% to 99.7% for the removal of anions.

7.
ACS Omega ; 3(6): 6217-6223, 2018 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-29978144

RESUMO

The chemistry between layered MWW zeolite and carbon black pearls (BP 2000) as an inexpensive hard template was investigated to develop a rational one-pot synthesis of MCM-22 microspheres. The characterization results showed that the insertion of BP 2000 in the gel synthesis did not substantially compromise the crystallinity and microporosity, and the microscopic analyses showed that BP 2000 played a key role in controlling the final morphology of the MCM-22 zeolite, creating beautiful dandelion-like microspherical particles. The morphology obtained is due to the tortuous shape of the hard template, the particular MWW particle crystals, the interaction with the external surface of the MWW zeolitic precursor, and the synthesis conditions. The stacking of MWW crystals with edge-to-face orientations generates meso-/macrovoids, allowing access to the interiors of the microspheres. The microspheres were homogeneous with sizes ranging from 6 to 8 µm with an increase of the external surface and a macroporous size distribution centered at 200 nm, which is two times that of the traditional MCM-22 zeolite.

8.
Chem Commun (Camb) ; 54(17): 2122-2125, 2018 Feb 22.
Artigo em Inglês | MEDLINE | ID: mdl-29419825

RESUMO

Here, we present the synthesis and structure determination of the new zeolite ITQ-62. Its structure was determined via ultra-fast electron diffraction tomography and refined using powder XRD data of the calcined material. This new zeolite contains a tridirectional channel system of highly distorted 8-rings, as well as a monodirectional 12-ring channel system.

9.
ACS Omega ; 3(10): 13538-13550, 2018 Oct 31.
Artigo em Inglês | MEDLINE | ID: mdl-31458061

RESUMO

The present work introduces new functional bionanocomposite materials based on layered montmorillonite and fibrous sepiolite clays and two biopolymers (carboxymethylcellulose polysaccharide and zein protein) to produce drug-loaded bionanocomposite films for antibiotic topical delivery. Neomycin, an antibiotic indicated for wound infections, was employed as the model drug in this study. The physical properties and the antimicrobial activity of these materials were evaluated as a function of the type of hybrid and the amount of zein protein incorporated in the bionanocomposite films. In addition, the interfacial and physicochemical properties of these new clay-drug hybrids have been studied through a combination of experimental and computational methodologies, where the computational studies confirm the intercalation of neomycin into the montmorillonite layers and the possible penetration of the drug in the tunnels of sepiolite, as pointed out by N2 adsorption and X-ray diffraction techniques. The antimicrobial activity of these bionanocomposite materials show that the films based on montmorillonite-neomycin display a more pronounced inhibitory effect of the bacterial growth than those prepared with the sepiolite-neomycin hybrid. Such effect can be related to the difficult release of neomycin adsorbed on sepiolite due to a strong interaction between both components.

10.
Materials (Basel) ; 10(7)2017 Jun 27.
Artigo em Inglês | MEDLINE | ID: mdl-28773066

RESUMO

Pillared clays (PILCs) are interesting materials mostly due to their high basal spacing and surface area, which make them suitable for adsorption and catalysis applications, for example. However, the production of these materials on industrial scale is dependent on research about what parameters influence the process. Thus, the objective of this work was to evaluate what parameters influence the pillaring procedure. For this, pillared clays were synthesized following three series of experiments. In the first series, the effect of the amount of water in a clay suspension was evaluated. The best results were obtained by using diluted suspensions (1 g of clay to 100 mL of water). In the second series, several pillaring methods were tested. In the third series, the amount of pillared clay was raised to 50 g. Fifty grams of pillared clay can be obtained using the pillaring agent synthesized at 60 °C with further aging for 24 h, and this material exhibited high basal spacing (17.6 Å) and surface area (233 m²/g). These values are comparable with the traditional pillaring method using only 3 g of clay.

11.
Materials (Basel) ; 10(7)2017 Jun 27.
Artigo em Inglês | MEDLINE | ID: mdl-28773068

RESUMO

This work describes the synthesis and characterization of pillared clays using a new pillaring method: the reuse of the pillaring solution. First, an Al pillared clay (PILC) was synthesized, and after filtration, the pillaring agent was stored and reused for an additional three pillaring procedures (P1, P2, and P3). The filtered pillaring solution was stored for one year and then reused for one additional pillaring procedure (P4). The samples were analyzed using XRD, N2 physisorption measurements and chemical analysis (EDX). All of the samples exhibited basal spacings larger than 17 Å and BET surface areas greater than 160 m²/g. After the P4 pillaring, the pillaring agent was precipitated with a Na2SO4 solution, and the resulting solid was analyzed using XRD and SEM. The results indicated that even after a total of five pillaring procedures, Al13 ions were still present in solution. Therefore, it is possible to reuse the pillaring solution four times and to even store the solution for one year, which is important from an industrial perspective.

12.
Molecules ; 22(8)2017 Aug 06.
Artigo em Inglês | MEDLINE | ID: mdl-28783089

RESUMO

Zeolite synthesis is a wide area of study with increasing popularity. Several general reviews have already been published, but they did not summarize the study of imidazolium species in zeolite synthesis. Imidazolium derivatives are promising compounds in the search for new zeolites and can be used to help understand the structure-directing role. Nearly 50 different imidazolium cations have already been used, resulting in a variety of zeolitic types, but there are still many derivatives to be studied. In this context, the purpose of this short review is to help researchers starting in this area by summarizing the most important concepts related to imidazolium-based zeolite studies and by presenting a table of recent imidazolium derivatives that have been recently studied to facilitate filling in the knowledge gaps.


Assuntos
Cátions/química , Imidazóis/química , Zeolitas/síntese química , Técnicas de Química Sintética , Modelos Moleculares , Estrutura Molecular
13.
Mater Sci Eng C Mater Biol Appl ; 75: 1250-1258, 2017 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-28415414

RESUMO

Olanzapine (OLZ) is a drug that is used in the treatment of schizophrenia and other psychoses, and it belongs to the thienobenzodiazepine class. The OLZ molecule has low solubility decreasing bioavailability, but has high permeability in membrane biological being classified as a Class II drug substance according to the Biopharmaceutics Classification System. It was reported many side effects of administering OLZ orally. So, in order to increase the bioavailability of drug and possibly reducing some of side effects, this paper proposes a new material able to controllably release the drug in the body. To control the dissolution rate, this work proposes a system that incorporates the drug into montmorillonite (MMT) dispersed in a mixture of alginate (ALG) and xanthan gum (XG) biopolymers. The proposed hybrids and bionanocomposites were characterized by several physicochemical techniques, including XRD, IR-ATR, TG DTA, SEM-EDS and HPLC. The characterization data confirmed the intercalation of the OLZ into the MMT by the ion exchange process, as well as the interaction of the MMT-OLZ with the biopolymers. The release test, conducted under various pH conditions, showed that the proposed system exhibited a more controlled drug release than commercial tablets, indicating that the ALG-XG/MMT-OLZ bionanocomposite can act as a controlled release system for OLZ.


Assuntos
Alginatos/química , Bentonita/química , Benzodiazepinas , Nanocompostos/química , Polissacarídeos Bacterianos/química , Benzodiazepinas/química , Benzodiazepinas/farmacocinética , Preparações de Ação Retardada , Ácido Glucurônico/química , Ácidos Hexurônicos/química , Olanzapina
14.
Materials (Basel) ; 5(5): 872-881, 2012 May 18.
Artigo em Inglês | MEDLINE | ID: mdl-28817013

RESUMO

Benzene alkylation with propylene was studied in the gas phase using a catalytic membrane reactor and a fixed-bed reactor in the temperature range of 200-300 °C and with a weight hourly space velocity (WHSV) of 51 h-1. ß-zeolite was prepared by hydrothermal synthesis using silica, aluminum metal and TEAOH as precursors. The membrane's XRD patterns showed good crystallinity for the ß-zeolite film, while scanning electron microscopy SEM results indicated that its random polycrystalline film was approximately 1 µm thick. The powders' specific area was determined to be 400 m²×g-1 by N2 adsorption/desorption, and the TPD results indicated an overall acidity of 3.4 mmol NH3×g-1. Relative to the powdered catalyst, the catalytic membrane showed good activity and product selectivity for cumene.

15.
Bioprocess Biosyst Eng ; 35(3): 351-8, 2012 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-21779888

RESUMO

Both stability and catalytic activity of two commercial immobilized lipases were investigated in the presence of different organic solvents in ultrasound-assisted system. In a general way, for Novozym 435, the use of ethanol as solvent led to a loss of activity of 35% after 10 h of contact. The use of iso-octane conducted to a gradual increase in lipase activity in relation to the contact time, reaching a maximum value of relative activity of 126%. For Lipozyme RM IM, after 5 h of exposure, the enzyme presented no residual activity when ethanol was used as solvent. The solvents tert-butanol and iso-octane showed an enhancement of about 20 and 17% in the enzyme activity in 6 h of exposure, respectively. Novozym 435 and Lipozyme IM presented high stability to storage after treatment under ultrasound-assisted system using n-hexane and tert-butanol as solvents.


Assuntos
Enzimas Imobilizadas/química , Lipase/química , Octanos/química , Solventes/química , Som , Temperatura , Fatores de Tempo
16.
Water Res ; 38(17): 3699-704, 2004 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-15350421

RESUMO

In this work the adsorption features of Na Y zeolite with the magnetic properties of iron oxides have been combined in a composite to produce a magnetic adsorbent. These magnetic composites can be used as an adsorbent for metallic contaminants in water and subsequently removed from the medium by a simple magnetic process. The zeolites:iron oxide magnetic composites, were prepared by using Na Y with weight ratio of 3:1 and were characterized by powder X-ray diffraction (XRD), magnetization measurements, chemical analyses, N(2) adsorption isotherms and Mössbauer spectroscopy. Nitrogen adsorption isotherms showed that the surface area decreased from 505 m(2)g(-1) for the pure Na Y to 353 m(2)g(-1) for the Na Y:Fe oxide 3:1 composite. The adsorption isotherms of metal ions Cr(3+), Cu(2+) and Zn(2+) from aqueous solution onto the composites also showed that the presence of iron oxide does not affect the adsorption capacity.


Assuntos
Cromo/isolamento & purificação , Cobre/isolamento & purificação , Poluentes da Água/isolamento & purificação , Purificação da Água/métodos , Zeolitas/química , Zinco/isolamento & purificação , Adsorção , Magnetismo
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