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1.
Medicina (Kaunas) ; 59(12)2023 Nov 21.
Artigo em Inglês | MEDLINE | ID: mdl-38138160

RESUMO

Background and Objectives: Tachycardia is a common cardiovascular disease. Drugs blocking ß1-adrenergic receptors (ADRB1) are used in the therapy of arrhythmogenic heart diseases. Disease-related polymorphisms can be observed within the ADRB1 gene. The two most important are Ser49Gly and Arg389Gly, and they influence the treatment efficacy. The family of the cytochrome P450 system consists of the isoenzyme CYP2D6 (Debrisoquine 4-hydroxylase), which is involved in phase I metabolism of almost 25% of clinically important drugs, including antiarrhythmic drugs. A study was conducted to detect the ADRB1 and CYP2D6 gene polymorphisms. Materials and Methods: The material for the test was whole blood from 30 patients with ventricular and supraventricular tachycardia and 20 controls. The samples were obtained from the Department of Pediatric Cardiology. The first to be made was the extraction of DNA using a GeneMATRIX Quick Blood DNA Purification Kit from EURx. The selected ADRB1 and CYP2D6 gene polymorphisms were detected by high-resolution melting polymerase chain reaction (HRM-PCR) analysis. Results: Based on the analysis of melt profile data for each PCR product, the identification of polymorphisms was carried out. Heterozygotes and homozygotes were found in the examined alleles. Conclusions: The frequency of the Arg389Gly polymorphism differs statistically significantly between the control group and patients with supraventricular and ventricular arrhythmias, as well as between these two groups of patients. Moreover, the Arg389Gly polymorphism was statistically more prevalent in the group of girls with SVT arrhythmia compared to girls with VT. A few carriers of homozygous and heterozygous systems of the S49G polymorphism were detected among patients with arrhythmias, as well as control group. The percentage of individuals carrying the CYP2D6 4 allele as either homozygous or heterozygous was observed in the study and control groups. The high prevalence of the CYP2D6*4 allele carriers in both groups prompts the optimization of beta-1 blocker therapy.


Assuntos
Antagonistas Adrenérgicos beta , Citocromo P-450 CYP2D6 , Criança , Feminino , Humanos , Antagonistas Adrenérgicos beta/uso terapêutico , Arritmias Cardíacas/genética , Citocromo P-450 CYP2D6/genética , DNA , Polimorfismo Genético/genética , Receptores Adrenérgicos beta 1/genética
2.
Molecules ; 28(21)2023 Oct 28.
Artigo em Inglês | MEDLINE | ID: mdl-37959732

RESUMO

The present work concerns proton-conducting composites obtained by replacing the water molecules present in aluminophosphate and silicoaluminophosphate AFI-type molecular sieves (AlPO-5 and SAPO-5) with azole molecules (imidazole or 1,2,4-triazole). Both the introduction of azoles and the generation of Brønsted acid centers by isomorphous substitution in aluminophosphate materials were aimed at improving the proton conductivity of the materials and its stability. In the presented study, AlPO-5 and several SAPO-5 materials differing in silicon content were synthesized. The obtained porous matrices were studied using PXRD, low-temperature nitrogen sorption, TPD-NH3, FTIR, and SEM. The proton conductivity of composites was measured using impedance spectroscopy. The results show that the increase in silicon content of the porous matrices is accompanied by an increase in their acidity. However, this does not translate into an increase in the conductivity of the azole composites. Triazole composites show lower conductivity and significantly higher activation energies than imidazole composites; however, most triazole composites show much higher stability. The different conductivity values for imidazole and triazole composites may be due to differences in chemical properties of the azoles.

3.
Molecules ; 28(17)2023 Aug 31.
Artigo em Inglês | MEDLINE | ID: mdl-37687206

RESUMO

This study focuses on the catalytic properties of ruthenium catalysts supported on modified silicalite-1 (with an MFI structure). By post-synthesis modification of silicalite-1 with solutions of alkali metal compound, a novel and cost-effective method was discovered to create basic centers on the surface of silicalite-1 supports. The modification not only affected the basicity of the supports but also their porosity. The influence of the type of alkali solution (KOH or NaOH) and its concentration (0.1 M or 1.0 M) on both the basicity and porosity was investigated. The modified silicalite-1 materials were employed as supports for ruthenium catalysts (1 wt.% Ru) and evaluated for their CO2 methanation activity. The results were compared with the hydrogenation performance of ruthenium catalysts supported on unmodified silicalite-1. Characterization of the supports and catalysts was conducted using techniques such as BET, XRD, FT-IR, ICP-OES, TPR-H2, H2 chemisorption, TPD-CO2, SEM, and TEM. Remarkably, the catalytic activity of ruthenium supported on silicalite-1 treated with 1.0 M NaOH (exhibiting selectivity toward methane above 90% in a reaction temperature range of 250-450 °C) outperformed both unmodified and KOH-modified silicalite-1 supported Ru catalysts.

5.
Biomater Adv ; 144: 213206, 2023 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-36434929

RESUMO

Novel multifunctional ZnO:Gd@ZIF-8 hybrid inorganic-organic nanocomposites with tunable luminescent-magnetic performance were successfully fabricated using wet chemistry synthesis routes. Physico-chemical characterization including crystal structure, phase compositions, morphology, surface properties, as well as photoluminescent and magnetic characteristics was performed using powder X-ray diffraction (XRD), FT-IR analysis, transmission and scanning electron microscopies (TEM/SEM), N2 adsorption/desorption, SQUID magnetometer, and photoluminescence spectroscopy. The biological studies of obtained materials, such as cytotoxicity profile and in vitro MRI imaging also investigated for potential use as contrast agents. Results showed that the doping with Gd3+ in a broad concentration range and the presence of ZIF-8 layer on ZnO affect the physico-chemical properties of the obtained composites. The obtained porous ZnO:Gd@ZIF-8 composites were highly crystalline with a large surface area. The XRD study indicated the formation of hexagonal wurtzite structure for ZnO and ZnO:Gd3+ (1-5 at.%). Luminescent studies showed, that ZnO is an ideal matrix for the incorporation of Gd3+ ions in a broad concentration range with efficient green luminescence. The PL intensity reached the maximum up to 5 at.% of Gd3+. The zeta potential values indicated the good stability of obtained nanoparticles. Proposed new materials with paramagnetic behavior and outstanding MR imaging capability could be used as potential contrast agents for magnetic resonance imaging.


Assuntos
Nanocompostos , Óxido de Zinco , Luminescência , Espectroscopia de Infravermelho com Transformada de Fourier , Meios de Contraste , Imageamento por Ressonância Magnética , Nanocompostos/química
6.
Cells ; 11(22)2022 11 18.
Artigo em Inglês | MEDLINE | ID: mdl-36429095

RESUMO

Oxidative stress (OS) is one of the reasons for male infertility. Seminal plasma contains a multitude of enzymes and ions which influence OS and thus may affect male fertility. The aim of the study was to check for associations between seminal plasma advanced oxidation protein products (AOPP) concentrations and levels of selected biochemical parameters (total protein, iron, uric acid, magnesium, calcium) in infertile men, and establish whether they are associated with sperm disorders. Seminal plasma AOPP, as well as total protein, iron, uric acid, calcium, and magnesium concentrations, were determined for the following patient groups: normozoospermic (N; n = 33), teratozoospermic (T; n = 30), asthenoteratozoospermic (AT; n = 18), and oligoasthenoteratozoospermic (OAT; n = 28). AOPP concentrations were significantly higher in N and T groups in comparison to AT and OAT groups. Total protein concentrations were significantly lower in the T group in comparison to the AT and OAT groups, whereas iron concentrations significantly decreased in the OAT group in comparison to the T and N patients. AOPP differentiates AT patients from men with other sperm disorders. Our results suggest that asthenozoospermia may be connected with total protein levels. Insufficient iron levels may reflect a decrease in sperm count.


Assuntos
Produtos da Oxidação Avançada de Proteínas , Infertilidade Masculina , Humanos , Masculino , Sêmen , Magnésio , Cálcio , Ácido Úrico , Oxirredução , Ferro
7.
Oxid Med Cell Longev ; 2022: 7657876, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-36071866

RESUMO

The present review gathers together the most important information about variability in clusterin molecular structure, its profile, and the degree of glycosylation occurring in human tissues and body fluids in the context of the utility of these characteristics as potential diagnostic biomarkers of selected pathophysiological conditions. The carbohydrate part of clusterin plays a crucial role in many biological processes such as endocytosis and apoptosis. Many pathologies associated with neurodegeneration, carcinogenesis, metabolic diseases, and civilizational diseases (e.g., cardiovascular incidents and male infertility) have been described as causes of homeostasis disturbance, in which the glycan part of clusterin plays a very important role. The results of the discussed studies suggest that glycoproteomic analysis of clusterin may help differentiate the severity of hippocampal atrophy, detect the causes of infertility with an immune background, and monitor the development of cancer. Understanding the mechanism of clusterin (CLU) action and its binding epitopes may enable to indicate new therapeutic goals. The carbohydrate part of clusterin is considered necessary to maintain its proper molecular conformation, structural stability, and proper systemic and/or local biological activity. Taking into account the wide spectrum of CLU action and its participation in many processes in the human body, further studies on clusterin glycosylation variability are needed to better understand the molecular mechanisms of many pathophysiological conditions. They can also provide the opportunity to find new biomarkers and enrich the panel of diagnostic parameters for diseases that still pose a challenge for modern medicine.


Assuntos
Clusterina , Doença , Glicosilação , Biomarcadores/metabolismo , Clusterina/metabolismo , Humanos , Polissacarídeos
8.
Int J Mol Sci ; 23(18)2022 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-36142505

RESUMO

Nearly 30% of infertility cases are caused by male factor. This study aimed at checking the associations between the sialylation degree of glycoprotein clusterin (CLU) and levels of oxidative-antioxidant balance markers in infertile men. Using lectin-ELISA with biotinylated lectins specific to α2,6-linked (Sambucus nigra agglutinin, SNA) and α2,3-linked (Maackia amurensis agglutinin, MAA) sialic acid (SA), the CLU sialylation in 132 seminal plasmas (SP) and 91 blood sera (BS) were analyzed. Oxidative-antioxidant status was measured by determining Sirtuin-3 (SIRT3), Sirtuin-5 (SIRT5), total antioxidant status (TAS), and ferric reducing antioxidant power (FRAP) levels. We indicate that multiple sperm disorders are associated with decreased expression of MAA-reactive SA in SP. Decreased SP SIRT3 concentrations may be associated with teratozoospermia and oligoasthenoteratozoospermia. ROC curve and cluster analysis revealed that SP relative reactivity of CLU glycans with MAA, the value of MAA/SNA ratio, and SIRT3 and SIRT5 concentrations may constitute an additional set of markers differentiating infertile oligoasthenoteratozoospermic patients (OAT) from normozoospermic (N), asthenoteratozoospermic (AT) and teratozoospermic (T). The multinomial logistic regression analysis confirmed the potential utility of SIRT3 determinations for differentiation between N and OAT groups as well as between N and T groups for SIRT3 and SIRT5. For BS, based on ROC curve and cluster analysis, relative reactivities of CLU glycans with SNA, MAA, SIRT3 and FRAP concentrations may be useful in the differentiation of normozoospermic patients from those with sperm disorders. The multinomial logistic regression analysis showed that the SNA relative reactivity with CLU glycans significantly differentiated the N group from AT, OAT and T groups, and FRAP concentrations significantly differed between N and AT groups, which additionally confirms the potential utility of these biomarkers in the differentiation of infertile patients with abnormal sperm parameters. The knowledge about associations between examined parameters may also influence future research aimed at seeking new male infertility therapies.


Assuntos
Antioxidantes , Sirtuína 3 , Aglutininas , Antioxidantes/metabolismo , Biomarcadores/metabolismo , Clusterina/metabolismo , Glicoproteínas/metabolismo , Humanos , Lectinas/metabolismo , Masculino , Ácido N-Acetilneuramínico/metabolismo , Estresse Oxidativo , Polissacarídeos/metabolismo , Sementes/metabolismo , Sirtuína 3/metabolismo , Espermatozoides/metabolismo
9.
Sci Rep ; 12(1): 8148, 2022 05 17.
Artigo em Inglês | MEDLINE | ID: mdl-35581357

RESUMO

The aim of our work was the synthesis of ZnO nano- and microparticles and to study the effect of shapes and sizes on cytotoxicity towards normal and cancer cells and antibacterial activity toward two kinds of bacteria. We fabricated ZnO nano- and microparticles through facile chemical and physical routes. The crystal structure, morphology, textural properties, and photoluminescent properties were characterized by powder X-ray diffraction, electron microscopies, nitrogen adsorption/desorption measurements, and photoluminescence spectroscopy. The obtained ZnO structures were highly crystalline and monodispersed with intensive green emission. ZnO NPs and NRs showed the strongest antibacterial activity against Escherichia coli and Staphylococcus aureus compared to microparticles due to their high specific surface area. However, the ZnO HSs at higher concentrations also strongly inhibited bacterial growth. S. aureus strain was more sensitive to ZnO particles than the E. coli. ZnO NPs and NRs were more harmful to cancer cell lines than to normal ones at the same concentration.


Assuntos
Nanopartículas Metálicas , Óxido de Zinco , Antibacterianos/química , Antibacterianos/farmacologia , Escherichia coli , Química Verde/métodos , Nanopartículas Metálicas/química , Testes de Sensibilidade Microbiana , Extratos Vegetais/farmacologia , Espectroscopia de Infravermelho com Transformada de Fourier , Staphylococcus aureus , Difração de Raios X , Óxido de Zinco/química , Óxido de Zinco/farmacologia
11.
Adv Med Sci ; 66(2): 411-417, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34509057

RESUMO

PURPOSE: Aberrant expression of various miRNA species has been implicated in numerous cardiac diseases, e.g., heart failure, hypertrophy, conduction disturbances, and arrhythmogenesis. The aim of this study was to determine whether miR-1, miR-133a, and miR-133b can serve as biomarkers in the diagnosis of ventricular (Va) and supraventricular (SVa) arrhythmias in pediatric patients. MATERIALS AND METHODS: Molecular analysis included 30 patients with SVa or Va (13-17.5 years; 14 boys/16 girls) and 20 non-arrhythmic controls. Arrhythmia was confirmed by 24-h Holter ECG recording. miRNA was extracted from serum using the miRNeasyR Serum/Plasma Kit. miScript SYBR Green PCR Kit (Qiagen) was used to quantify miRNA expression. RESULTS: The levels of miR-1 and miR-133a expression were significantly higher in the SVa group than in the controls (p â€‹= â€‹0.0327 and p<0.0001, respectively). Additionally, both groups of patients with arrhythmia presented significantly lower expression levels of miR-133b than the controls (p<0.01 for both comparisons). The level of miR-133a expression in the SVa group was significantly higher than in the Va group (p â€‹= â€‹0.0124). ROC analysis demonstrated that the expressions of miR-1 and miR-133a could differentiate between the SVa patients and arrhythmia-free controls (AUC â€‹= â€‹0.7091, p â€‹= â€‹0.07 and AUC â€‹= â€‹0.8021, p â€‹= â€‹0.007, respectively). Furthermore, the expression of miR-133b was shown to distinguish patients with SVa and Va from the arrhythmia-free controls (AUC â€‹= â€‹0.7273, p â€‹= â€‹0.07 and AUC â€‹= â€‹0.8030, p â€‹= â€‹0.04, respectively). CONCLUSIONS: miR-1, miR-133a, and miR-133b have the potential to become diagnostic biomarkers of arrhythmia in pediatric patients.


Assuntos
MicroRNA Circulante , MicroRNAs , Arritmias Cardíacas/diagnóstico , Arritmias Cardíacas/genética , Biomarcadores , Criança , MicroRNA Circulante/genética , Feminino , Humanos , Masculino , MicroRNAs/genética , Curva ROC
12.
Sci Rep ; 11(1): 15674, 2021 08 02.
Artigo em Inglês | MEDLINE | ID: mdl-34341430

RESUMO

In the seminal plasma (n = 118) and serum (n = 90) clusterin (CLU) the fucosylation and the expression of selected fucosyltransferases (FUTs) were analyzed. Samples from infertile men were divided into groups based on the results of the standard semen analysis: normozoospermic (N), teratozoospermic (T), asthenoteratozoospermic (AT) and oligoasthenoteratozoospermic (OAT). The CLU fucosylation was analyzed using lectin-ELISAs with biotinylated lectins specific to α1,3-, α1,2-linked antennary fucose, and α1,6-linked core fucose (LTA, UEA, and LCA, respectively). The concentrations of FUT3 and FUT4, reflecting the expression of Le oligosaccharide structures, were measured using ELISA tests. The differences in serum CLU and FUT4 concentrations, and in the expression of core fucose and antennary fucose α1,2-linked in CLU glycans between the N group and other groups examined suggest that the disturbances in sperm count, motility, and morphology are not the only cause of male infertility. Lack of similarities between levels of examined parameters in blood serum and seminal plasma may suggest the differences in mechanisms leading to glycoproteins glycosylation. It confirmed the observed differences in concentrations of seminal plasma CLU, FUT3, and FUT4 between the OAT group and N, T, AT groups, indicating that decreased sperm count may be related to these parameters expression. The serum CLU concentrations and expression of core fucose and fucose α1,2-linked in CLU, seem to be good markers differentiating normozoospermic men from those with abnormal sperm parameters, which was not observed for seminal plasma.


Assuntos
Clusterina , Infertilidade Masculina , Biomarcadores/metabolismo , Clusterina/metabolismo , Glicosilação , Humanos , Masculino , Polissacarídeos/metabolismo
13.
Materials (Basel) ; 14(16)2021 Aug 09.
Artigo em Inglês | MEDLINE | ID: mdl-34442987

RESUMO

This paper investigates the catalytic properties of the iridium catalysts supported on modified silicalite-1. Post-synthesis modification of silicalite-1, with solutions of ammonium compounds (NH4F and NH4OH), appeared to be an efficient method to generate the acidic sites in starting support. The modification of support led not only to changes in its acidity but also its porosity-formation of additional micro- and mesopores. The novel materials were used as supports for iridium. The iridium catalysts (1 wt.% Ir) were characterized by N2 adsorption/desorption measurements, temperature-programmed reduction with hydrogen (TPR-H2), H2 chemisorption, transmission electron microscopy (TEM), temperature-programmed desorption of ammonia (TPD-NH3), X-ray photoelectron spectroscopy (XPS) and tested in the hydrogenation of toluene reaction. The catalytic activity of iridium supported on silicalite-1 treated with NH4OH (higher porosity of support, better dispersion of active phase) was much higher than that of Ir supported on unmodified and modified with NH4F silicalite-1.

14.
Materials (Basel) ; 14(4)2021 Feb 18.
Artigo em Inglês | MEDLINE | ID: mdl-33670803

RESUMO

The modification of commercial silica with solutions of NH4F or NH4Cl salts, followed by thermal treatment, enabled generation of the acidic sites in SiO2 and changed its textural properties. The use of ammonium salts solution also caused the generation of additional porosity. Using NH4F solution caused significant decrease in the specific surface area and the increase in the average pore diameter. The number and strength of resulting acid sites depend on the nature of anion in the applied ammonium salt and the concentration of salt solution. It has been found that the sample treated with NH4F presented higher total acidity (TPD-NH3) and the amount as well as the strength of acid sites increased with the concentration of the used modifier. As modified amorphous SiO2 materials used as a support for iridium (1 wt %, Ir(acac)3) nanoparticles permitted to obtain highly active catalysts for toluene hydrogenation under atmospheric pressure. The highest activity (expressed as the apparent rate and TOF) was obtained for iridium catalysts supported on silica modified by NH4F with the highest acidity. The modification of silica with NH4F favors the generation of centers able to adsorb toluene, which results in higher activity of this catalyst.

15.
Mol Reprod Dev ; 87(5): 515-524, 2020 05.
Artigo em Inglês | MEDLINE | ID: mdl-32222009

RESUMO

Male infertility is becoming a rapidly growing problem around the world, mainly in the highly developed countries. Seminal proteome composition seems to be one of the crucial factors of the proper course of fertilization - clusterin (CLU) is among the most important ones. CLU, as one of the crucial seminal plasma glycoproteins, plays a very important role in sperm capacitation and immune tolerance in the female reproductive tract. CLU is also known as a sensitive marker of oxidative stress. It has six n-glycosylation sites and also exhibits chaperone activity. An analysis of changes in the profile and degree of CLU glycosylation may shed some new light on the molecular mechanisms of the fertilization process and may be used as an additional diagnostic marker of male fertility. This study constitutes a review of the recently available literature concerning human seminal CLU, including changes in its glycosylation, analyzed in the context of human reproduction.


Assuntos
Clusterina/metabolismo , Infertilidade Masculina/diagnóstico , Sêmen/metabolismo , Animais , Biomarcadores/análise , Biomarcadores/metabolismo , Clusterina/análise , Feminino , Glicoproteínas/análise , Glicoproteínas/metabolismo , Glicosilação , Humanos , Infertilidade Masculina/metabolismo , Masculino , Estresse Oxidativo/fisiologia , Proteoma/metabolismo , Sêmen/química , Capacitação Espermática/fisiologia
16.
Molecules ; 25(4)2020 Feb 19.
Artigo em Inglês | MEDLINE | ID: mdl-32093052

RESUMO

Zeolite-based catalysts are globally employed in many industrial processes, such as crude-oil refining and bulk chemical production. In this work, the cracking of low-density polyethylene (LDPE) was thoroughly followed in a FTIR operando study to examine the catalytic efficiency of purely microporous zeolites of various textural characteristics. To provide complementary and valuable information on the catalytic activity of the zeolite studied, the thermogravimetric analysis results were compared with yields of the products generated under operating conditions. The reaction products were analyzed via GC-MS to determine the hydrocarbon chain distribution in terms of paraffin, olefins, and aromatics. The individual impact of textural and acidic parameters on catalytic parameters was assessed. The accumulation of bridging hydroxyls of high strength in the zeolite benefited the decrease in polymer decomposition temperature. Through a strategic comparison of purely microporous zeolites, we showed that the catalytic cracking of LDPE is dominated by the acidic feature inherent to the microporous environment.


Assuntos
Polietileno/química , Zeolitas/química , Catálise , Porosidade , Espectroscopia de Infravermelho com Transformada de Fourier
17.
Materials (Basel) ; 14(1)2020 Dec 29.
Artigo em Inglês | MEDLINE | ID: mdl-33383718

RESUMO

In this study, GNF@ZnO composites (gelatin nanofibers (GNF) with zinc oxide (ZnO) nanoparticles (NPs)) as a novel antibacterial agent were obtained using a wet chemistry approach. The physicochemical characterization of ZnO nanoparticles (NPs) and GNF@ZnO composites, as well as the evaluation of their antibacterial activity toward Gram-positive (Staphyloccocus aureus and Bacillus pumilus) and Gram-negative (Escherichia coli and Pseudomonas fluorescens) bacteria were performed. ZnO NPs were synthesized using a facile sol-gel approach. Gelatin nanofibers (GNF) were obtained by an electrospinning technique. GNF@ZnO composites were obtained by adding previously produced GNF into a Zn2+ methanol solution during ZnO NPs synthesis. Crystal structure, phase, and elemental compositions, morphology, as well as photoluminescent properties of pristine ZnO NPs, pristine GNF, and GNF@ZnO composites were characterized using powder X-ray diffraction (XRD), FTIR analysis, transmission and scanning electron microscopies (TEM/SEM), and photoluminescence spectroscopy. SEM, EDX, as well as FTIR analyses, confirmed the adsorption of ZnO NPs on the GNF surface. The pristine ZnO NPs were highly crystalline and monodispersed with a size of approximately 7 nm and had a high surface area (83 m2/g). The thickness of the pristine gelatin nanofiber was around 1 µm. The antibacterial properties of GNF@ZnO composites were investigated by a disk diffusion assay on agar plates. Results show that both pristine ZnO NPs and their GNF-based composites have the strongest antibacterial properties against Pseudomonas fluorescence and Staphylococcus aureus, with the zone of inhibition above 10 mm. Right behind them is Escherichia coli with slightly less inhibition of bacterial growth. These properties of GNF@ZnO composites suggest their suitability for a range of antimicrobial uses, such as in the food industry or in biomedical applications.

18.
RSC Adv ; 10(17): 10144-10154, 2020 Mar 06.
Artigo em Inglês | MEDLINE | ID: mdl-35498567

RESUMO

V-containing mesoporous silica with 3D structure was prepared by a hydrothermal procedure using NH4VO3 as the vanadium precursor and with varied reaction mixture pH values (pH = 3 and pH = 5). The combined use of DR UV-vis and H2-TPR techniques confirmed the successful incorporation of vanadium into the structure of the mesoporous silica material. The number of acid sites, evidenced by ammonia TPD, strongly correlates with the vanadium content. Propene oxidation with N2O revealed the noticeable activity of the synthesised vanadium-containing mesoporous materials in epoxidation reactions. The activity of the synthesized vanadosilicates is compared with the performance of vanadium-supported catalysts (on mesoporous silica of 3D structures) prepared by wet-impregnation method. On the basis of TOF analysis indicating the activity of particular vanadium ions, it was evidenced that although the presence of isolated V species is crucial in propene epoxidation, the availability of the active species is of paramount importance for proper vanadium utilization.

19.
RSC Adv ; 9(9): 4671-4681, 2019 Feb 05.
Artigo em Inglês | MEDLINE | ID: mdl-35514626

RESUMO

V-containing silica SBA-3 mesoporous catalysts were prepared by means of one-pot hydrothermal procedure with NH4VO3 or VOSO4 as vanadium precursors under various acidic medium of the reaction mixture (pH < 1, 2.2 or 3.1). The combined spectral techniques (DR UV-vis, FTIR, EPR) as well H2-TPR allowed to determine the nature of vanadium species in the studied samples. A successful incorporation of vanadium into the structure of silica SBA-3 was attained for the samples with low V content (<1 wt%), whereas the V-rich samples (i.e. >5 wt%) exhibited the presence of isolated vanadium and also of polynuclear surface species. The resulting V-bearing samples contain the Brønsted and Lewis acidic centres evidenced by FTIR spectra of adsorbed pyridine and by catalytic activity for 2-propanol decomposition and cumene cracking. Ammonia TPD allowed to estimate the number and strength of acid sites in regards to the vanadium content. Propene oxidation with N2O revealed noticeable activity of the synthesised V-SBA-3 samples in epoxidation reaction. On the basis of TOF analysis indicating the activity of particular vanadium ions it seems that not all of the introduced V atoms take part in the formation of mild electrophilic oxygen species responsible for propene oxide formation.

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