scholarly journals Copper(II)-Bis-Cyclen Intercalated Graphene Oxide as an Efficient Two-Dimensional Nanocomposite Material for Copper-Catalyzed Azide–Alkyne Cycloaddition Reaction

2022 ◽  
Vol 9 ◽  
Author(s):  
Angel Green Samuel ◽  
Sowmya Subramanian ◽  
Vijaikanth Vijendran ◽  
Jebasingh Bhagavathsingh

We report stable and heterogeneous graphene oxide (GO)–intercalated copper as an efficient catalyst for the organic transformations in green solvents. The GO-intercalated copper(II) complex of bis(1,4,7,10-tetraazacyclododecane) [Cu(II)-bis-cyclen] was prepared by a facile synthetic approach with a high dilution technique. The as-prepared GO-Cu(II)-bis-cyclen nanocomposite was used as a click catalyst for the 1,3 dipolar Huisgen cycloaddition reaction of terminal alkyne and azide substrates. On directing a great deal of attention toward the feasibility of the rapid electron transfer rate of the catalyst in proliferating the yield of 1,2,3-triazole products, the click catalyst GO-Cu(II)-bis-cyclen nanocomposite was designed and synthesized via non-covalent functionalization. The presence of a higher coordination site in an efficient 2D nanocomposite promotes the stabilization of Cu(I) L-acetylide intermediate during the catalytic cycle initiated by the addition of reductants. From the XRD analysis, the enhancement in the d-interlayer spacing of 1.04 nm was observed due to the intercalation of the Cu(II)-bis-cyclen complex in between the GO basal planes. It was also characterized by XPS, FT-IR, RAMAN, UV, SEM, AFM, and TGA techniques. The recyclability of the heterogeneous catalyst [GO-Cu(II)-cyclen] with the solvent effect has also been studied. This class of GO-Cu(II)-bis-cyclen nanocomposite paves the way for bioconjugation of macromolecules through the click chemistry approach.

2020 ◽  
Vol 2020 ◽  
pp. 1-15
Author(s):  
Shengqiong Fang ◽  
Yueqi Xiao ◽  
Huiqiang Wang

Pristine montmorillonite (Mont) was used as raw materials to prepare hydroxyl-Fe-pillared Mont, hydroxyl-Al-pillared Mont, and hydroxyl-Fe-Al-pillared Mont composites. By varying the OH/Fe and Fe/Al molar ratios during the preparation of the pillared Mont, the adsorption capacity of zearalenone (ZEA) and the kinetics were elucidated. The characterization of X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy reveals the adsorption mechanism of pristine and modified Mont. The results indicated that the ZEA adsorption capacity is Mont (0.05 mg/g) << 1.5OH/Fe-Mont (0.28 mg/g) << OH/Al-Mont (0.51 mg/g) < 0.5Fe/Al-Mont (0.56 mg/g) in the condition of pH = 8 and 37°C, in which both 0.5Fe/Al-Mont and OH/Al-Mont reached maximum adsorption capacity and 1.5OH/Fe-Mont attained 5 times the capacity of Mont. Adsorption isotherm studies revealed that Freundlich adsorption isotherms best represented the experimental data. The kinetic data for ZEA adsorption revealed that the Mont adsorption capacity for ZEA equilibrates in 1 hour and is best described using the pseudo-second-order rate equation. The XRD analysis indicated that the amplification of Fe-dominant pillared Mont interlayer spacing is the main reason for the observed increases in the adsorption capacity of ZEA, while Al-dominant pillared Mont has a relatively stable Keggin structure; therefore, interlayer spacing is not the primary mechanism for changes in the adsorption capacity of both OH/Al-Mont and Al-dominant pillared Mont. An FT-IR analysis demonstrated that cationic exchange was the dominant mechanism that allowed ZEA and hydroxyl-Al ions to enter the Mont interlayers, while this cationic exchange mechanism was not the dominant mechanism used by hydroxyl-Fe entering the Mont layers.


Polymers ◽  
2020 ◽  
Vol 12 (10) ◽  
pp. 2424
Author(s):  
Elena Iuliana Bîru ◽  
Sorina Alexandra Gârea ◽  
Horia Iovu

The covalent functionalization of graphene oxide (GO) surface with hyperbranched benzoxazine (BZ) structures has been achieved using poly(amidoamine) dendrimers (PAMAM) of different generations. By increasing the PAMAM generation, multiple benzoxazine rings were synthesized decorating the GO layers. The polymerization process and the exfoliation behavior were investigated. The novel BZ-functionalized GO hybrid materials were characterized by a combination of techniques such as FT-IR, XPS, and 1H-NMR for the confirmation of benzoxazine formation onto the GO layer surfaces. Raman and XRD investigation showed that the GO stacking layers are highly disintegrated upon functionalization with hyperbranched benzoxazine monomers, the exfoliation being more probably to occur when lower PAMAM generation (G) is involved for the synthesis of hybrid GO-BZ nanocomposites. The polymerization of BZ rings may occur either between the BZ units from the same dendrimer molecule or between BZ units from different dendrimer molecules, thus influencing the intercalation/exfoliation of GO. DSC data showed that the polymerization temperature strongly depends on the PAMAM generation and a significant decrease of this value occurred for PAMAM of higher generation, the polymerization temperature being reduced with ~10 °C in case of GO-PAMAM(G2)-BZ. Moreover, the nanoindentation measurements showed significant mechanical properties improvement in case of GO-PAMAM(G2)-BZ comparing to GO-PAMAM(G0)-BZ in terms of Young modulus (from 0.536 GPa to 1.418 GPa) and stiffness (from 3617 N/m to 9621 N/m).


2021 ◽  
Vol 21 (12) ◽  
pp. 6016-6023
Author(s):  
Pouran Pourayoob Foumani ◽  
Hassan Tajik ◽  
Farhad Shirini ◽  
Shahed Hassanpoor

Manganese dioxide (α-MnO2) and graphene oxide (GO nanocomposites were prepared and successfully characterized using Fourier-transform infrared (FT-IR), field emission scanning-electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDX) mapping methods and Xray diffraction (XRD) analyses. This reagent is an efficient catalyst for the aerobic oxidation of trimethylsilyl (TMS), tetrahedropyranyl (THP), and methoxymethyl ethers (MOM) to their corresponding carbonyl compounds in the presence of K2CO3. All reactions were performed in n-hexane under mild and completely heterogeneous reaction conditions. Our novel method has the advantages of excellent yields, short reaction times, availability and reusability of the catalyst and simple and easy work-up procedure compared to the conventional methods reported in the literature.


2016 ◽  
Vol 10 (4) ◽  
pp. 395-400 ◽  
Author(s):  
Deepali Kelkar ◽  
◽  
Ashish Chourasia ◽  
◽  

Poly(3,4-ethylenedioxythiophene) (PEDOT) was chemically synthesized, undoped and then re-doped using FeCl3 as well as camphorsulfonic acid (CSA). FT-IR results confirm the nature of the synthesized and doped samples. XRD analysis indicates crystal structure modification after doping and was also used to calculate crystallinity of samples. Crystallinity increases after FeCl3 doping, whereas it reduces due to CSA doping. TGA-DTA results show reduction in Tg value for FeCl3 doped sample while it increases for CSA doped samples compared to that of undoped PEDOT. Reduction in Tg indicates plasticizing effect of FeCl3 whereas increase in Tg show anti-plasticizing effect of CSA in PEDOT. Conductivity value () increases by two orders of magnitude after doping. Log vs. 1/T graph show metallic nature of undoped PEDOT above 308 K, however both doped samples show semiconducting nature from 301 to 383 K.


Author(s):  
Soumitra Satapathi ◽  
Rutusmita Mishra ◽  
Manisha Chatterjee ◽  
Partha Roy ◽  
Somesh Mohapatra

Nano-materials based drug delivery modalities to specific organs and tissues has become one of the critical endeavors in pharmaceutical research. Recently, two-dimensional graphene has elicited considerable research interest because of its potential application in drug delivery systems. Here we report, the drug delivery applications of PEGylated nano-graphene oxide (nGO-PEG), complexed with a multiphoton active and anti-cancerous diarylheptanoid drug curcumin. Specifically, graphene-derivatives were used as nanovectors for the delivery of the hydrophobic anticancer drug curcumin due to its high surface area and easy surface functionalization. nGO was synthesized by modified Hummer’s method and confirmed by XRD analysis. The formation of nGO, nGO-PEG and nGO-PEG-Curcumin complex were monitored through UV-vis, IR spectroscopy. MTT assay and AO/EB staining found that nGO-PEG-Curcumin complex afforded highly potent cancer cell killing in vitro with a human breast cancer cell line MCF7.


2020 ◽  
Vol 17 (11) ◽  
pp. 857-863
Author(s):  
Mohammad Ali Nasseri ◽  
Seyyedeh Ameneh Alavi ◽  
Milad Kazemnejadi ◽  
Ali Allahresani

A convenient and efficient chiral CuFe2O4@SiO2-Mn(III) Ch.salen nanocatalyst has been developed for the C-N cross-coupling reactions of aryl halides/ phenylboronic acid with N-heterocyclic compounds in water and/or DMSO under mild conditions. The catalyst could be applied for the N-arylation of a variety of nitrogen-containing heterocycles with aryl chlorides, bromides, iodides and phenylboronic acid under mild conditions. Moderate to good yields were achieved for all substrates. The structure of catalyst was characterized using various techniques including FT-IR, FE-SEM, EDX, XRD, TEM and TGA. The catalyst can be simply recovered and reused for several times without significant loss of activity.


2020 ◽  
Vol 17 (2) ◽  
pp. 117-130 ◽  
Author(s):  
Mehdi Kalhor ◽  
Zohre Zarnegar ◽  
Zahra Seyedzade ◽  
Soodabeh Banibairami

Background: SO3H-functionalized zeolite-Y was prepared and used as a catalyst for the synthesis of 2-aryl-N-benzimidazole-4-thiazolidinones and tri-substituted imidazoles at ambient conditions. Objective: The goals of this catalytic method include excellent yields and high purity, inexpensive procedure and ease of product isolation, the use of nontoxic and heterogeneous acid catalyst, shorter reaction times and milder conditions. Materials and Methods: NMR spectra were recorded on Brucker spectrophotometer using Me4Si as internal standard. Mass spectra were recorded on an Agilent Technology 5975C VL MSD with tripe-axis detector. FTIR spectra were obtained with KBr disc on a galaxy series FT-IR 5000 spectrometer. The surface morphology of nanostructures was analyzed by FE-SEM (EVO LS 10, Zeiss, Carl Zeiss, Germany). BET analysis were measured at 196 °C by a Japan Belsorb II system after the samples were vacuum dried at 150°C overnight. Results: The NSZ was characterized by FT-IR, FESEM, EDX, XRF, and BET. The catalytic activity of NSZ was investigated for synthesis of 1,3-tiazolidin-4-ones in H2O/Acetone at room temperature. Moreover, NSZ was used for synthesis of tri-substituted imidazoles at 60 °C via solvent-free condensation. Different kinds of aromatic aldehydes were converted to the corresponding of products with good to excellent yields. Conclusion: Sulfonated zeolite-Y was as an efficient catalyst for the preparation of N-benzimidazole-2-aryl-1,3- thiazolidin-4-ones and 2,4,5-triaryl-1H-imidazoles. High reaction rates, elimination toxic solvent, simple experimental procedure and reusability of the catalyst are the important features of this protocol.


Nanophotonics ◽  
2020 ◽  
Vol 9 (15) ◽  
pp. 4601-4608 ◽  
Author(s):  
Pengyu Zhuang ◽  
Hanyu Fu ◽  
Ning Xu ◽  
Bo Li ◽  
Jun Xu ◽  
...  

AbstractInterfacial solar vapor generation has revived the solar-thermal-based desalination due to its high conversion efficiency of solar energy. However, most solar evaporators reported so far suffer from severe salt-clogging problems during solar desalination, leading to performance degradation and structural instability. Here, we demonstrate a free-standing salt-rejecting reduced graphene oxide (rGO) membrane serving as an efficient, stable, and antisalt-fouling solar evaporator. The evaporation rate of the membrane reaches up to 1.27 kg m−2 h−1 (solar–thermal conversion efficiency ∼79%) under one sun, out of 3.5 wt% brine. More strikingly, due to the tailored narrow interlayer spacing, the rGO membrane can effectively reject ions, preventing salt accumulation even for high salinity brine (∼8 wt% concentration). With enabled salt-antifouling capability, flexibility, as well as stability, our rGO membrane serves as a promising solar evaporator for high salinity brine treatment.


2013 ◽  
Vol 678 ◽  
pp. 56-60 ◽  
Author(s):  
Cherukutty Ramakrishnan Minitha ◽  
Ramasamy Thangavelu Rajendrakumar

Reduced graphene oxide is an excellent candidate for various electronic devices such as high performance gas sensors. In this work Graphene oxide was prepared by oxidizing graphite to form graphite oxide. From XRD analysis the peak around 11.5o confirmed that the oxygen was intercalated into graphite. By using hydrazine hydrate, the epoxy group in graphite oxide was reduced then the solution of reduced graphite oxide (rGO) is exfoliated. Raman spectrum of rGO contains both G band (1580 cm-1), D band (1350 cm-1). The remarkable structural changes reveals that reduction of graphene oxide from the values of ID/IG ratio that increase from 0.727 (GO) to 1.414 (rGO). The exfoliated reduced graphite oxide solution is spin coated on to the SiO2/Si substrates.


Author(s):  
Erdoğan Karip ◽  
Mehtap Muratoğlu

People are exposed to different kinds of diseases or various accidents in life. Hydroxyapatite (HA) has been widely employed for bone treatment applications. In this study, HA was extracted from sheep bones. Bio-composites were doped with 1, 5, and 10 wt.% of expanded perlite and 5 wt.% of ZrO2–MgO-P2O5. The bio-composites were prepared by the cold isostatic pressing method (250 MPa) and sintered at 900°C for 1 h. In order to evaluate the characteristics of the bio-composites, microhardness, density, X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) analyses were carried out on them. Additionally, the specimens whose characteristics were determined were kept in synthetic body fluid (SBF), and their in vitro behavior was examined. As a result, it was observed that microhardness increased as both the weight and the grain size of the expanded perlite were increased. Calcium silicate, tri-calcium phosphate, and hydroxyapatite were observed in the XRD analysis of all samples, and the formation of apatite structures was increased by addition of ZrO2–MgO–P2O5.


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