Search Results (31)

An experimental study was conducted on the feasibility of using frozen beads with the properties of Rupert’s drops—solid frozen beads with enhanced strength made from a mixture of aromatic hydrocarbons—in cryogenic neutron moderators utilizing bead technology. It is demonstrated that the use of a new modification of the dosing device with a high discharge rate (approximately 6 units/s) significantly improves process efficiency. With standard pneumatic transport parameters maintained, it was possible to load solid frozen beads made from a mixture of mesitylene and meta-xylene into the cryogenic moderator chamber. The loading speed increased five-fold, while the beads remained intact during pneumatic transport. Full article

Liquid and vapor phase transfer hydrogenation with 2-alkanols as hydrogen donors in the presence of MgO as a catalyst was studied. A series of dicarbonyl compounds as well as the equimolar mixtures of various monocarbonyl compounds were used as hydrogen acceptors in order to determine the chemoselectivity (ChS) in the reduction of their carbonyl groups. Thus, 1,4-diacetylbenzene was reduced to 1-(4-acetylphenyl)-1-ethanol with 89% ChS and 1,3-diacetyl-4,6-dimethylbenzene with 100% ChS. Mesitylene diacyl derivatives were unreactive in the studied reaction. CTH of an equimolar mixture of benzaldehyde and acetophenone gave benzyl alcohol and 1-PhEtOH with yields of 91 and 3%, respectively (97% ChS). An equimolar mixture of acetophenone and 6-undecanone underwent CTH with yields of the corresponding alcohols of 89 and 2%, respectively, with 98% ChS towards 1-PhEtOH. Significant differences in reactivity in CTH were reported for an equimolar mixture of regioisomeric 1- and 2-acetylnaphthalenes. The yields of the corresponding alcohols were 20 and 68% with a ChS of 77% towards 2-NphCH(OH)Me. In the case of CTH of 3-oxo-2,2-dimethylbutanal and 2,4-bis(spirocyclohexyl)-1,3-cyclobutanedione with 2-propanol, only the solvolysis of the substrates was observed. The products were methyl isopropyl ketone and isopropyl formate for the former diketone and 1-(cyclohexylcarbonyl)-1-(carboisopropoxy)cyclohexane for the latter. Full article

Amorphous mesoporous materials are promising as catalysts for processes involving or forming bulk molecules. In a reaction such as acetone condensation to form mesitylene, an effective catalyst should not only have a developed porous structure but also have active centers of acidic and basic types. The sol–gel approach allows one to obtain titanosilicates with such characteristics. This work demonstrates the possibility of controlling their properties by varying the conditions for the synthesis of titanosilicate gels. It has been established that controlling hydrolysis allows one to increase the activity of amorphous mesoporous titanosilicates by 10 times: from acetone conversion of 6% to 60%. It has been shown that the use of titanium acetylacetonate complexes in the synthesis of gels leads to an increase in the content of tetracoordinated Ti in the structure and contributes to an increase in the acidity of titanosilicates. During the condensation of acetone on the obtained mesoporous titanosilicates, high acetone conversion (60–79%) and mesitylene selectivity of up to 83% were achieved. Full article

Easy-to-handle N-hydroxyacridinecarbimidoyl chloride hydrochlorides were synthesized as convenient nitrile oxide precursors in the preparation of 3-(acridin-9/2-yl)isoxazole derivatives via 1,3-dipolar cycloaddition with terminal alkynes, 1,1-dichloroethene, and acrylonitrile. Azirines with an acridin-9/2-yl substituent attached directly or via the 1,2,3-triazole linker to the azirine C2 were also synthesized. The three-membered rings of the acridine–azirine hybrids were found to be resistant to irradiation in the UV/visible boundary region, despite their long-wave absorption at 320–420 nm, indicating that the acridine moiety cannot be used as an antenna to transfer light energy to generate nitrile ylides from azirines for photoclick cycloaddition. The acridine–isoxazole hybrids linked at the C9–C3 or C2–C3 atoms under blue light irradiation underwent the addition of such hydrogen donor solvents, such as, toluene, o-xylene, mesitylene, 4-chlorotoluene, THF, 1,4-dioxane, or methyl tert-butyl ether (MTBE), to the acridine system to give the corresponding 9-substituted acridanes in good yields. The synthesized acridine–azirine, acridine–isoxazole, and acridane–isoxazole hybrids exhibited cytotoxicity toward both all tested cancer cell lines (HCT 116, MCF7, and A704) and normal cells (WI-26 VA4). Full article

The new Lewis acid–base adducts of general formula X(nad)B←NC₅H₄-C₅H₄N→B(nad)X [nad = 1,8-O₂C₁₀H_6, X = C₆H₅ (2c), 3,4,5-F₃-C₆H₂ (2d)] were synthesized in high yields via reactions of 1,8-dihydroxy naphthalene [nadH₂] and 4,4′-bipyridine with the aryl boronic acids C₆H₅B(OH)₂ and 3,4,5-F₃-C₆H₂B(OH)₂, respectively, and structurally characterized by multi-nuclear NMR spectroscopy and SCXRD. Self-assembled H-shaped Lewis acid–base adduct 2d proved to be effective in forming thermally stable host–guest complexes, 2d × solvent, with aromatic hydrocarbon solvents such as benzene, toluene, mesitylene, aniline, and m-, p-, and o-xylene. Crystallographic analysis of these solvent adducts revealed host–guest interactions to primarily occur via π···π contacts between the 4,4′-bipyridyl linker and the aromatic solvents, resulting in the formation of 1:1 and 1:2 host–guest complexes. Thermogravimetric analysis of the isolated complexes 2d × solvent revealed their high thermal stability with peak temperatures associated with the loss of solvent ranging from 122 to 147 °C. 2d, when self-assembled in an equimolar mixture of m-, p-, and o-xylene (1:1:1), preferentially binds to o-xylene. Collectively, these results demonstrate the ability of 1,8-dihydroxy naphthalene to serve as an effective building block in the selective self-assembly to supramolecular aggregates through dative covalent N→B bonds. Full article

The synthesis of a scaffold that can accommodate big molecules with a pharmaceutical role is important to shield them and maintain their biological activity. In this field, silica particles with large pores (LPMS) are innovative supports. Large pores allow for the loading of bioactive molecules inside the structure and contemporarily their stabilization and protection. These purposes cannot be achieved using classical mesoporous silica (MS, pore size 2–5 nm), because their pores are not big enough and pore blocking occurs. LPMSs with different porous structures are synthesized starting from an acidic water solution of tetraethyl orthosilicate reacting with pore agents (Pluronic^® F127 and mesitylene), performing hydrothermal and microwave-assisted reactions. Time and surfactant optimization were performed. Loading tests were conducted using Nisin as a reference molecule (polycyclic antibacterial peptide, with dimensions of 4–6 nm); UV-Vis analyses on loading solutions were performed. For LPMSs, a significantly higher loading efficiency (LE%) was registered. Other analyses (Elemental Analysis, Thermogravimetric Analysis and UV-Vis) confirmed the presence of Nisin in all the structures and its stability when loaded on them. LPMSs showed a lower decrease in specific surface area if compared to MS; in terms of the difference in LE% between samples, it is explained considering the filling of pores for LPMSs, a phenomenon that is not allowed for MSs. Release studies in simulated body fluid highlight, only for LPMSs, a controlled release, considering the longer time scale of release. Scanning Electron Microscopy images acquired before and after release tests shows the LPMSs’ maintenance of the structure, demonstrating strength and mechanical resistance of structures. In conclusion, LPMSs were synthesized, performing time and surfactant optimization. LPMSs showed better loading and releasing properties with respect to classical MS. All collected data confirm a pore blocking for MS and an in-pore loading for LPMS. Full article

Porous polymer gels (PPGs) are characterized by inherent porosity, a predictable structure, and tunable functionality, which makes them promising for the heavy metal ion trap in environmental remediation. However, their real-world application is obstructed by the balance between performance and economy in material preparation. Development of an efficient and cost-effective approach to produce PPGs with task-specific functionality remains a significant challenge. Here, a two-step strategy to fabricate amine-enriched PPGs, NUT-21-TETA (NUT means Nanjing Tech University, TETA indicates triethylenetetramine), is reported for the first time. The NUT-21-TETA was synthesized through a simple nucleophilic substitution using two readily available and low-cost monomers, mesitylene and α, α′-dichloro-p-xylene, followed by the successful post-synthetic amine functionalization. The obtained NUT-21-TETA demonstrates an extremely high Pb²⁺ capacity from aqueous solution. The maximum Pb²⁺ capacity, q_m, assessed by the Langmuir model was as high as 1211 mg/g, which is much higher than most benchmark adsorbents including ZIF-8 (1120 mg/g), FGO (842 mg/g), 732-CR resin (397 mg/g), Zeolite 13X (541 mg/g), and AC (58 mg/g). The NUT-21-TETA can be regenerated easily and recycled five times without a noticeable decrease of adsorption capacity. The excellent Pb²⁺ uptake and perfect reusability, in combination with a low synthesis cost, gives the NUT-21-TETA a strong potential for heavy metal ion removal. Full article

Three new Metal-Organic Frameworks, containing mesitylene tribenzoic acid as a linker and zinc (1) or cadmium as metals (2,3), were synthesized through solvothermal reactions, using DMF/ethanol/water as solvents, at temperatures of 80 °C (structures 1 and 3) and 120 °C (structure 2). Following single-crystal X-ray diffraction, it was found that 1 and 3 crystallize in the P2₁/c and C2/c space groups and form 2D networks, while 2 crystallizes in the Fdd2 space group, forming a 3D network. All three frameworks, upon heating, were found to be stable up to 350 °C. N₂ sorption isotherms revealed that 1 displays a BET area of 906 m²/g. Moreover, the porosity of this framework is still present after five cycles of sorption/desorption, with a reduction of 14% of the BET area, down to 784 m²/g, after the fifth cycle. The CO₂ loading capacity of 1 was found to be 2.9 mmol/g at 0 °C. Full article

High-efficiency production of xylene/trimethylbenzene from benzene/toluene with methanol is a potential way to promote the implementation on the coupled cycle development strategy of petrochemical and coal chemical industry and optimize the resource structure. At the same time, relying on the innovation of catalytic new materials, physical chemistry, intelligent capture technology, process engineering, and other principles and methods, p-xylene (PX) and trimethylbenzene (TMB) with higher added value were prepared by C_6-8~arene methylation, which could elevate the level of methylation field and improve the competitiveness of the industry. This paper focuses on the one-step methylation reaction of benzene with methanol or toluene with methanol to obtain high-purity p-xylene (BM-PX/TM-PX), and the one-step methylation reaction of xylene with methanol to obtain mesitylene (XM-TMB). The methylation reaction mechanism and the preparation strategy of a high-performance catalyst were reviewed. The high selectivity of PX obtained by precisely controlling the pore size and acid site distribution of zeolites was emphasized. Meanwhile, the current research progress of TMB, the kinetic/thermodynamics of the BM-PX/TM-PX, and XM-TMB methylation reaction were described. Based on a literature research and the conclusion of our research group, the mechanism of methylation reaction process was expounded. Finally, the new research direction of catalysts used and reaction process in methylation reaction were prospected in order to guide the rapid development of this field. Full article

Nanocomposite sensors were prepared using carbon soot (CNPs), nickel oxide nanoparticles (NiO-NPs), and cellulose acetate (CA), which was used to detect and study the sensing mechanism of mesitylene vapour at room temperature. Synthesised materials were characterised using high-resolution transmission electron microscopy (HR-TEM), powder x-ray diffraction (PXRD), Raman spectroscopy, and nitrogen sorption at 77 K. Various sensors were prepared using individual nanomaterials (NiO-NPs, CNPs, and CA), binary combinations of the nanomaterials (CNPs-NiO, CNPs-CA, and NiO-CA), and ternary composites (NiO-CNPs-CA). Among all of the prepared and tested sensors, the ternary nanocomposites (NiO-CNPs-CA) were found to be the most sensitive for the detection of mesitylene, with acceptable response recovery times. Fourier-transform infrared (FTIR) spectroscopy coupled with an LCR meter revealed that the mesitylene decomposes into carbon dioxide. Full article

We investigated the kinetics, mechanism and secondary organic aerosols formation of the ozonolysis of trans-2-pentenal (T2P) using four different reactors with Fourier Transform InfraRed (FTIR) spectroscopy and Gas Chromatography (GC) techniques at T = 298 ± 2 K and 760 Torr in dry conditions. The rate coefficients and branching ratios were also evaluated using the canonical variational transition (CVT) state theory coupled with small curvature tunneling (CVT/SCT) in the range 278–350 K. The experimental rate coefficient at 298 K was (1.46 ± 0.17) × 10⁻¹⁸ cm³ molecule⁻¹ s⁻¹, in good agreement with the theoretical rate. The two primary carbonyls formation yields, glyoxal and propanal, were 57 ± 10% and 42 ± 12%, respectively, with OH scavenger compared to 38 ± 8% for glyoxal and 26 ± 5% for propanal without OH scavenger. Acetaldehyde and 2-hydroxypropanal were also identified and quantified with yields of 9 ± 3% and 5 ± 2%, respectively, in the presence of OH scavenger. For the OH production, an upper limit of 24% was estimated using mesitylene as OH tracer. Combining experimental and theoretical findings enabled the establishment of a chemical mechanism. Finally, the SOA formation was observed with mass yields of about 1.5%. This work provides additional information on the effect of the aldehyde functional group on the fragmentation of the primary ozonide. Full article

Low-molecular-weight acid vapors cause aging and destruction in material processing. In this paper, facile fabrication of novel corn-husk-shaped fullerene C₆₀ crystals (CHFCs) through the dynamic liquid–liquid interfacial precipitation method is reported. The CHFCs were grown at the liquid–liquid interface between isopropyl alcohol (IPA) and a saturated solution of C₆₀ in mesitylene under ambient temperature and pressure conditions. The average length, outer diameter, and inner diameter of CHFCs were ca. 2.88 μm, 672 nm, and 473 nm, respectively. X-ray diffraction (XRD) analysis showed the CHFCs exhibit a mixed face-centered cubic (fcc) and hexagonal-close pack (hcp) crystal phases with lattice parameters a = 1.425 nm, V = 2.899 nm³ for fcc phase and a = 2.182 nm, c = 0.936 nm, a/c ratio = 2.33, and V = 3.859 nm³ for hcp phase. The CHFCs possess mesoporous structure as confirmed by transmission electron microscopy (TEM) and nitrogen sorption analysis. The specific surface area and the pore volume were ca. 57.3 m² g⁻¹ and 0.149 cm³ g⁻¹, respectively, are higher than the nonporous pristine fullerene C₆₀. Quartz crystal microbalance (QCM) sensing results show the excellent sensing performance CHFCs sensitive to acetic acid vapors due to the enhanced diffusion via mesoporous architecture and hollow structure of the CHFCs, demonstrating the potential of the material for the development of a new sensor system for aliphatic acid vapors sensing. Full article

The combination of layered double hydroxides (LDH) with graphene oxide (GO) enables the formation of nanohybrids with improved properties. This work focuses on the structural and catalytic properties of Ce-containing MgAl LDH-GO composites bearing different concentrations of GO in the range of 5–25 wt.%. The synthesis of the composites was performed by co-precipitating the LDH phase in the presence of GO, while their characterization was performed using XRF, XRD, DRIFT, Raman, SEM, nitrogen adsorption-desorption, and acidity-basicity measurements. The LDH-GO composites, showing redox, basic, and acid catalytic functions, were tested in two different types of organic transformations: (i) Knoevenagel condensation and (ii) one-pot cascade oxidation-Knoevenagel condensation. (i) The cinnamic acid was synthesized by the Knoevenagel condensation of benzaldehyde with diethylmalonate. The composites showed catalytic performances in strong contrast to neat LDH or GO, suggesting a synergistic interaction between the two components. During Knoevenagel condensation, the catalytic activity increased with the GO content in the hybrids up to 15 wt.% and decreased afterwards. (ii) 2-Benzoyl-3-phenylacrylonitrile was synthesized by the aerobic oxidation of benzyl alcohol followed by the Knoevenagel condensation with benzoyl acetonitrile using three different non-polar solvents, i.e., toluene, benzene, and mesitylene. The conversion of benzyl alcohol was higher for the hybrid materials compared to the individual components but decreased with the increase of the graphene oxide concentration. Full article

Mesitylene was used as a core in seven new tritopic nitrogen containing linkers. Three of the linkers, each containing three nitrile groups, were obtained through Suzuki, Sonogashira and Heck-type coupling reactions. Next, these were converted to tetrazol-5-yl moieties by the cycloaddition of sodium azide to the nitrile functionalities. The last linker, containing three 1,2,3-triazol-4-yl moieties, was synthesized by the Huisgen cycloaddition of phenyl azide to the corresponding alkyne. The latter was obtained via a Corey–Fuchs reaction sequence from the previously reported formyl derivative. As the proof of concept for their potential in MOF design, one of the nitriles was used to build an Ag-based network. Full article

Reactions of divalent metal salts with 4,4-oxybis(N-(pyridine-4-yl)-benzamide), L, and naphthalene-1,4-dicarboxylic acid (1,4-H₂NDC) in various solvents gave [Zn(L)(1,4-NDC)·H₂O]_n, 1, [Cd(L)(1,4-NDC)(H₂O)·MeOH]_n, 2, and [Co(L)(1,4-NDC)(H₂O)_0.5·MeOH]_n, 3, which have been structurally characterized. Complexes 1–3 show eight-fold interpenetrating frameworks with the dia topology, which exhibit porosities substantiated by CO₂ adsorption, whereas 1 and 2 manifest stability in aqueous environments and show high selectivity toward sensing of mesitylene molecules and Fe³⁺ ions with low detection limits and good reusability up to five cycles. Full article