Optimal Reaction Conditions Research Articles

Decontamination of Bacterial Spores Using a Bio-reaction System

This report describes the test results of decontamination of Bacillus atrophaeus spores. The spore solution at 109 cfu/mL concentration was treated with chemical decontaminants, hydrogen peroxide, DF-200, sodium dichloroisocyanurate(NaDCC), and perasasfe. DF-200 was not suitable for decontamination of the spore solution. Among them, the optimal decontamination reaction conditions of perasafe and NaDCC were established from test tube experiments in a mL-scale, and they were validated in a bio-reaction system in a L-scale. The optimal conditions of perasafe and NaDCC were 1.0 % of concentration with 5 minutes of reaction time and 0.3 % of concentration with 10 minutes of reaction time, respectively. Also, both decontaminants required adequate agitation for decontamination. The results in the bio-reaction system were similar with the results from the smaller scale using test tubes, showing that the optimal conditions from the smaller scale experiments can be applied to the larger scale.

A novel dual-way inference modeling method for coal coking: Predicting H2 and CH4 concentrations in coke oven gas and inferring optimal reaction conditions

Coal coking is an efficient and environmentally friendly technology for energy utilization that yields various industrial materials. However, the intricate nature of the coal coking reaction poses a challenge for chemical theories to fully capture and derive its reaction process. To address this challenge, a novel dual-way inference modeling method was proposed to simulate the coal coking process. This modeling method not only predicts H2 and CH4 concentrations, but also infers optimal operating conditions based on the desired H2 and CH4 concentrations. In this work, three representative machine learning methods (XGBoost, Random Forest, and ANN) are compared with dual-way inference modeling method, and the key factors affecting H2 and CH4 concentrations are thoroughly explored. The experimental results show that the primary factor influencing CH4 concentration is C, H2 concentration is predominantly affected by fixed carbon, while C plays the most important role for CH4 + H2. The dual-way inference modeling method achieved excellent performance in predicting H2 and CH4 concentrations and operating conditions. In the prediction task of H2, CH4, and H2 + CH4 concentrations, the coefficient of R2 achieved 0.9767, 0.9936, and 0.9851, respectively. The result for predicting coking temperature based on the desired H2 and CH4 concentrations indicate a positive correlation between coking temperature and both H2 and CH4 concentrations. In general, as coking temperature increases, the concentrations of both H2 and CH4 will increase.

One-Pot multicomponent synthesis of novel pyrazole-linked thiazolyl-pyrazolines: Molecular docking and cytotoxicity assessment on breast and lung cancer cell-lines

Cancer remains a foremost cause of mortality globally, with approximately 20 million new cases and nearly 10 million deaths reported in 2022. Lung and breast cancers are particularly prevalent and deadly, underscoring the critical need for novel therapeutic strategies. This study utilized a one-pot, multicomponent reaction (MCR) approach to synthesize a novel series of pyrazole-linked thiazolyl-pyrazolines. The optimal reaction conditions were determined by systematically varying bases, temperatures, reaction times, and solvents. The best yield was achieved using NaOH as the base at 50 °C with 2 h of stirring in ethanol. The synthesized compounds underwent thorough characterization through IR, mass spectrometry, and NMR spectroscopy. Molecular docking studies indicated strong binding affinities to the ErbB4 kinase, suggesting potential utility as kinase inhibitors. Compounds 5E, 5F, and 5G exhibited significant cytotoxicity against breast cancer cell lines, with IC50 values ranging from 15.79±1.272 to 28.38±1.520 µM. Meanwhile, compounds 5A, 5B, 5D, and 5G demonstrated potent effects against lung cancer cell lines, with IC50 values between 7.945±0.99 and 9.295±1.074 µM. Remarkably, compound 5G showed potent efficacy against both breast and lung cancers, with IC50 values of 28.38±1.520 µM and 9.02±1.07 µM, respectively. This study illuminates the critical role of pyrazole-linked thiazolyl-pyrazoline scaffolds in crafting powerful cancer therapeutics targeting ErbB4 (HER4) kinase. Unique in its dual functionality, ErbB4 can act as either an oncogene or a tumor suppressor in lung and breast cancers, contingent on specific cellular contexts and isoform variations. The dynamic expression of ErbB4 intricately modulates tumor growth and patient outcomes, marking it as a compelling therapeutic target for innovative treatments in both breast and lung cancer.

Geometric isomerization of dietary monounsaturated fatty acids by a cis/trans fatty acid isomerase from Pseudomonas putida KT2440

Pseudomonas putida KT2440 encodes a defense system that rigidifies membranes by a cytochrome c-type cis/trans fatty acid isomerase (CTI). Despite its potential as an industrial biocatalyst for directly regulating the geometric isomerism of monounsaturated fatty acids, its original catalytic and structural properties have remained elusive. In this study, the catalytic nature of wild-type CTI purified P. putida KT2440 against dietary monounsaturated fatty acids was investigated. It showed substrate preference for palmitoleic acid (C16:1, cis-Δ9), along with substrate promiscuity with chain length and double bond position (palmitoleic acid>cis-vaccenic acid>oleic acid). Under determined optimum reaction conditions, its catalytic efficiency (kcat/Km) was evaluated as 5.13 × 102 M−1·sec−1 against palmitoleic acid. Furthermore, computational predictions of the protein structure revealed its monoheme cytochrome c-type domain and a parasol-like transmembrane domain, suggesting its catalytic mode of action. For effective cis/trans isomerization, the ethylene double bond of monounsaturated fatty acids should be precisely positioned at the heme center of CTI, indicating that its substrate specificity can be determined by the alkyl chain length and the double bond position of the fatty acid substrates. These findings shed light on the potential of CTI as a promising biocatalyst for the food and lipid industry.

Integrating environmental remediation with biodiesel production from toxic non-edible oil seeds (Croton bonplandianus) using a sustainable phyto-nano catalyst

In the current situation of the environmental uprising toxicology, rising global temperature, and energy-depleting urges to explore and discover more renewable and greener ecological-benefiting energy resources. Biobased renewable fuels generated by using waste products can help in waste management, climate change mitigation, and a low-carbon future. The main objective of this research is to produce environment-friendly and cost-effective biofuel. The potentiality of the novel, toxic, waste, and inedible feedstock Croton bonplandianus was evaluated for biodiesel synthesis through transesterification utilizing a Phyto-nano catalyst of potassium oxide prepared by Croton bonplandianus floral stalk's aqueous extract focusing on waste management. Phyto-nano catalyst characterization was done through innovative tools such as Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), Zeta Potential (ZP), X-Ray Diffraction (XRD), Fourier Transformed Infrared spectroscopy (FTIR), and Diffuse Reflectance Spectroscopy (DRS). The characterization results revealed that the potassium oxide phyto-nanocatalyst possesses an average nanoparticle size of 44.5 nm. This size is optimal for enhanced catalytic activity, indicating significant potential for efficient catalysis. The highest yield (94 %) of biodiesel was secured at optimized reaction conditions of catalyst quantity (0.50 wt%), reaction time (180 min), methanol: oil ratio (9:1), and reaction thermal point (70 °C). Transformation of triglycerides to methyl esters was confirmed by GC/MS, NMR, and FTIR techniques. A total of 21 methyl esters were observed in Croton bonplandianus biodiesel confirmed via GC/MS results. Evaluation of fuel properties was done and matched with international fuel standards. The conclusive remarks for the conducted research are that Croton bonplandianus has a high potential for biodiesel production by applying Phyto-nanocatalysts of potassium oxide while dealing with hazardous environmental conditions and waste management. Phyto nanocatalyst of potassium oxide can be reused and gives the same yield after several cycles of reusability, this reusability of heterogenous Phyto nanocatalyst can reduce to total cost of biodiesel production and can contribute towards circular economy.

Improved Photocatalytic Activity of Dion-Jacobson-Type Tantalate Perovskites Modified with FeCl2.

A rapid and feasible approach was used to develop visible-light-driven-type Dion-Jacobson perovskites by the modification of the RbLaTa2O7 host (RbLTO) with FeCl2 through the molten salt route. X-ray diffraction (XRD) characterization showed that FeCl2-modified layered perovskite (e.g., Fe@RbLTO) preserved its lamellar structure. SEM micrographs confirmed the layered morphology of both RbLTO and Fe@RbLTO perovskite materials. The UV-Vis spectra illustrated a significant red shift of the absorption edge after Fe2+ modification, with the band gap energy reducing from 3.88 to 1.82 eV. H2-TPR measurements emphasized the anchorage of Fe2+ species located on the surface of the layered perovskite as well as in the interlayer space. The synthesized materials were valorized as photocatalysts for the degradation of phenol under both Xe lamp and simulated solar irradiation (SSL) conditions. The photocatalytic reaction follows first-order kinetics. By-product formations during phenol (Ph) degradation were identified and quantified using high-performance liquid chromatography (HPLC). Hydroquinone, 1,2-dihydroxi-benzene, benzoquinone, and pyrogallol were identified as the main Ph degradation intermediates. Pristine RbLaTa2O7 exhibited a phenol conversion value of about 17% using an Xe lamp, while a ≈ 11% conversion was achieved under SSL. A substantial increase in Ph conversion and selectivity was perceived after Fe2+ modification. Fe@RbLTO demonstrated superior photocatalytic performances (43% conversion of phenol under an Xe lamp, and 91% selectivity to aromatic intermediate compounds) at optimized reaction conditions. The stability of the Fe@RbLTO photocatalyst when exposed to an Xe lamp was also assessed. These results suggest that the existence of iron species on the layered perovskite's surface is responsible for the improved redox properties of Fe@RbLTO, resulting in a valuable material for environmental applications.

A high-efficiency and selective fluorescent assay for the detection of tetracyclines

Tetracyclines (TCs) rank second globally in the use of animal infection therapy and animal husbandry as growth promoters among all antibiotics. However, large amounts of TCs residue in food products and more than 75% of TCs are excreted into the environment, causing adverse effects on the ecological system and human health. It has been challenging to simultaneously realize low-cost, rapid, and highly selective detection of TCs. Here, inspired by the fluorogenic reactions between resorcinol and catecholamines, we find the fluorescence quenching ability of tetracycline (TC) and firstly propose a fluorescent “turn-off” detection of TC using dopamine and 4-fluororesorcinol. The optimal reaction condition for the fluorescent assay is investigated and the optimized probe showed a good limit of detection (LOD of 1.7 µM) and a wide linear range (10 µM to 350 µM). Moreover, this fluorescent assay proved to be an effective tool for detecting TC in river, Sprite, and beer samples, which represent the aquatic environments and food and may contain tetracyclines residues. Finally, the high selectivity of the method for TC has been confirmed by eliminating the interference from common substances. The proposed strategy provides a high-efficiency and selective solution for the detection of TCs in environment and food and the application fields of this fluorescent assay could be further expanded in the future.

Preparation of Titanium Dioxide (TiO<sub>2</sub>) from Waste of Polymetallic Ore Processing <i>via</i> Sulfurization Treatment

Various experimental conditions were applied to extract titanium oxide from the waste of polymetallic ore. X-ray diffraction (XRD) analysis confirms that the waste of polymetallic ore contains including various minerals such as almandine (Fe,Mg,Ca)3Al2Si3O12, brownmillerite (FeAlO3(CaO)2), quartz (SiO2), magnetite (Fe3O4). Using H2SO4 acid with a concentration of 93% in the S/L mass ratio of 1:1.5 at 140 °C is suggested as an optimum reaction condition. Its hydrolysis subsequently leads to the formation of the titanyl sulfate (TiOSO4), and relatively pure titanium oxide is obtained through precipitation and calcination at 600 °C. The observed band gap value of 3.2 eV for the obtained TiO2 corresponds to the typical band gap value of anatase-type TiO2. We calculated the crystallite size of extracted anatase-type titanium oxide according to the Debye-Scherrer equation it was determined to be 96.35 nm. Fully reflecting X-ray fluorescence (XRF) determined that the purity of extracted TiO2 is 93.18%. This report presents a newly developed process that enables the production of relatively high-purity TiO2 (93.18%) from the waste of polymetallic ore (TiO2 5.39%) by a simple sulfurization process.

Innovative Recycling and Conversion of Aluminum Waste to Hydrogen and Aluminum Chloride: Enhancing Economic Feasibility and Sustainability in Saudi Arabia

The rapid industrialization and urbanization in Saudi Arabia have led to significant challenges in waste management, particularly in recycling aluminum waste. This study explores an innovative approach for converting aluminum waste, specifically beverage cans, into valuable products such as aluminum chloride (AlCl3) and hydrogen (H2). The process involves the chemical reaction of aluminum with hydrochloric acid (HCl), producing AlCl3 and H2, and is modeled using Aspen Plus software. Two scenarios are evaluated: one without recycling and one incorporating recycling processes. In the first scenario, the direct conversion process yields 355 tons of AlCl3 and 9 tons of H2 per day from 100 metric tons of aluminum waste. The minimum selling price (MSP) of AlCl3 is calculated to be $764 per ton, with an annual profit of $25 million, assuming a market price of $1000 per ton. However, the economic viability of this scenario is highly sensitive to conversion efficiencies and market conditions. The second scenario integrates a recycling loop, processing 90% of the aluminum waste back into aluminum, significantly enhancing economic stability. This scenario produces 35 tons of AlCl3 and 1 ton of H2 per day, with an MSP of $1068 per ton. Despite the higher MSP, the inclusion of recycled aluminum, sold at $2400 per ton, results in a higher annual profit of $38 million, demonstrating greater economic resilience and sustainability. This study provides a comprehensive techno-economic analysis, highlighting the dual benefits of waste reduction and resource recovery. By optimizing reaction conditions and incorporating recycling, the proposed process aligns with Saudi Arabia's Vision 2030 sustainability goals, offering a viable pathway for enhancing economic feasibility and environmental sustainability in aluminum waste management.

Palladium‐N‐heterocyclic Carbene Complexes: Synthesis, Characterization and Catalytic Application of C−H Activation for Carboxaldehyde Derivatives

AbstractA series of palladium‐N‐heterocyclic carbene complexes (2 a‐e) were synthesized from corresponding N‐heterocyclic carbene precursors (1 a‐e) in good yields. The structural analysis of all novel compounds was done by spectroscopic methods and elemental analysis was also performed to evaluate the purity of the complexes. Further confirmations of complexes 2 a‐d were provided by X‐ray crystallography technique. Under optimized reaction conditions, the catalytic activity of the palladium‐N‐heterocyclic carbene complexes was reviewed by direct arylation of furan‐2‐carboxaldehyde and 1‐methylpyrrole‐2‐carboxaldehyde with varied aryl halides. This arylation showed productive and selective reaction at the C5‐position of heteroaryl derivatives.

Nickel Molybdenum Selenide (NiMoSe2) Nanostructures: A Binary Transition Metal Dichalcogenide for Regioselective Synthesis of 2,3,5‐Tri Substituted Pyrrole Derivatives

AbstractBinary transition metal dichalcogenides (BTMDs) have attracted a lot of researchers to exploit their unique properties for different applications in various fields, mainly in energy and environment. Surprisingly, there are no attempts of utilizing BTMDs materials particularly nickel molybdenum selenide (NiMoSe2) as a catalyst support for organic transformations. Reusable catalysts are better alternatives to the transition metal‐free protocols for the synthesis of heterocyclic compounds. Herein, we report a NiMoSe2 BTMD catalyst with Lewis acidic (transition metal) and strongly basic (selenide) sites for the regioselective synthesis of 2,3,5‐tri(het)aryl‐pyrroles from β‐thioxoketone precursors. The present method is capable of giving the expected products in good to excellent yields (up to 80%). Different substituents like ester, cyano, alkyl, trifluoromethyl, methoxy, and halogens have shown tolerance under optimized reaction conditions. The recyclability and reusability of the catalyst was checked for five catalytic cycles without notable loss in reactivity.

Experimental investigation on product and temperature distribution in a continuous flow packed-bed reactor for dodecahydro-N-ethylcarbazole dehydrogenation

The dehydrogenation of dodecahydro-N-ethylcarbazole (H12-NEC) generates enormous gas accompanied by intense heat absorption, affecting heat and mass transfer in porous catalysts. A packed-bed reactor equipped with a temperature measurement device was designed to investigate the continuous flow dehydrogenation of H12-NEC. The effects of weight hourly space velocity (WHSV), reaction temperature, catalyst particle size, and pressure were evaluated. The results reveal that the volume flow rate of hydrogen will increase with the increase of WHSV. And the reduction of gas–liquid ratio and catalyst particle size facilitates heat transfer causing a more uniform axial temperature distribution within the reactor. As the temperature rises, the hydrogen yield increases along with more by-products. 456 K and 2 mm of catalyst particle size are determined to be the optimal reaction conditions in the study, achieving the hydrogen production rate of 9.61 molH2·gPd-1·h-1. With pressure increasing, the hydrogen yield gradually decreases, but the decreased evaporation of H12-NEC results in a smaller temperature difference between the reactor and heating wall. A comparison with the thermodynamic equilibrium model reveals that the effect of pressure on chemical equilibrium may be more significant than the temperature.

Ligand‐Controlled Regioselective Hydroacylation Reactions of Methylenecyclobutanes under Rhodium Catalysis

AbstractIn this study, we report a Rh(I)/dppf catalytic system that can tune the regioselectivity of methylenecyclobutanes. Under the optimal reaction conditions, a series of 1,3‐disubstituted cyclobutanes were prepared in high yields (up to 95%) with excellent regioselectivity (>20:1 r.r.). Scale‐up synthesis of the cyclobutane product at a low catalyst loading (2 mol%) demonstrates the robustness of this dppf‐controlled hydroacylation.

Unveiling Cas12j Trans-Cleavage Activity for CRISPR Diagnostics: Application to miRNA Detection in Lung Cancer Diagnosis.

Cas12j, a hypercompact and efficient Cas protein, has potential for use in CRISPR diagnostics, but has not yet been used because the trans-cleavage activity of Cas12j is veiled. Here, the trans-cleavage behavior of Cas12j1, 2, and 3 variants and evaluate their suitability for nucleic acid detection is unveiled. The target preferences and mismatch specificities of the Cas12j variants are precisely investigated and the optimal Cas12j reaction conditions are determined. As a result, the EXP-J assay for miRNA detection by harnessing the robust trans-cleavage activity of Cas12j on short ssDNA is developed. The EXP-J method demonstrates exceptional detection capabilities for miRNAs, proving that Cas12j can be a pivotal component in molecular diagnostics. Furthermore, the translational potential of the EXP-J assay is validated by detecting oncogenic miRNAs in plasma samples from lung cancer patients. This investigation not only elucidates the trans-cleavage characteristics of Cas12j variants, but also advances the Cas12j-based diagnostic toolkit.

Cerium(III) phosphate as a promising support for gold catalysts addressed to selective oxidation of glucose under base-free conditions

Supported gold nanoparticles are widely used active oxidation catalysts, however, their efficiency and stability vastly depend on the type of supports utilized. This study aims to unravel the potential application of cerium(III) phosphate as a new support for gold catalysts for selective oxidation of glucose under base-free conditions. Particular interest was directed to: i) the identification of the key factors that promote high activity of supported gold species, ii) the optimization of reaction conditions to assess the impact of catalyst loading and reaction time/temperature on the efficiency of glucose oxidation, and iii) the elucidation of the stability of Au/CePO4 catalyst in several reaction cycles. The results show that Au/CePO4 exhibits unique surface properties that enable obtaining of much higher activity of gold species in glucose oxidation compared to other well-known metal oxide-based systems. Precisely, it was found that the TOF value calculated for Au/CePO4 was ca. 2.5 times higher than in the case of Au/CeO2 (TOF = 5846 vs. 2309 h-1, respectively), and ca. 1.5 times higher than that observed for Au/TiO2 (Mintek, TOF = 3839 h-1). The presented results facilitate the development of more active and highly selective supported gold catalysts for oxidation of biomass-derived platform molecules (e.g., glucose).

Efficient Defluoridation of Drinking Water using Mesoporous Magnetic Malachite Nanocomposites

The study evaluated the efficacy of magnetic mesoporous Malachite nanoparticles (NPs) in eliminating fluoride (F−) from drinking water. Screening experiments were conducted to gauge the F− adsorption capabilities of the synthesized material under different Fe3O4 loading conditions. Among the various nanomaterials examined, 0.25-Fe-M demonstrated optimal performance, exhibiting consistent Fe3O4 distribution with a crystal size of 16.66 nm with revealed irregular morphology exhibiting magnetic properties, a surface area of 13.595 m2/g and a pore size of 1.6574 nm. The optimized reaction conditions determined were: 10 minutes of contact time, a NC dose of 0.5 mg/mL, and an F− concentration of 10 mg/L. The maximum adsorption capacities recorded were 6.57 mg/g for Fe3O4 NPs and 7.87 mg/g for malachite NPs. Notably, the optimal adsorption capacity for F− removal was achieved with 0.25 Fe-M-NCs, reaching 8.44 mg/g, demonstrating superior performance compared to other NCs. The interplay between surface area, pore volume, and adsorption is intricate and contingent upon the unique properties of the adsorbent and adsorbate, with specific interactions governing the adsorption process. Furthermore, this study unveiled accelerated adsorption with shorter contact time and high adsorption capacity at the working pH.

Yeast protein‐derived γ‐glutamyl peptides prepared by transpeptidation reaction exhibit a pronounced taste‐enhancing effect

AbstractA high‐salt diet can induce hypertension, so salt reduction can prevent hypertension. γ‐Glutamyl peptides (GGPs) have obvious taste‐enhancing effects, while their contents in natural foods are relatively low. Yeast protein rich in Glu/Gln is a good precursor for the preparation of GGPs. In this study, yeast protein‐derived GGPs were prepared through hydrolysis and transpeptidation reactions, followed by sensory evaluation and E‐tongue analysis. Peptide sequences were identified by LC−MS/MS and screened for molecular docking. The optimal reaction conditions were hydrolysis for 4 h, enzyme concentration of 16 U/g, and transpeptidation for 4 h. GGPs could increase salt and umami intensity by 60.78% and 40.93% based on sensory evaluation, 22.52%, and 16.40% according to E‐tongue analysis. Fifteen γ‐glutamyl peptides with different peptide lengths were selected for molecular docking. Molecular docking confirmed their binding to calcium‐sensing receptors (CaSr) through hydrogen bonds and hydrophobic interaction, while interaction between CaSR receptor and γ‐glutamyl di‐, tri‐, and oligo‐peptides varied in binding energy. The stimulation received by CaSR lasted a longer time and varied in intensity. It was further proved that the flavor of mixed peptides has a layered sense and can give people a rich taste experience. Overall, yeast protein‐derived GGPs can enhance salt and umami taste, which can reduce salt usage without compromising taste.

Evaluation, optimization study, and life cycle assessment of novel eco-friendly PVA-based nanocomposite hydrogel adsorbents for methylene blue and paracetamol removal

In this study, an eco-friendly and novel hydrogel based on a crosslinked polyvinyl alcohol (PVA), iota carrageenan (IC) and polyvinylpyrrolidone (PVP) scaffold, containing a large amount (10–50 wt%) of nanoscale palm fronds (NPF) as additives, for water purification was demonstrated. A life cycle assessment (LCA) findings on NPF as biomass waste incorporated into PVA_PVP_IC polymer matrix was presented, and the results highlight the necessity of focused actions to reduce environmental impact and support the palm waste utilization in a sustainable manner. The multicomponent nanocomposite hydrogels were examined as adsorbents in a system work in batches for methylene blue (MB) and paracetamol (PCT) removal. The results show that, the presence of NPF, which dispersed in the hydrogel PVA_PVP_IC scaffolds containing both covalent and non-covalent cross-linking bonds, greatly enhanced the MB and PCT adsorption efficiency. A response surface methodology (RSM) model was used to find the best operating parameters of contaminant adsorption, including time, adsorbent dose, and starting concentration of pollutants. By using this statistical model, it was found that the optimal conditions for the adsorption reaction to achieve the complete removal of MB are 66.7 h adsorption time duration, 98.5 mg L−1 starting concentration, and an adsorbent dose of 5.9 mg, while for the complete removal of PCT, it is 57.6 h adsorption time duration, 80 mg L−1 starting concentration, and an adsorbent dose of 6 mg. The reusability of the nanocomposite hydrogels were tested for 5 cycles, all showed high adsorption capacity, indicating the potential for practical application of this nanocomposite hydrogel system. This study indicates that the prepared nanocomposite hydrogel raises the standard used for treatment of wastewater and also gives a solution to protect the environment and mitigate global warming.

Tetrabutylammonium Hydrogen Sulfate (TBAHS) Catalyzed Microwave-Assisted Synthesis of 3,4,5,6,7,9-Hexahydro-1H-xanthene-1,8-(2H)-dione Derivatives and its Biological Study

In this study, a facile and eco-friendly synthesis of novel 3,4,5,6,7,9-hexahydro-1H-xanthene-1,8(2H)-dione derivatives using tetrabutylammonium hydrogen sulfate (TBAHS) as a catalyst in the microwave reactor is presented. The reaction involved the condensation of aromatic aldehydes with 1,3-cyclohexanedione in ethanol as solvent, offering significant advantages in terms of reaction rate, yield and purity. The use of TBAHS as catalyst in conjunction with microwave irradiation facilitated the formation of the target xanthene derivatives in remarkably short reaction times. Moreover, Monowave 50 microwave reactor provided precise control over reaction parameters, enabling rapid optimization of reaction conditions. Further these synthesized compounds were systematically evaluated for their antibacterial, antituberculosis and antioxidant activities.

Diimide-Mediated Hydrogenation of Nitrile Butadiene Rubber

The hydrogenation of nitrile butadiene rubber (NBR) has shown great potential for improving its physical, thermal, mechanical, and chemical stability. Hydrogenation process of NBR in this work involved the utilization of diimide produced from the interaction between hydrazine hydrate (N2H4) and hydrogen peroxide (H2O2), with the addition of boric acid as a promoter. Attenuated total reflectance Fourier transform infrared (ATR-FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) were used to evaluate the degree of hydrogenation, glass transition, thermal stability, and rubber crystallinity, respectively. The highest hydrogenation degree was 99%, which resulted in a 57% gel content. Upon hydrogenation, both the glass transition temperature (Tg) and decomposition temperature (Td) increased. The hydrogenated rubber samples generally showed an amorphous state, except for the 99% hydrogenated sample, which displayed a semi-crystalline state. However, using diimide for direct hydrogenation yields a side reaction from the free radicals in the system, which leads to gel formation. Optimization was accomplished by employing the response surface methodology (RSM), which entailed manipulating parameters such as the total solid content (TSC) of NBR, reaction time, and the mole ratio of H2O2 to N2H4, to reduce the percentage of gel content. The RSM analysis identified the optimum reaction conditions as a 1:1 mole ratio of H2O2: N2H4 and 25% TSC, with a reaction time of 8 h, which yielded 32% gel content percentage, where a mole ratio of H2O2 to N2H4 and reaction time indicated a synergistic effect, whereas TSC denoted an antagonistic effect.