The possibility of obtaining carbon sorbents from a fine fraction of medium-temperature coke for the removal of phenols from industrial water and wastewater was demonstrated. This excludes the carbonization of coal material as one of the economically costly stages. The resulting samples were tested for the ability to absorb phenol. The phenol content of water after purification with K12 and ShK sorbents decreased from 251.00 to 0.0572 and 0.737 mg/L, respectively.
The research topic is the influence of preliminary ultrasonic treatment of coal tar at ArcelorMittal Temirtau on the individual composition of the products of hydrolytic treatment in the presence of iron-bearing composite catalysts with a carbon carrier (Fe 2 O 3 /C and FeSO 4 /C), within a hydrogen atmosphere. In ultrasound treatment with Fe 2 O 3 /C catalyst, the tetralin content increases to 23.60%, the dihydrophenanthrene content to 1.47%, and the indane content to 2.26%. For FeSO 4 /C catalyst, by contrast, the tetralin content increases to 11.09%, the dihydrophenanthrene content to 1.66%, and the tetrahydrophenanthrene content to 1.27%. Acenaphthylene is almost completely hydrogenated to acenaphthene (2.63%).
Composite materials based on amino-containing humic acids with the introduction of carbon nanotubes, capable of molecular recognition and selective binding of a target metal, were obtained using molecular imprinting, and their composition and physicochemical properties were studied.
Aminophthalide derivatives of cytisine, anabasine, and salsoline were obtained in high yields via condensation of the alkaloids with o-formylbenzoic acid. Their structures were proven using 1H and 13C NMR spectroscopy and data from 2D COSY 1H–1H and HMQC 1H–13C spectra. Studies of their antimicrobial activity showed moderate antimicrobial activity of 3-(N-cytisin-1-yl)isobenzofuran-1(3H)-one and 3-(N-salsolin-1-yl)isobenzofuran-1(3H)-one against Gram-positive test strain Staphylococcus aureus ATCC 6538 and Gram-negative test strain Escherichia coli ATCC 25922.
The paper presents the results of a physicochemical analysis of a coke sample from “Euromet” LLP (Karaganda, Kazakhstan), which is carbonaceous material with high carbon content, the absence of volatiles matter and low ash content. Carbon sorbents were obtained from low-value fractions of carbonized materials of the Karaganda region coke production by the steam-gas activation. An important advantage of using screenings (coke breeze class 0–10 mm, which was crushed and fractionated to a particle size of 2–5 mm.) is the exclusion of the energy-intensive carbonization stage from the technological process, which releases a large amount of environmentally harmful substances (phenols, cresols, gaseous emissions etc.). The optimal conditions for obtaining a sorbent from low-value coke breeze are a temperature of 850 °C and an activation time of 2 hours. The physicochemical properties (ash content, bulk density, sorption capacity for iodine and methylene blue, total pore volume for water) of carbon sorbents were determined.
The article describes the results of studies on the synthesis and structural features of 4-lupinylbenzaldehydes and azomethine derivatives of the lupinine alkaloid. Chemical modification of the lupinine alkaloid was carried out by the halomethylene group in the C-1 position of the quinolysin backbone. The reactions were carried out in several stages. The results of the synthesis of 4-lupinylbenzaldehydes (4-hydroxybenzaldehyde and 4-hydroxy-3-ethoxy-benzaldehyde) synthons in the synthesis of biologically active substances with yields of 67.3% and 74.0%, respectively, are presented. The interaction of 4-lupinylbenzaldehyde with 4-chlorobenzylamine and vinyl ester of monoethanolamine synthesized lupinyl-containing azomethines with yields of 78.4% and 77.4%, respectively. The structure of the obtained compounds was established based on the analysis of the ¹H and 13C NMR spectra, the multiplicity of signals in the 13C NMR spectra was determined from the spectra recorded in the J-modulation mode. The assignment of signals in the spectra was carried out using various modern methods of correlation spectroscopy 1H-1H (COZY), and 1H-13C (HMBC, HSQC). The values of chemical shifts, multiplicity and integral intensity of 1H and 13C signals in one-dimensional NMR spectra are determined. Bioscreening of new 4-lupinylbenzaldehydes and azomethines was carried out, among which substances with high antimicrobial activity were identified. The antimicrobial activity of all the presented samples was studied on reference test microorganisms: facultative anaerobic gram-positive cocci of Staphylococcus aureus ATCC 6538, aerobic gram-positive spore-forming Bacillus subtilis ATCC 6633, gram-negative rods facultative anaerobes of Escherichia coli ATCC 25922 aerobic Pseudomonas aeruginosa ATCC 27853 and yeast fungus Candida albicans ATCC 10231 by diffusion into agar (wells).
Бас редактор: ЖҰРЫНОВ Мұрат Жұрынұлы, химия ғылымдарының докторы, профессор, ҚР ҰҒА академигі, Қазақстан Республикасы Ұлттық ғылым академиясының президенті, АҚ «Д.В.Сокольский атындағы отын, катализ және электрохимия институтының» бас директоры (
We obtained modified humic acid-based cross-linked composite pre-tuned to the sorbed copper ion. The composite synthesis had three stages. At first, we obtained prepolymerization complex using humic acids iso-lated from Shubarkol deposit oxidized coals and multi-walled carbon nanotubes (MWCNTs) with template (CuSO4). We used ultrasonic activation for uniform dispersion of multi-walled carbon nanotubes. Second stage comprised copolymerization in the presence of amine and cross-linker; here the prepolymerization composite complex with the template was fixed in certain nodes of polymer network. At the third stage, acid hydrolysis destroyed the bonds of the template with the composite macromolecules, the template was re-moved, and imprints complementary to the template in shape, size, and functionality were formed and re-tained “molecular memory”. Such tuning forms adsorption centers in the polymer network of the composite, which can repeatedly and highly specifically interact with the template, and highly selectively extract target molecules from solution, leading to significant increase in sorbent capacity. The reaction was controlled by direct and back titration, and added amine, which was determined using Elementar Unicube elemental ana-lyzer. The crosslinked composite can be used as a selective sorbent tuned to a specific metal ion.
The article presents data on the synthesis and study of the structure of thiourea derivatives of functionally substituted pyridines. New thiourea derivatives containing a pharmacologically active pyridine moiety in their structure were obtained. As the starting synton, 2-amino-5-bromopyridine, 2-amino-3-hydroxypyridine and 2-aminomethylpyridine were selected. It was shown that the interaction of 2-amino-5-bromopyridine, 2-amino-3-hydroxypyridine and 2-aminomethylpyridine with ethyl and phenylisothiocyanates in ethanol leads to the formation of the corresponding pyridine-containing thioureas. The synthesis of the initial isothiocyanates was carriedout in situ from the corresponding acidic chlorides (benzoyl chloride and p-brombenzoyl chloride) by heating them with potassium thiocyanate in acetone. The structure of the synthe-sized compounds was studied by 1H and 13C NMR spectroscopy, as well as by the data of two-dimensional spectra of COSY (1H-1H) and HMQC (1H-13C). The values of chemical shifts, multiplicity, and integrated in-tensity of 1H and 13C signals in one-dimensional NMR spectra were determined. Using spectra in the formats COSY (1Н-1Н) and HMQC (1Н-13С), homo-and heteronuclear interactions were established, confirming the structure of the studied compounds.
The article is devoted to the reactions of [2+3] cycloaddition of pyridine-4-aldehyde to fullerene C60, as well as to the preparation of its water-soluble from of the resulting reaction product N-methyl-2-(pyrid-4-yl)-3,4-fulleropyrrolidine. A literature review of organic compounds containing the pyrrolidine cycle was carried out. It is noted that such compounds have a wide spectrum of biological activity and are part of many drugs of both natural and synthetic origin. In this regard, an interesting “pharmacophore” group is the pyridine cycle, which is part of about 5% of all known drugs. The reaction of pyridin-4-aldehyde with fullerene C60 was carried out in the presence of sarcosine under the conditions of the Prato reaction. The reaction mechanism of 1,2-dipolar cycloaddition, leading to fulleropyrrolidine, is described. The water-soluble complex fulleropyrrolidinas with poly-N-vinylpyrrolidone was obtained. The structures of the synthesized compounds were studied by IR, UV, 1H and 13C NMR spectroscopy, as well as by the date of two-dimensional spectra of COSY (1H-1H) and HMQC (1H-13H). The values of chemical shifts, multiplicity and integrated intensity of 1H and 13C NMR signals in one-dimensional NMR spectra were determined. Using spectra in the formats COSY (1H-1H) and HMQC (1H-13C) homo- and heteronuclear interaction were established, confirming the structure of the studied compounds. Key words: fullerene C60, sarcosine, pyridine-4-aldehyde, fulleropyrrolidines, Prato reaction, NMR spectra.
The article presents literature review on the physicochemical and biological properties of fullerene C60, as well as the authors' own experimental data on the synthesis of fullerene derivatives of amines and natural alkaloids. It is shown that the presence of a fullerene fragment in the structure of the compound provides a significant improvement or the appearance of qualitatively new mechanical, chemical, physical, biological and other properties associated with the manifestation of nanoscale factors. The issues of the relationship of the structure, water solubility and biological activity of fullerene С60 derivatives are considered. Many biologically active effects of various modified derivatives of fullerene C60 are described, which have membrane-active, antibacterial, antiviral, immunomodulating, HIV inhibitory enzymes and other properties. It was noted that preparations containing a fullerene fragment are effective against hepatitis C virus, and are also able to efficiently trap free radicals. Derivatives of fullerenes can also be used as antioxidant, neuroprotective and other agents. Particular attention is paid to the authors' own results on the synthesis of amino derivatives of fullerenes.
The article considers data on the in vitro study of new fulleropyrrolidine compounds for anti-inflammatory and cytotoxic activity in cultures of human monocyte cell lines MonoMac-6 and THP-1Blue and also as inhibitors of human neutrophil elastase. This enzyme is a regulator of inflammation. In different situations, it can act both as a pro-inflammatory and as an anti-inflammatory agent. An imbalance in the regulation of elastase activity plays an important role in the pathogenesis of cystic fibrosis, acute respiratory distress syndrome, bronchiectasis, chronic obstructive pulmonary disease, type 2 diabetes mellitus, atherosclerosis and hypertension. In the future, such studies should lead to the creation of optimal in vitro models that most adequately reflect the situation in vivo and establish the relationship between the structure and activity of the studied drugs. It is noted that the presence of lipophilic properties in fullerene C60 derivatives is especially important in the development of pharmaceuticals for the control of pathogens of various infectious diseases. Fullerene C60 derivatives have the ability to easily penetrate lipid membranes, overcome the blood-brain barrier, and modulate ion transport. Compounds were tested for anti-inflammatory and cytotoxic activity (in vitro) on cultures of human monocytic cell lines MonoMac-6 and THP-1Blue. Modified fullerene compounds of various structures were tested for their inhibitory ability against neutrophil elastase enzyme (in vitro). Elastase activity was evaluated by the ability of fulleropyrrolidine compounds to hydrolyze the synthetic substrate N-methylsuccinyl-Ala-Ala-Pro-Val-7-amino-4-me-thylcoumarin (Calbiochem). The results of studies of fullerene compounds in relation to their anti-inflammatory and cytotoxic activity are obtained. The analysis of the fluorescence kinetics of the compounds was carried out. The cytotoxic activity of the samples was investigated in the Brine Schrimp test using Artemia salina. All compounds have cytotoxicity, which suggests a lack of selectivity of chemotherapeutic action. In general, the presence of a cytotoxic effect confirms the reality of antimicrobial action. The results of the study of the antibacterial and antifungal activity of the synthesized new fulleropyrrolidines and their starting substrates are described (S. aureus 505, Bacillus subtilis, Str.agalactiae, E. Coli M-17, Ps.aeruginosa, Candida аlbicans, Penicillium citrinum, Aspergillus niger, Aspergillus flavus, Trichophyton mentagraphytos, Epidermophyton fioccosum). As a result of the study of the potential antifungal activity of the compounds, it was found that only two drugs inhibit the growth of test cultures in vitro. All other studied samples have practically no activity against the yeast fungi Candida albicans. In general, the presence of a cytotoxic effect in the studied fullerene compounds confirms the reality of the antimicrobial action.
The article presents the results of a study of the synthesis of composite materials based on coal waste combined with coal and polymer raw materials, using ultrasonic chemistry methods and determining the possibility of their use as an active mineral additive for replacing part of cement in fine-grained concrete. By varying the composition of the matrix and the filler, a composite material is obtained whose properties are quantitatively and qualitatively different from the properties of each of its components. As a filler in the composition of the composite material, burned rock is used - the product of oxidative self-firing of waste rock, extracted together with coal to the surface. Burned rocks contain an organic part (unburned carbonaceous impurities) and a mineral part (calcined clay-sandy part). Features of the material composition of burned rocks, coal industry waste allows us to consider them as secondary mineral raw materials. The binder in the composite material used is thiourea-formaldehyde resin. The resin was obtained by the standard method of polycondensation of thiourea with formaldehyde at a molar ratio of thiocarbamide:formaldehyde = 1:2. The choice of thiourea-formaldehyde resin is due to the availability, water solubility and the presence of a sufficient number of proton acceptor centers capable of complexation with a modifier. The modifier for composite materials used a coal waste product related to promising natural polymers in nanotechnology, sodium humate, extracted by alkaline extraction from oxidized coal from the Shubarkol deposit. Sodium humate refers to polyfunctional polymers with a unique combination of hydrophobic and hydrophilic sites, a variety of oxygen-containing functional groups, aromatic, heterocyclic and other groups. All this suggests a high ability of sodium humate to intermacromolecular interactions with both the burned rock and thiourea-formaldehyde resin. Composite material based on burned rock, sodium humate with thiourea-formaldehyde resin was synthesized by impregnation using ultrasonic treatment. The decisive role of ultrasonic activation is shown and the effectiveness of its application to the process of producing composites is noted. The modern physicochemical and physicomechanical methods have characterized the composition and structure of the obtained composite materials. The mineralogical composition of composite materials was studied using x-ray phase analysis, and surface morphology based on microscopic analysis using a scanning electron microscope. Filling the composite material with burnt rock provides higher physical and mechanical properties. The strength of burnt-filled composites is higher than that of samples of a similar composition without burnt rock. The resulting composite can be used as a building material. Key words: composite material, filler, binder, burned rock, thiourea-formaldehyde resin.
A nanocomposite material based on humic acid and functionalized multiwalled carbon nanotubes was obtained using ultrasonic treatment. The composition and properties of the nanocomposite were characterized. The applicability of the nanocomposite material as a sorbent for wastewater treatment was demonstrated.
На основе соединения [S-(R*,R*)]-α-[1-(Метиламино)этил]бензолметанола и α-бромциннамальдегида синтезирован соответствующий 1,3-оксазолидин, строение которого доказано методом ЯМРН спектроскопии, а также изучено влияние его на процесс электровосстановления кислорода (ЭВ О) в различных концентрациях. В качестве метода оценки применена катодная вольтамперометрия на ртутно-пленочном электроде, отражающая количество активных форм кислорода нейтрализованных антиоксидантом за определенное время. Показано, что водный раствор (4S,5S)-2-(1’-бром-2’-фенилвинил)-3,4-диметил-5-фенил-1,3-оксазолидин проявляет антиоксидантную активность в широком диапазоне концентраций. Based on the compound [S- (R*,R*)]-α-[1-(Methylamino)ethyl]benzenemethanol and α-bromocinnamaldehyde, the corresponding 1,3-oxazolidine was synthesized, the structure of which was proved by H NMR spectroscopy, and its effect on the process of electroreduction of oxygen (ER O) in various concentrations. Cathodic voltammetry on a mercury-film electrode, reflecting the amount of reactive oxygen species neutralized by an antioxidant for a certain time, was used as an assessment method. It was shown that an aqueous solution of (4S, 5S)-2-(1'-bromo-2'-phenylvinyl)-3,4-dimethyl-5-phenyl-1,3-oxazolidine exhibits antioxidant activity in a wide range of concentrations.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.