Fine Chemical Technologies最新文献

{"title":"One-pot determination of amino acids in drugs by pre-column derivatization with phenyl isothiocyanate","authors":"P. A. Kalmykov, T. P. Kustova, S. O. Kustov, P. S. Shestakovskaya, T. R. Azmetov, A. A. Kalmykova","doi":"10.32362/2410-6593-2024-19-2-127-138","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-2-127-138","url":null,"abstract":"Objectives. To develop a new method to determine amino acids in drugs by means of reverse-phase high-performance chromatography (RP HPLC) with pre-column derivatization using phenyl isothiocyanate (PITC) and one-pot sample preparation.Methods. The initial standard solutions of amino acids were prepared by weighing, followed by dissolution in water. Working solutions were then prepared: standard, test, and blank, by dilution in 20 mM hydrochloric acid. Further sample preparation was carried out in Safe-lock polypropylene tubes (Eppendorf) in a reaction buff containing mobile phase A, acetonitrile, and triethylamine in a ratio of 85 : 10 : 5, labeled with a 5% PITC solution in acetonitrile. After thorough mixing for 3–5 min on a vortex, the tubes were kept in a solid-state thermostat with a thermally insulating lid for 2 h. The samples were then cooled for 10 min, centrifuged for 1 min at 13000 rpm, the supernatant was transferred into vials, and the mixture of amino acids was separated by RP HPLC using hydrophobic silica gel with grafted C18 groups as a stationary phase. The quantitative determination of amino acid derivatives was carried out using a diode array detector.Results. A new method for the separation and determination of amino acids in medicinal preparations was developed and validated. Simple one-pot sample preparation using available reagents and equipment enabled studies to be carried out without using commercial kits, for example, the AccQ.Tag Ultra Derivatization Kit, USA. Using the analysis of mixtures of histidine and glycine as an example, it was shown that when using two mobile phases, an acceptable separation of amino acid derivatives in a gradient mode can be achieved for 20 min at a flow rate of 1.0 mL/min. The samples prepared according to the new method demonstrated a high level of stability in use and storage. A composition of mobile phases A and B consisting of 10 mM acetate buffer pH 3.5 and 80% acetonitrile solution was proposed. Validation of the method hereby developed in the analysis of the drug Innonafactor®, containing glycine and histidine as excipients, demonstrated high convergence of the results of the quantitative determination of these amino acids.Conclusions. The new method to determine amino acids in medicinal preparations by RP HPLC with PITC pre-column derivatization has a wide range of applications, has a number of advantages when compared to imported commercial kits for the determination of amino acids. These include: lower cost of reagents and materials, high accuracy and repeatability. Thus, it can be recommended for use in quality control laboratories of pharmaceutical enterprises.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141013764","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A study of the mechanical and thermophysical properties of crystal matrices for the immobilization of high-level wastes","authors":"I. V. Kuznetsov, A. Y. Zobkova, M. Kalenova, A. S. Shchepin, O. N. Budin, V. A. Stepanov, I. M. Melnikova, O. I. Stefanovskaya, K. V. Klemazov","doi":"10.32362/2410-6593-2024-19-2-149-162","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-2-149-162","url":null,"abstract":"Objectives. The aim of the study was to confirm the compliance of the mechanical and thermophysical properties of titanate-zirconate mineral-like matrices intended for immobilization of the rare-earth-actinide fraction of high-level waste (HLW) with pyrochlore structures (Nd2ZrTiO7) and orthorhombic titanate of rare earth elements (Nd4Ti9O24+TiO2) with the Russian requirements for the final forms of radioactive waste sent for disposal. With regard to fractionated radioactive waste, this type of matrix is preferable when compared with conservative aluminophosphate and borosilicate glasses. This is due to larger capacity, and a better level of chemical, thermal, and radiation resistance.Methods. The synthesis of mineral-like matrices was carried out by remelting a granular precursor consisting of mineral-forming metal oxides and a solution imitating the rare earth-actinide fraction of HLW in an induction furnace with a cold crucible. The thermal diffusivity was determined by the laser flash method. The heat capacity of the matrix samples was measured by differential scanning calorimetry. Ultimate flexural and compressive strengths were determined using universal test machines. The elastic moduli (Young’s) were measured by the acoustic method. The temperature coefficients of linear expansion were determined using a high-temperature dilatometer.Results. The ultimate strength of the matrices (Nd2ZrTiO7) and (Nd4Ti9O24+TiO2) was found to be 150–179 and 20.6–57.8 MPa in compression and bending respectively. Young’s moduli vary from 3.7 ∙ 107 to 2.15 ∙ 108 kN/m2. With an increase in temperature from 50 to 500°C, the values of thermal conductivity have a pronounced tendency to decrease from 1.71 to 0.91 W/(m∙K). The temperature coefficients of linear expansion increase from 6.96 ∙ 10−6 to 1.01 ∙ 10−5 K−1 in the same temperature range.Conclusions. Comprehensive studies of titanate-zirconate mineral-like matrices show that their mechanical and thermal properties in certain cases significantly exceed the minimum requirements of regulatory documentation for the final forms of HLW.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141014490","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Natural and synthetic isoprene rubbers obtained using Ziegler–Natta catalysts","authors":"A. A. Zuev, V. L. Zolotarev, I. P. Levenberg, L. A. Kovaleva, I. S. Nasyrov","doi":"10.32362/2410-6593-2024-19-2-139-148","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-2-139-148","url":null,"abstract":"Objectives. To compare the properties of rubber compounds and rubbers based on natural rubber RSS1 and synthetic isoprene rubbers obtained using Ti, Nd, Gd catalysts, both when used individually in the formulation of rubber compounds and when synthetic analogues partially replace natural rubber.Methods. Rubber compounds were prepared using a laboratory roll and a 100 cm3 rubber mixer. For rubber compounds, the following factors were determined: Mooney viscosity, cohesive strength, and vulcanization characteristics. For rubbers, the following factors were determined: physical and mechanical parameters, Shore A hardness, rebound resilience, and volume loss upon abrasion.Results. Based on the results of the rubber compound tests, the study showed that compounds based on all the synthetic polyisoprenes studied are significantly inferior to compounds based on natural rubber in terms of cohesive strength. The partial replacement of natural rubber with synthetic rubber (regardless of the type of catalytic system) leads to a significant decrease in the cohesive strength of the blends. Despite the differences observed in the properties of the rubber compounds, the results of the rubbers based on individual rubbers do not manifest significant differences.Conclusions. The study demonstrated the influence of defects (oligomers, gel, low molecular weight fractions, branches, and 3,4-units) in the structure of synthetic polyisoprenes on the cohesive strength index of rubber compounds based on them, in which the number of 3,4-units plays a decisive role. The study also showed the potential of studying synthetic polyisoprenes as analogues of natural rubber in formulations of rubber compounds in the aims of resolving the problem of import substitution in the tire and rubber goods industry.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141013747","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Dichlorocarbenation of polar olefins in conditions of microwave irradiation","authors":"Y. Borisova, A. I. Musin, R. Sultanova, S. S. Zlotskii","doi":"10.32362/2410-6593-2024-19-2-104-110","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-2-104-110","url":null,"abstract":"Objectives. To evaluate the influence and efficiency of using microwave irradiation on the dichlorocarbenation of polar olefins. To determine the conditions (reaction time and process temperature) under which the maximum yield of target gem-dichlorocyclopropanes is achieved.Methods. The target compounds were obtained by classical methods of organic synthesis— acetalization of polyols and dichlorocarbenation of unsaturated compounds. The preparation of gem-dichlorocyclopropanes was carried out using the microwave activation method on a Sineo device (microwave system for organic synthesis, made in China). In order to determine the qualitative and quantitative composition of the reaction masses, gas–liquid chromatography (using the Kristall 2000 hardware complex), mass-spectroscopy (using Chromatek-Kristall 5000M device with NIST 2012), and nuclear magnetic resonance spectroscopy (using Bruker AM-500 device with operating frequencies of 500 and 125 MHz) were carried out.Results. Under microwave irradiation at 25°C for 2 h with the maximum yield (92–98%), the target substituted gem-dichlorocyclopropanes were obtained: 2-(2,2-dichloro-3-methylcyclopropyl)-1,3-dioxolane, 2-(2, 2-dichloro-3-phenylcyclopropyl)-1,3-dioxolane, 8,8-dichloro4-isopropyl-3,5-dioxabicyclooctane, diethyl-2,2-dichloro-3-phenylcyclopropane-1,1-dicarboxylate, and diethyl-2,2-dichloro-3isopropylcyclopropane-1,1-dicarboxylate.Conclusions. Under the conditions herein proposed, the use of the microwave stimulation method in the dichlorocarbenation of double C=C bonds containing polar substituents allows the reduce the temperature and reaction time to be significantly reduced, and the yield of target gem-dichlorocyclopropanes to be increased.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141016689","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Preparation of fine suspensions using stirred media bead mill","authors":"L. S. Elinevskaya, D. V. Dzardanov, O. V. Ulybina, R. N. Ivanov","doi":"10.32362/2410-6593-2024-19-2-95-103","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-2-95-103","url":null,"abstract":"Objectives. To determine the change patterns for the main physical properties of suspensions after their grinding in bead mills, with the prospect of optimizing the preparation technology and extending the results obtained to other dispersed phases.Methods. The study used the Fraunhofer laser diffraction method to determine particle size. The obtained data on the particle size distribution of suspensions were qualitatively verified by optical microscopy. The Brookfield relative viscosity method was used to evaluate the rheological properties of the resulting suspensions. The density of the resulting suspensions was measured by the hanging method using a calibrated pycnometer.Results. The dependencies of the change in the particle size distribution after grinding in a bead mill were established. The viscosity of the suspensions was observed to increase following grinding. Common regularities of changes in the density of the considered suspensions were established.Conclusions. The conducted studies showed that the physical and mechanical properties of suspensions are affected by the type and the filling ratio of the grinding media; the residence time of the suspension in the grinding chamber; the number of grinding operations; mill designs.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141017202","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis and application of chromium complexes based on 4,5-bis(diphenylphosphanyl)-H-1,2,3-triazole ligands to obtain higher С10–С18 olefins","authors":"A. A. Senin, K. B. Polyanskii, A. M. Sheloumov, V. V. Afanasiev, T. M. Yumasheva, K. B. Rudyak, S. V. Vorobyev","doi":"10.32362/2410-6593-2024-19-1-39-51","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-1-39-51","url":null,"abstract":"Objectives. To synthesize 4,5-bis(diphenylphosphanyl)-H-1,2,3-triazole ligands and new chromium complexes based on them, in order to obtain a fraction of higher C10–C18 alpha-olefins from ethylene.Methods. The Schlenk technique was used to obtain the target chromium complexes. Diphenylphosphanyl triazole ligands can be characterized by nuclear magnetic resonance spectroscopy. The composition of the final products was confirmed by elemental analysis. The liquid phase of the oligomerization reaction was studied by gas chromatography.Results. L1–L9 ligands were obtained, and K1–K9 chromium complexes were synthesized based on the correspondent ligands using commercially available chromium (III) trichloride tris(tetrahydrofuran). The K1–K9 complexes thus obtained were tested in the process of ethylene oligomerization.Conclusions. Chromium complexes based on 4,5-bis(diphenylphosphanyl)-H-1,2,3-triazoles K1–K9 were produced in high yields using the Schlenk technique. It was found that systems based on the K4–K7 and K9 complexes enable the ethylene oligomerization process to be carried out with a sufficiently high level of productivity. It was shown that the introduction of a dialkyl zinc derivative increases the performance and selectivity of the catalytic system for the target fraction.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140082257","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis of copolymers based on divinylbenzene and dibenzocyclobutyldimethylsilane and a study of their functional characteristics","authors":"A. V. Lobanova, K. S. Levchenko, G. E. Adamov, P. S. Smelin, E. P. Grebennikov, А. D. Kirilin","doi":"10.32362/2410-6593-2024-19-1-52-60","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-1-52-60","url":null,"abstract":"Objectives. To create new polymer materials based on organosilicon derivatives of benzocyclobutene and to study the possibility of their use as insulating dielectric layers in micro- and microwave electronics devices.Methods. The synthesis of the dibenzocyclobutyldimethylsilane (diBCB-DMS) monomer was carried out from 4-brombenzocyclobutene through the production stage of the Grignard reagent. Copolymers based on divinylbenzene and dibenzocyclobutyldimethylsilane were obtained by means of thermal polymerization. The properties and structure of the copolymers thus obtained were studied using the following methods: thermogravimetric analysis, infrared spectroscopy, nuclear magnetic resonance (NMR), mass spectroscopy, and by means of high-frequency measurements of volt-ampere characteristics and volumetric resonator.Results. diBCB-DMS was synthesized with a yield of 81.5%. The composition and structure were confirmed by 1H and 13C NMR spectroscopy. The dielectric constant of the diBCB-DMS homopolymer is ~2.6. The tangent of the dielectric loss angle at 1 GHz of the diBCB-DMS homopolymer is 2.3∙10−4. The tangent of the dielectric loss angle at 10 GHz of the diBCB-DMS homopolymer is 2.6∙10−4. The study of divinylbenzene and diBCB-DMS copolymers in different molar ratios on a thermogravimetric analyzer showed that the copolymers are able to withstand temperatures up to 470°C. The dielectric permittivity of diBCB-DMS and divinylbenzene copolymers in a molar ratio of 1 : 1 was 2.6. The values of the loss tangent at 1 and 10 GHz of copolymers in a molar ratio of 1 : 1 were 4.0∙10−4 and 5.6∙10−4, respectively.Conclusion. Analysis of the obtained results shows that the samples of the diBCB-DMS homopolymer have the same dielectric characteristics as the samples based on diBCB-DMS and divinylbenzene, therefore, the introduction of divinylbenzene into the polymer structure does not worsen the dielectric parameters and such polimer materials can be used at high temperatures.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140082731","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Sorption of picolinic acid by Cu(II)-containing sulfocationite KU-2-8","authors":"H. Altshuler, V. N. Nekrasov, S. Lyrshchikov, O. Altshuler","doi":"10.32362/2410-6593-2024-19-1-7-16","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-1-7-16","url":null,"abstract":"Objectives. To study the equilibrium distribution of components between KU-2-8 sulfocationite and an aqueous solution containing picolinic acid and Cu(II); to show the possibility of immobilization of cations of picolinic acid and Cu2+ in sulfonic cation exchanger KU-2-8; to calculate the component compositions of the equilibrium solution, in order to obtain the required ionic composition of the KU-2-8 sulfonic cation exchanger according to the selectivity coefficients of binary ion exchange, and the constants of formation of such complexes in water.Methods. The concentrations of the individual components in multicomponent solutions were calculated using the HySS 2009 program (Hyperquad Simulaton and Speciation). The calculation of the equilibrium ionic compositions of KU-2-8 sulfocationite was performed using the selectivity coefficients of binary ion exchanges and the formation constants of complexes of picolinic acid with Cu2+ and H+ cations. Experimental study of the equilibrium distribution of components between aqueous solutions of picolinic acid, copper nitrate, and KU-2-8 sulfocationite was carried out by means of the dynamic method at a temperature of 298 K. Fourier-transform infrared spectroscopy and electron paramagnetic resonance spectroscopy were used, in order to determine the ionic forms of the components contained in the sulfocationite.Results. It was shown that the equilibrium solution contains H+ protons, Cu2+ cations, LH picolinic acid molecules, protonated picolinic acid cations [H2L]+, deprotonated picolinic acid anions L-, Cu2+ complexes with the deprotonated picolinic acid anion [CuL]+, and Cu2+ complexes with two anions of deprotonated picolinic acid [CuL2]. The concentration of H+, Cu2+, and [H2L]+ cations in the solution significantly exceeds the concentration of other components at pH values from 0 to 0.5. The content of [CuL]+ cations and neutral complexes [CuL2] increases significantly in the solution, while the [H2L]+ cations disappear at pH greater than 1. It was experimentally established that the concentrations of picolinic acid and copper in the polymer phase are many times higher than the concentrations of these components in an aqueous solution. The partition coefficients are about 24 and 210 for picolinic acid and Cu(II), respectively. The calculated dependencies of the concentrations of Cu2+, [H2L]+, H+, [CuL]+ cations in the polymer vs pH of an equilibrium solution containing picolinic acid were obtained. The experimental data on the concentrations of all cations in the ion exchanger is in the intervals of the calculated compositions within the limits of measurement errors.Conclusions. KU-2-8 sulfocationite is proposed as a container for obtaining drugs based on picolinic acid and Cu2+ cations. It was shown that the selectivity coefficients of binary ion exchanges and the formation constants of [H2L]+, [CuL]+ complexes can be used to precalculate the ionic compositions of the equilibrium solution, in order t","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140081732","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Kinetic regularities of neopentyl glycol esterification with acetic and 2-ethylhexanoic acids","authors":"D. S. Chicheva, E. L. Krasnykh, V. A. Shakun","doi":"10.32362/2410-6593-2024-19-1-28-38","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-1-28-38","url":null,"abstract":"Objectives. Development of a domestic technology for producing environmentally friendly non-phthalate plasticizers, lubricants and transformer fluids based on neopentyl glycol (NPG), an oxo-synthesis product.Methods. The methodology of the work was to study the kinetic laws of NPG esterification with acetic and 2-ethylhexanoic acids under self-catalysis conditions with an 8-fold molar excess of monocarboxylic acids. The production of NPG esters was carried out by azeotropic esterification in the presence of solvents—benzene and m-xylene. The resulting diesters were isolated from the reaction mass by vacuum rectification. The purity of the obtained NPG diesters was no less than 99.7 wt %. Analysis of the qualitative and quantitative composition of reaction samples was carried out using infrared spectroscopy, gas chromatography–mass spectrometry and gas–liquid chromatography.Results. The paper presents the results of kinetic studies on NPG esterification of with acetic and 2-ethylhexanoic acids. It compares the reaction rates and reactivity of the acids used. Under the given conditions, NPG diesters were produced, and some of their physicochemical properties were determined. This enabled the data obtained to be used for the development of industrial technology in the production of NPG diesters.Conclusions. It was established that with an eightfold molar excess of acid under self-catalysis conditions, a yield of NPG diacetate equal to 95% is achieved within 20–22 h at an optimal process temperature of 100–110℃; NPG di(2-ethylhexanoate)—within 26–28 h at 160–170℃. The activation energies and pre-exponential factors for the formation of NPG mono- and diesters with acetic and 2-ethylhexanoic acids were established. The paper presents the kinetic models of esterification.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140081924","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Effect of glucose–citric acid deep eutectic solvent on the vapor–liquid equilibrium of an aqueous ethanol solution","authors":"A. Klinov, A. Khairullina","doi":"10.32362/2410-6593-2024-19-1-17-27","DOIUrl":"https://doi.org/10.32362/2410-6593-2024-19-1-17-27","url":null,"abstract":"Objectives. To study the effect of a deep eutectic solvent (DES) based on glucose and citric acid on the vapor–liquid equilibrium of an aqueous solution of ethanol.Methods. A qualitative and quantitative analysis of the conditions of vapor–liquid equilibrium in an ethanol–water–DES ternary mixture was performed based on the open evaporation method and the measurement of TPxy data using a Świętosławski ebulliometer. Since the volatility of the DES is negligible in comparison with that of water and ethanol, the composition of the vapor phase was measured by means of Karl Fischer titration. The conditions of vapor–liquid phase equilibrium were modeled using the UNIFAC model.Results. The open evaporation method was used to determine the curves of residual concentrations for the ethanol–water–DES mixture at various DES concentrations and compositions (glucose–citric acid ratios). TPxy data was obtained for the mixture produced by adding 30 wt % DES to an aqueous solution of ethanol at atmospheric pressure. Studies show that DES based on glucose and citric acid has a significant effect on the relative volatility of ethanol in aqueous solution, leading to the disappearance of the azeotropic point. This effect is due to only the presence of glucose. Citric acid does not change the composition of the equilibrium phases, but rather increases the solubility of glucose in aqueous ethanol solutions. This is especially important at high ethanol concentrations, since glucose is poorly soluble in ethanol.Conclusions. Addition of DES based on glucose and citric acid to an aqueous solution of ethanol leads to the disappearance of the azeotropic point. DES can thus be considered as a promising entrainer for extracting ethanol from aqueous solutions using extractive distillation. Modeling of the conditions of vapor–liquid equilibrium in the ethanol–water–DES system using the UNIFAC model showed a satisfactory level of accuracy. The error in the calculated data increases with increasing the glucose concentration, while remaining acceptable for practical use.","PeriodicalId":12215,"journal":{"name":"Fine Chemical Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140082025","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}