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2015, №2

pp. 4-16

Articles

Improvement of Functionality of Carbonate Macadam via Supercritical Fluid Impregnation with Bituminous Compounds

F.M. Gumerov, M.I. Farakhov, V.F. Khairutdinov, R.F. Gabitov, Z.I. Zaripov, I.Sh. Khabriev, T.R. Akhmetzyanov.

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Key words: propane-butane mixture, supercritical fluid state, deasphaltizate, solubility, carbonate macadam, impregnation

A comprehensive process for deasphaltizing of heavy oil residue and subsequent treatment (impregnation using a solvent in supercritical fluid state) of a carbonate macadam by bituminous compounds (deasphaltizate) is developed. The purpose is to improve its functionality of the material and, above all, to reduce its water absorption capacity. The process parameters are specified based on the newly obtained data on thermal capacity of heavy oil residue and deasphaltizate. The results of the process experimental realization and characteristics of impregnated macadam, including the water absorption capacity decreased from 3.6 to 0.54 %, are presented.

2015, №2

pp. 17-30

Articles

Determination of Natural Aromatic Acids Using Supercritical Fluid Chromatography

D.V. Ovchinnikov, D.S. Kosyakov, N.V. Ul’yanovskii, K.G. Bogolitsyn, D.I. Falev, O.I. Pokrovskiy.

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Key words: supercritical fluid chromatography, SFC, natural aromatic acids

Derivatives of benzoic and cinnamic acids are secondary metabolites of plants, widely spread in nature and possessing biological activity. It is shown that supercritical fluid chromatography (SFC) provides a high performance separation of nine most important representatives of this class of compounds with selectivity, which is dramatically different from the reversed-phase high-performance liquid chromatography. The retention and separation parameters of analytes for four chromatographic stationary phases of different nature are compared and the effect of supercritical fluid parameters and the composition of the mobile phase onto the chromatographic separation are analyzed. The optimum separation can be achieved using a silica-based sorbent with 2-ethylpyridinium linked groups. The proposed approach to determine the above mentioned compounds is based on the combination of chromatographic separation with multiwavelength spectrophotometric detection. It provides the detection limits in the range of 13.0—51.3 mg/L and the duration of analysis about 2.5 min. The developed approach is successfully tested on the analysis of real objects — three different kinds of wine.

2015, №2

pp. 31-39

Articles

Hydrolysis of Aralosides from Aralia Manchurian in Subcritical Water to Oleanolic Acid and its Derivatives

O.V. Filonova, A.V. Lekar, S.N. Borisenko, E.V. Vetrova, E.V. Maksimenko, N.I. Borisenko, V.I. Minkin.

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Key words: subcritical water, aralosides, aralia manchurian, saponins, saparal, oleanolic acid, HPLC-MS

A method to obtain oleanolic acid (OA) and its derivatives by hydrolysis of aralia manchurian in subcritical water is developed. It is carried out on an example of pharmaceutical preparation «Saparal» at 120—240 °C in static regime. A maximal yield of OA is obtained at 210 °C.

2015, №2

pp. 40-50

Articles

Key words: supercritical fluid extraction, microwave radiation, rare earth elements, thorium, uranium, carbon dioxide, monazite concentrate, phosphogypsum, tributyl phosphate, di-(2-ethylhexyl)phosphoric acid

Supercritical fluid extraction (SCFE) using carbon dioxide containing tributyl phosphate (TBP) and di-(2-ethylhexyl)phosphoric acid (D2EHPA) or their adducts with HNO3 is proposed as a method to extract rare earth elements (REE), Th and U from monazite concentrate (MC) and phosphogypsum (PG). On the first stage, the product of baking the MC with Na2CO3 (MCS) is obtained in the presence of coal under microwave irradiation, in which phosphates of REE, Th and U present in the MC are converted into their oxides. Up to 50 % of REE can be recovered from the powdered MCS by the adducts of TBP and D2EHPA with HNO3 in SCFE conditions, whereas Th and U remain in the solid phase. After a complete dissolution of the MCS residue in the mixture of 4 M HCl and 0.05 M HF, Th and U are quantitatively extracted using supercritical carbon dioxide containing D2EHPA and thus separated from the REE that remain in an acidic solution. The conditions of quantitative isolation of REE, Th and U from PG are determined and the schemes for complex processing of MC and PG targeted to the recovery of REE separated from Th and U are suggested.

2015, №2

pp. 51-59

Articles

Key words: supercritical carbon dioxide, SCF-micronization, supercritical antisolvent precipitation, arbidol, bioavailability

The possibility to obtain microparticles of arbidol using supercritical antisolvent (SAS) precipitation method is demonstrated. Non-monotonic dependence of average particle size on arbidol concentration in methanol and DMSO is observed. The position of its minimum depends on the type of used solvent. SAS technique allows one to vary the size (1.8—500 μm) and morphology of arbidol particles which can be operated by process parameters.

2015, №2

pp. 60-70

Articles

Key words: ammonium palmitate, supercritical carbon dioxide, solubility, dynamic regime

The solubility of ammonium palmitate in supercritical carbon dioxide is studied in the dynamic regime at 308.15—333.15 K and 10.0—35.0 MPa. Experimental data are described in the framework of the Peng—Robinson equation of state.

2015, №2

pp. 71-83

Articles

Biodiesel Production in Supercritical Fluid State Using Heterogeneous Catalysts

S.V. Mazanov, A.R. Gabitova, L.H. Miftahova, R.A. Usmanov, F.M. Gumerov, Z.I. Zaripov, V.A. Vasil’ev, E.A. Karalyn.

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Key words: transesterification, heterogeneous catalysts, fatty acids ethyl esters, thermal decomposition, kinematic viscosity

Catalytic and non-catalytic transesterification of rapeseed oil in ethanol at supercritical fluid conditions with exposure to ultrasonic reactive environment are studied at 623— 653 K, 30 MPa and molar «alcohol-to-oil» ratios 12 : 1 and 18 : 1. The effect of heterogeneous catalysts on the reaction rate us revealed. Correlation between the fatty acids ethyl esters content in biodiesel and kinematic viscosity of the reaction product is established.