Supercritical Fluid Technologies Laboratory

• Preparative separation processes using supercritical fluids and liquefied gases, namely extraction, selective adsorption, chromatography, selective crystallization.
• The development of methods for the synthesis of dispersed materials, including one — and two-dimensional ones, using liquefied gases and supercritical fluids.
• The research into regularities of physical and chemical processes in supercritical fluids, i.e., solubility of substances in single-and multicomponent fluids, crystallization thermodynamics, and adsorption of substances from sub-and supercritical fluids, reactions involving supercritical fluids.
• The design and diagnostics of polymer materials formed in supercritical fluids.

• A new method for measuring the solubility of substances in multicomponent sub — and supercritical fluids has been developed, based on the at-line combination of supercritical antisolvent deposition and supercritical fluid chromatography. The method is characterized both by higher expressiveness compared to standard dynamic methods for measuring the solubility of substances in media with high isothermal compressibility, and low amounts of target substances used. It is suitable for simultaneous measurement of the solubility of several compounds in the solution.
• The influence of mobile phase parameters in supercritical fluid chromatography (SFC) on the separation selectivity of structurally close compounds has been described.
• The pressure and temperature of the supercritical fluid have been shown to have a negligible effect on the separation selectivity of polar substances using the supercritical fluid chromatography method.
• The possibility of implementing the polar ionic mode of enantiomer separation in SFC using glycopeptide chiral selectors has been demonstrated. A number of specific effects of the influence of mobile phase parameters on selectivity, not previously described for the SFC method, have been found, i.e. the dependence of the elution order of polyethylene glycol oligomers on the flow rate of the mobile phase, the inversion of the elution order of various structurally similar substances with small variations in the proportion of the co-solvent in the mobile phase, the separate cation and anion elution of ammonium salts, using amines as modifiers.
• The method for producing composites based on polymers and carbon nanotubes by the SAS method has first been developed. The composite materials obtained by the SAS method (Fig. 2) have exceed the composites obtained by the solution method in strength by 40 – 50%, in relative elongation by 2 – 3.75 times. Thus, the addition of carbon nanotubes to the polymer matrix leads to the simultaneous increase in both strength and ductility with an almost constant Young’s modulus.
• A technology to produce the medication «Salbutamol» based on enantiomeric pure micronized substance obtained using supercritical fluid technologies (a joint project with the Altai State University and the pharmaceutical company «Altayvitaminy») has been created.

Scientific and organizational projects of the laboratory staff:

• Arrangement and holding of a series of conferences «Supercritical fluids: fundamentals, technologies, innovations».
• Publication of the scientific journal «Supercritical fluids: theory and practice»

1. Anton M. Vorobey Junior Researcher
2. Aleksey E. Lazhko Junior Researcher
3. Mikhail O. Kostenko Junior Researcher
4. Konstantin B. Ustinovich Head Technologist

1. A.M. Vorobei, O.I. Pokrovskiy, K.B. Ustinovich, O.O. Parenago, S.V. Savilov, V.V. Lunin, V.M. Novotortsev. Preparation of polymer – multi-walled carbon nanotube composites with enhanced mechanical properties using supercritical antisolvent precipitation // Polymer. V. 95, 2016. DOI: 10.1016/j.polymer.2016.04.059
2. A.M. Vorobei, O.I. Pokrovskiy, K.B. Ustinovich, O.O. Parenago, V.V. Lunin. A method for measuring solubility in multi-component sub- and supercritical fluids using an online hyphenation of supercritical antisolvent precipitation and supercritical fluid chromatography // J. Mol. Liq. V. 280, 2019. DOI: 10.1016/j.molliq.2019.02.056
3. P.M. Kalachikova, A.E. Goldt, E.M. Khabushev, T.V. Eremin, K.B. Ustinovich, A. Grebenko, O.O. Parenago, T.S. Zatsepin, O.I. Pokrovskiy, E.D. Obraztsova, A.G. Nasibulin. Direct injection of SWCNTs into liquid after supercritical nitrogen treatment // Carbon. V. 152, 2019. DOI: 10.1016/j.carbon.2019.06.003
4. S.Z. Vatsadze, A.V. Medved’ko, S.A. Kurzeev, O.I. Pokrovksiy, O.O. Parenago, M.O. Kostenko, I.V. Ananyev, K.A. Lyssenko, D.A. Lemenovsky, G.M. Kazankov, V.V. Lunin. Stereocontrol in preparation of cyclopalladated alkylaromatic oximes and evaluation of their stereoselective esterase type catalytic activity // Organometallics. V. 36 (16), 2017. DOI: 10.1021/acs.organomet.7b00410
5. R.D. Oparin, M.A. Krestyaninov, E.A. Vorobyev, O.I. Pokrovskiy, O.O. Parenago, M.G. Kiselev. An insight into possibility of chemical reaction between dense carbon dioxide and methanol // J. Mol. Liq. V. 239, 2017. DOI: 10.1016/j.molliq.2016.12.027
6. K.B. Ustinovich, V.V. Ivanov, Y.M. Tokunov, A.A. Loshkarev, N.I. Sapronova, A.M. Vorobei, O.O. Parenago, M.G. Kiselev. Study of Dispersions of Carbon Nanotubes Modified by the Method of Rapid Expansion of Supercritical Suspensions // Molecules. V. 25, 4061, 2020. DOI: 10.3390/molecules25184061

Grants of the Russian Foundation for Basic Research

• 18-29-06071 – Parenago O. O. «Formation of nanostructured materials using supercritical fluid dispersion and exfoliation technologies».
• 17-03-01134 – Pokrovsky O. I. «The influence of the supercritical antisolvent deposition process parameters on the size and morphology of the particles obtained».
• 17-53-40020 – Parenago O. O. «New approaches to the selective isolation of biologically active substances from plant product»
• 13-03-12270 – Parenago O. O.»Supercritical fluid microencapsulation as the basis for the creation of prolonged-action medication».

Grants of the Russian Science Foundation

17-73-20377– Pokrovsky O. I. «Selectivity control in supercritical fluid technologies for mixture separation of substances to isolate pharmaceutical and food ingredients».