Supercritical fluid reverse micelle systems

Compositions – Inorganic luminescent compositions – Tungsten containing

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252312, 252314, 25218311, 240643, 240656, B01J 1300, B01D 1700, C02F 128

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051587041

DESCRIPTION:

BRIEF SUMMARY
ritical fluid have very low solubility in the media to be extracted, and the large density difference between these systems and the liquid or solid phases. Other stationary phases may also be used which have been extracted greatly augments the recovery of each of these two phases after separation.
In a specific application of the invention, reverse micelle chromatography decreases retention times for polar solutes with silica stationary phases. The most valuable chromatographic applications are envisioned to be process chromatography (i.e., larger scale than analytical) applications). In applications to separation or extraction of biological and biochemical compounds, the invention offers a wide range of options for separation processes, utilizing selective uptake of the biological/biochemical components into the reverse micelle phase and phase separation by manipulation of the maximum polar fluid-to-surfactant ratio (W.sub.o) by control of density. Some near critical nonpolar fluids that are gases at standard temperature and pressure, such as propane, can be used under pressures in which they are liquids, and so controlled, at temperatures safe for thermally-sensitive biological compounds. Other fluids under supercritical conditions may also be advantageous. This method is shown to be effective for selectively extracting proteins, such as hemoglobin, myoglobin, and cytochrome-C, using density control contrary to experience in liquid AOT/iso-octane reverse micelle separations (3). Such separations can be conducted without substantial loss of activity or denaturing of proteins.
The foregoing and additional objects, features, and advantages of the present invention will be more readily apparent from the following detailed description of a preferred embodiment which proceeds with reference to the accompanying drawings.


BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a diagram of an idealized reverse micelle structure.
FIG. 2 shows six ternary phase diagrams for alkane-AOT-water systems: (a) liquid ethane, 25.degree. C., (b) supercritical ethane, 37.degree. C., (c) liquid propane, 25.degree. C., (d) supercritical propane, 103.degree. C., (e) liquid iso-octane, 25.degree. C., and (f) liquid iso-octane, 103.degree. C. In the region to the right of the phase boundary lines a single, clear reverse micelle phase exists; in the region to the left the system contains two phases.
FIG. 3 is a graph of water to surfactant ratio (W) v. reverse micelle diameter.
FIG. 4 is a graph of a minimum supercritical ethane (T.sub.c =32.4.degree. C.) density required for the formation of stable reverse micelles as a function of temperature. Densities correspond closely to those for the pure ethane at similar conditions.
FIG. 5 is a graph of solubility of AOT in supercritical ethane at 37, 50 and 100.degree. C., W=1.
FIG. 6 is a graph of solubility of AOT in supercritical propane at 103.degree. C., W=1.
FIG. 7 is a graph of conductivity of reverse micelle phases in supercritical propane and liquid iso-octane at various pressures, W=1.
FIG. 8 is a graph of density of AOT-supercritical ethane solutions at 37.degree. C. and 240 bar.
FIG. 9 is an enlargement of FIG. 2(b) showing the ethane-rich corner of the ethane/AOT/water ternary phase diagram (weight %) at 37.degree. C. and at two pressures, 250 and 350 bar.
FIG. 10 is an enlargement of FIG. 2(d) showing the propane-rich corner of the propane/AOT/water ternary phase diagram (weight %) at 103.degree. C. and at three pressures, 100, 200 and 300 bar.
FIG. 11 is an enlargement of FIG. 2(f) showing the iso-octane rich corner of the iso-octane/AOT/water ternary phase diagram (weight %) at 103.degree. C. and at three pressures, 100, 200 and 300 bar.
FIG. 12 is a normal-phase reverse micelle supercritical propane chromatogram: propane 110.degree. C., 250 bar; [AOT]=5.times.10.sup.-2 M, W=5.0. Peak identification is as follows: (A) phenol, (B) 2-naphthol, (C) resorcinol.
FIG. 13 is another chromatogram showing separation of two polar dyes: propane 103.degree. C., 375 bar; [AOT]=5.times.10.sup.

REFERENCES:
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R. W. Gale, J. L. Fulton and R. D. Smith "Organized Molecular Assemblies in the Gas Phase: Reverse Micelles and Microemulsions in Supercritical Fluids " J.A.C.S., 109, 920 (1987).
R. D. Smith, J. L. Fulton and H. K. Jones "Reverse Micelle Sypercritical Fluid Separations", Separation Science Technology, vol. 23, Oct., 1988.
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Zulauf, M.; Eicke, H. F., "Inverted Micelles and Microemulsions in the Ternary System H.sub.2 O/Aerosol-OT/Isooctane as Studied by Photon Correlation Spectroscopy," J. Phys. Chem., 1979, 83,480-486.
Kotlarchyk, M.; Huang, J. S.; Chen, S. H., "Structure of AOT Reversed Micelles Determined by Small-Angle Neutron Scattering," J. Phys. Chem., 1985, 89, 4382-4386.
Wong, J. M.; Johnston, K. P., "Solubilization of Biomolecules in Carbon Dioxide Based Supercritical Fluids," Biotechnol. Prog., 1986, vol. 2, No. 1, 29-39.
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Nagy, J. B.; Gourgue, A.; DeRouance, E. G., "Preparation of Monodispersed Nickel Boride Catalysts Using Reversed Micellar System," Pre
The United States has rights in this invention under Department of Energy Contract DE-AC06-76RL0-1830.
This application is a continuation of U.S. Ser. No. 07/152,256, filed Feb. 4, 1988, which is a continuation-in-part of U.S. Ser. No. 07/125,842, filed Nov. 24, 1987, by D. W. Matson, J. L. Fulton and R. D. Smith, entitled CHEMICAL REACTIONS IN SUPERCRITICAL FLUID MICELLE SYSTEMS now both abandoned.

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