US 5,626,827 A · Basic aluminum antiperspirant active materials having enhanced activity, antiperspirant active compositions containing such materials, and methods for preparation of such materials and compositions

Abstract

Disclosed are basic aluminum antiperspirant materials having univalent complex oxoanions (e.g., nitrate); methods of making such materials; antiperspirant compositions containing such basic aluminum materials, another antiperspirant active material (e.g., a basic zirconium halide salt), and optionally a neutral amino acid; and methods of making such compositions. Size exclusion high performance liquid chromatography chromatograms of the disclosed basic aluminum materials have a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the peaks 3 and 4 being at least 50%; and less than 10% of the chromatographic peaks eluting at peaks 1 and 2. The disclosed basic aluminum materials have less than 25% of the aluminum in the form of Al.sup.b polyhydroxyaquoaluminum, and have a .sup.27 Al NMR spectrum in which the area of the 71.5-73.5 ppm resonance line includes more than 50% of the combined areas of the 62.5-63.5 ppm and 71.5-73.5 ppm resonance lines, and 5%-30% of the total area under the spectrum from 140 ppm to -80 ppm is contained in the resonance line at 71.5-73.5 ppm. The basic aluminum material of the present invention can be produced by adding a stoichiometric or near-stoichiometric amount of aluminum metal to a solution of an aluminum salt having a univalent complex oxoanion; the basic aluminum material can also be made by adding to such solution of the aluminum salt, aluminum metal having, in total, a relatively small surface area (large-sized particles of aluminum).

Claims26

Dependent claims

Basic aluminum materials having the empirical formula:

Al.sub.2 (OH).sub.6-a X.sub.a,
where 0.5.ltoreq.a.ltoreq.5.0;
and X is a univalent complex oxoanion of nitrogen or a halogen, which forms salts with Al.sup.3+ in aqueous solution, so that these salts are essentially completely dissociated, which is readily soluble in water with metallic ions in the solution, and which forms conjugate acids that are strong acids, the materials being further characterized by:
(a) size exclusion high performance liquid chromatography peaks corresponding to peak 3 and peak 4 of the size exclusion chromatogram produced from a high performance liquid chromatography technique;
(b) a peak 4 relative area of at least 25%, and a peak 3 relative area of less than 60%, the sum of the relative peak 3 and peak 4 areas being at least 50%;
(c) less than 10% chromatographic peaks eluting at shorter retention times than peak 3, corresponding to peaks 1 and 2;
(d) less than 25% of the aluminum being in the form of Al.sup.b polyhydroxyaquoaluminum;
(e) an .sup.27 Al NMR spectrum wherein 5% to 30% of the total area under the spectrum from 140 ppm to -80 ppm is contained in a resonance line at 71.5-73.5 ppm;
and
(f) an .sup.27 Al NMR spectrum in which the area of the 71.5-73.5 ppm resonance line includes more than 50% of the combined areas of the 62.5-63.5 ppm and 71.5-73.5 ppm resonance lines.

7 more elements

Basic aluminum materials having the empirical formula:

Al.sub.2 (OH).sub.6-a X.sub.a
where 0.5.ltoreq.a.ltoreq.5.0;
and X is a univalent complex oxoanion of nitrogen or a halogen, which forms salts with Al.sup.3+ in aqueous solution, so that these salts are essentially completely dissociated, which is readily soluble in water with metallic ions in the solution, and which forms conjugate acids that are strong acids, the material being further characterized by:
(a) a size exclusion high performance liquid chromatography chromatogram which contains:
(1) a peak 4 relative area of at least 60%, a peak 3 relative area of less than 25%, the sum of the relative peak 3 and peak 4 areas being at least 70%;
(2) a combined peak 5 and peak 6 relative area of less than 20%;
and
(3) less than 10% chromatographic peaks eluting at shorter retention times than peak 3, corresponding to peaks 1 and 2;
(b) a .sup.27 Al NMR spectrum in which:
(1) a 71.5-73.5 ppm resonance line comprises at least 5% of the total area of the NMR spectrum;
(2) a 0-5 ppm resonance line comprises less than 10% of the total area of the NMR spectrum;
and
(3) a 62.5-63.5 ppm resonance line comprises less than 10% of the total area of the NMR spectrum;
and
(c) less than 25% of the total aluminum in the form of Al.sup.b hydroxyaquoaluminum.

12 more elements

Dependencies are inferred from the claim text.

Basic aluminum antiperspirant active materials having enhanced activity, antiperspirant active compositions containing such materials, and methods for preparation of such materials and compositions

Life of this patent

Basic aluminum antiperspirant active materials having enhanced activity, antiperspirant active compositions containing such materials, and methods for preparation of such materials and compositions

Life of this patent

Abstract

Claims26