Antiperspirant active compositions and manufacture thereof

Patent metadata

Field	Value
Publication number	US-9717663-B2
Application number	US-201615224681-A
Country	US
Kind code	B2
Filing date	Aug 1, 2016
Priority date	Apr 26, 2011
Publication date	Aug 1, 2017
Grant date	Aug 1, 2017

Abstract

An antiperspirant active composition comprising an aluminum salt, the aluminum salt (i) having an aluminum to chloride molar ratio of 0.3:1 to 3:1; and (ii) having a species of polyhydroxyoxoaluminum cation detectable at 76 ppm by 27 Al NMR that is present in a relative abundance on a 27 Al NMR spectrograph that is greater than any other polyhydroxyoxoaluminum cation detectable by 27 Al NMR. Also, disclosed are methods of making the antiperspirant active.

First claim

What is claimed is:

1. A method of making an antiperspirant active composition comprising:
I) heating an aqueous solution containing i) a first aluminum salt containing an Al 30 polyhydroxyoxoaluminum cation and having an aluminum to chloride molar ratio of 0.3:1 to 3:1, ii) an inorganic salt, and iii) a buffer, wherein the heating forms a fourth aluminum salt, and is one of
a) at a temperature of 100° C. to 250° C. in an isochoric reactor or under hydrothermal reaction for a time sufficient to form a species of polyhydroxyoxoaluminum cation detectable at 76 ppm by NMR; or
b) at 100° C. at reflux for about 10 days or greater.

2. A method of making an antiperspirant active composition comprising:
I) heating an aqueous solution containing a first aluminum salt having an aluminum to chloride molar ratio of 0.3:1 to 3:1 and a buffer, at a temperature of 50° C. to 100° C. for a period of time of 1 hour to 6 hours to obtain a first aluminum salt solution;
II) adding to the first aluminum salt solution an aqueous solution of an inorganic base to obtain a second pH adjusted aluminum sat solution having an OH:Al molar ratio of at most 2.6:1;
III) heating the second pH adjusted aluminum salt solution at a temperature of 50° C. to 100° C. for a period of time of at least 6 hours to obtain a third aluminum salt solution containing an Al 30 polyhydroxyoxoaluminum cation;
IV) heating the third aluminum salt solution to form a fourth aluminum salt at one of
a) at a temperature of 100° C. to 250° C. in an isochoric reactor or under hydrothermal reaction for a time sufficient to form a species of polyhydroxyoxoaluminum cation detectable at 76 ppm by 27 Al NMR; or
b) at 100° C. at reflux for about 10 days or greater; and

V) optionally adding an aqueous solution containing a zirconium compound to the second pH adjusted aluminum salt solution to thereby obtain a second pH adjusted aluminum-zirconium salt solution having a molar ratio of aluminum to zirconium of 5:1 to 10:1.

3. The method of claim 1 , wherein the inorganic salt is at least one chloride salt chosen from calcium chloride, strontium chloride, barium chloride, and yttrium chloride.

4. The method of claim 1 , wherein the buffer is at least one of an amino acid, betaine, quat, and glycine, and a molar ratio of buffer to aluminum is at least 0.1:1.

5. The method of claim 2 , wherein the buffer is at least one of an amino acid, betaine, quat, and glycine, and a molar ratio of buffer to aluminum is at least 0.1:1.

6. The method of claim 1 , wherein the inorganic salt is calcium chloride and the buffer is glycine.

7. The method of claim 1 , wherein heating in the isochoric reactor or under hydrothermal reaction is one of
i) at 100° C. for about 5 days,
ii) at 120° C. for about 12 hours, or
iii) at 150° C. for about 20 minutes.

8. The method of claim 2 , wherein heating in the isochoric reactor or under hydrothermal reaction is one of
i) at 100° C. for about 5 days,
ii) at 120° C. for about 12 hours, or
iii) at 150° C. for about 20 minutes.

9. The method of claim 1 , wherein the fourth aluminum salt exhibits a SEC chromatogram having a SEC Peak 4 area of at least 90% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

10. The method of claim 2 , wherein the fourth aluminum salt exhibits a SEC chromatogram having a SEC Peak 4 area of at least 90% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

11. The method of claim 2 , wherein the inorganic base includes at least one member chosen from calcium hydroxide, strontium hydroxide, barium hydroxide, calcium oxide, strontium oxide, barium oxide, calcium carbonate, barium carbonate, strontium carbonate, yttrium hydroxide, yttrium oxide, and yttrium carbonate.

12. The method of claim 11 , wherein the inorganic base is calcium hydroxide.

13. The method of claim 2 , wherein the second pH adjusted aluminum salt solution has an OH to Al molar ratio of 2:1 to 2.5:1.

14. The method of claim 2 , wherein the first aluminum salt is an aluminum chloride compound chosen from aluminum trichloride, aluminum chlorohexahydrate, and aluminum dichlorohydrate.

15. The method of claim 2 , wherein the composition further comprises zirconium and step V) is present in the method.

16. The method of claim 15 , wherein the zirconium compound is at least one of ZrOCl 2 .8H 2 O and Oxo-Hexameric Zirconium-Octaamino Acid.

17. The method of claim 1 , wherein the 27 Al NMR spectrum has a species distribution including at most 5% Al 13 polyhydroxyoxoaluminum cation in the species detectable by 27 Al NMR within the fourth aluminum salt.

18. The method of claim 2 , wherein the 27 Al NMR spectrum has a species distribution including at most 5% Al 13 polyhydroxyoxoaluminum cation in the species detectable by 27 Al NMR within the fourth aluminum salt.

19. The method of claim 1 , wherein the fourth aluminum salt has a SEC Peak 4 area of at least 95% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

20. The method of claim 2 , wherein the fourth aluminum salt has a SEC Peak 4 area of at least 95% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

21. The method of claim 1 , wherein the fourth aluminum salt has a SEC Peak 3 area of less than 5% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

22. The method of claim 2 , wherein the fourth aluminum salt has a SEC Peak 3 area of less than 5% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

23. The method of claim 2 , wherein the third aluminum salt has a SEC Peak 5 area of less than 5% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

24. The method according to claim 2 , wherein in step III) the period of time is at least 12 hours.

Assignees

• Colgate Palmolive Co

Inventors

• Vaughn John
• Pappas Iraklis
• Pan Long

Classifications

• C01F7/78

  Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements (aluminates C01F7/02; compounds containing aluminium, fluorine and alkali or alkaline earth metals C01F7/54; nitrates containing other cations besides aluminium C01F7/66; sulfides, sulfites or sulfates containing other cations besides aluminium C01F7/70 - C01F7/74) · CPC title

• C01F7/57

  Basic aluminium chlorides, e.g. polyaluminium chlorides · CPC title

• A61Q15/00

  Anti-perspirants or body deodorants (deodorisation of air A61L9/00) · CPC title

• A61K8/26 Primary

  Aluminium; Compounds thereof · CPC title

• A61K8/20

  Halogens; Compounds thereof · CPC title