Method of making aluminum-zirconium antiperspirant of enhanced efficacy
View Patent ↗A novel efficacious and less irritant aluminum-zirconium antiperspirant composition is provided by the addition of a small amount of AlCl 3 and/or HCl to the activated aluminum component. After the heating of diluted basic aluminum chlorohydrate solution, cooling to room temperature, mixing with small amount of AlCl 3 or HCl and then reacting with zirconium glycine complex, an aluminum-zirconium salt is produced with a maximum amount of depolymerization aluminum and zirconium species. The addition of a small amount of AlCl 3 or HCl to the diluted and activated aluminum chlorohydrate solution accelerates the depolymerization of the activated ACH solution, and upon the addition of zirconium glycinate the solution is further depolymerized and results in the formation of less polymerized zirconium species.
1. A method of making solid activated aluminum-zirconium composition having a metal/chloride ratio of about 1.2 to about 1.3 comprising:
i) heating 8–20% by weight basic aluminum halides or nitrate of the formula:
Al 2 (OH) 6-a X a
wherein X is Cl, Br or NO 3 , wherein a is from about 1 to 1.5 from 50° C., to about reflux for about 2 to 20 hours and cooling to RT, mixing with small amount of AlCl 3 or HCl or a mixture there of AlCl 3 and HCl at about RT for a period of about 5 minutes to about 30 minutes,
ii) mixing with the solution of a zirconium glycine compound of the formula:
ZrO(OH) b X 2-b A c
wherein b is a numerical number from 0 to 0.7, X is Cl, Br or NO 3 , A is an amino acid, c is a number from 0.8 to about 1.2 and
iii) drying the blended solution of (i) and (ii) to a solid.
2. The method according to claim 1 wherein the amount of AlCl 3 added is such that the weight ratio of aluminum in basic aluminum halides to the weight of AlCl 3 (32°Be) is about 0.5 to about 10.
3. The method according to claim 1 wherein the amount of AlCl 3 added is that the weight ratio of aluminum in basic aluminum halides to the weight of AlCl 3 (32°Be) is about 3 to about 5.
4. The method according to claim 1 wherein the mixing time of activated aluminum component and AlCl 3 is about 1 to about 5 minutes.
5. The method according to claim 1 wherein the mixing time of activated aluminum component and AlCl 3 is from about 25 to about 30 minutes.
6. The method according to claim 1 wherein the amino acid is glycine.
7. The method according to claim 1 wherein the molecular ratio of glycine to zirconium is 1.
8. An activated Al−Zr composition having a metal (Al+Zr) to chloride molar ratio of about 1.20 to about 1.30 and aluminum to zirconium atomic ratio of about 2 to 10 with at least 10% Al species at chemical shift about 0 ppm and at least 2% Al species at chemical shift about 63 ppm by 27 Al NMR.
9. A composition according to claim 8 wherein the composition has about 20% HPLC Band IV.
10. A composition according to claim 8 wherein the composition has a HPLC Band III/II area ratio of about 1.
11. A composition according to claim 8 wherein the composition has amino acid to zirconium mole ratio of about 0.8 to about 1.2.