IP Library Granted Patent US 7,074,394
Granted Patent B2
US 7,074,394 · App. 10/625,038 · Granted Jul 11, 2006

Stable aluminum/zirconium antiperspirant solution free of amino acid and polyhydric alcohol

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Quick Facts
Patent No.
US 7,074,394
App. No.
10/625,038
Granted
Jul 11, 2006
Kind
B2
Abstract

A stable aluminum-zirconium aqueous solution of enhanced efficacy having a high concentration free of amino acid and polyhydric alcohol is disclosed. Such aluminum-zirconium salts are selected from aluminum/zirconium tetrachlorohydrate; aluminum/zirconium pentachlorohydrate, and aluminum/zirconium octachlorohydrate in which the aluminum to zirconium (Al/Zr) atomic ratio of said salt falls within the limits of the shaded areas A, B, and C, respectively, of the drawing graph wherein the aluminum/zirconium tetrachlorohydrate has an Al/Zr atomic ratio from about 2 to about 6 and metal/chloride molecular ratio about 0.9 to about 1.25; aluminum/zirconium pentachlorohydrate having Al/Zr atomic ratio from about 6 to about 10 and metal/chloride atomic ratio from about 1.5 to about 1.65; and aluminum/zirconium octachlorohydrate having Al/Zr molecular ratio from about 6 to about 10 and metal/chloride molecular ratio from about 0.9 to about 1.5.

Claims (22)

1. A stable and highly efficacious aqueous antiperspirant solution free of amino acid and polyhydric alcohol and consisting essentially of from about 15 to about 40 percent anhydrous solid of a salt selected from aluminum/zirconium tetrachlorohydrate, aluminum/zirconium pentachlorohydrate, and aluminum/zirconium octachlorohydrate in which the aluminum to zirconium (Al/Zr) atomic ratio of said salt falls within the limits of the shaded areas A, B, and C, of the drawing graph and wherein, respectively, the aluminum/zirconium tetrachlorohydrate has an Al/Zr atomic ratio from about 2 to about 6 and metal/chloride atomic ratio about 0.9 to about 1.25; aluminum/zirconium pentachlorohydrate having Al/Zr atomic ratio from about 6 to about 10 and metal/chloride atomic ratio from about 1.5 to about 1.65; and aluminum/zirconium octachlorohydrate having Al/Zr atomic ratio from about 6 to about 10 and metal/chloride atomic ratio from about 0.9 to about 1.5.

2. The antiperspirant solution of claim 1 wherein the salt is the aluminum/zirconium octachlorohydrate.

3. The antiperspirant salt of claim 1 wherein the salt is the aluminum/zirconium tetrachlorohydrate.

4. The antiperspirant salt of claim 1 wherein the salt is the aluminum/zirconium pentachlorohydrate.

5. The antiperspirant salt of claim 2 wherein the percent of the anhydrous salt is from about 20 to about 40.

6. The antiperspirant salt of claim 3 wherein the percent of the anhydrous salt is from about 20 to about 40.

7. The antiperspirant salt of claim 4 wherein the percent of the anhydrous salt is from about 20 to about 40.

8. The antiperspirant solution according to claim 1 which is dried to a powder.

9. A method of making stable aluminum-zirconium salt solution free of amino acid and polyhydric alcohol which comprises mixing and reacting basic aluminum halides and nitrates of the formula:

Al 2 (OH) 6-a X a

wherein X is Cl, Br and/or NO 3 , wherein a is from about 1 to 2 with a zirconium compound of the formula:

ZrO(OH) b X 2-b .

wherein b is a numerical number from 0 to 1.3 and X is Cl, Br and/or NO 3 at temperature not in excess of about 80° C.

10. The method of claim 9 wherein the reaction is at room temperature.

11. The method of claim 9 wherein the basic aluminum halides and nitrate employed in the reaction is made by reacting (a) aluminum powder, (b) an aluminum halide or nitrate solution and (c) water at a temperature greater than about 85° C.

12. The method of claim 9 wherein the basic aluminum halides and nitrate is made by mixing about 50% aluminum chlorohydrate with AlCl 3 or HCl from about room temperature to about reflux for a period of about 0.5 hr. to 2 days.

13. The method of claim 9 ; wherein the zirconium halide complex is made by mixing basic zirconium carbonate with HCl or zirconium oxychloride at a temperature of about 50–70° C. until the solution is clear.

14. The method of claim 13 wherein the zirconium halide complex is heated at about 80–100° C. for 0.5 to 4 hrs.

15. The method of claim 9 wherein the aluminum-zirconium solution is dried to a powder.

16. A roll on formulation in which the solution of claim 1 is the active ingredient.

17. A clear gel formulation in which the solution of claim 1 is the active ingredient.

18. An antiperspirant stick formulation in which the powder of claim 8 is the active ingredient.

Assignments (20)
RELEASE OF SECURITY INTEREST Recorded Mar 27, 2017
From: CITIZENS BANK OF PENNSYLVANIA, AS ADMINISTRATIVE AGENT
To: REHEIS, INC.
Reel/Frame 041749/0496 →
RELEASE OF SECURITY INTEREST Recorded Dec 1, 2014
From: MVC CAPITAL, INC., AS ADMINISTRATIVE AGENT
To: REHEIS, INC.
Reel/Frame 034292/0767 →
RELEASE OF SECURITY INTEREST Recorded Apr 30, 2013
From: CHURCHILL FINANCIAL LLC, AS ADMINISTRATIVE AGENT
To: SUMMIT RESEARCH LABS, INC.; SUMMIT RESEARCH LABS HOLDING COMPANY; REHEIS, INC.; WBS CARBONS ACQUISITION CORP.
Reel/Frame 030318/0063 →
NOTICE OF GRANT OF SECURITY INTEREST IN PATENTS Recorded Apr 3, 2013
From: REHEIS, INC.
To: MVC CAPITAL, INC., AS ADMINISTRATIVE AGENT
Reel/Frame 030140/0011 →
SECURITY AGREEMENT Recorded Apr 1, 2013
From: REHEIS, INC.
To: CITIZENS BANK OF PENNSYLVANIA, AS ADMINISTRATIVE AGENT
Reel/Frame 030123/0168 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS Recorded Apr 1, 2013
From: MVC CAPITAL, INC., AS AGENT
To: SUMMIT RESEARCH LABS, INC.; SUMMIT RESEARCH LABS HOLDING COMPANY; REHEIS, INC.; WBS CARBONS ACQUISITION CORP.
Reel/Frame 030122/0653 →
TERMINATION OF SECURITY INTEREST IN PATENTS RECORDED AT REEL 015740/FRAME 0445 Recorded Nov 24, 2009
From: BANK OF AMERICA, NATIONAL ASSOCIATION, AS FIRST LIEN COLLATERAL AGENT
To: REHEIS, INC.
Reel/Frame 023565/0347 →
RELEASE OF SECURITY INTEREST Recorded Mar 27, 2008
From: BANK OF AMERICA, N.A.
To: REHEIS, INC.
Reel/Frame 020710/0248 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 14, 2008
From: REHEIS, INC.
To: SUMMIT RESEARCH LABS, INC.
Reel/Frame 020645/0837 →
SECURITY AGREEMENT Recorded Mar 14, 2008
From: SUMMIT RESEARCH LABS, INC.; SUMMIT RESEARCH LABS HOLDING COMPANY; REHEIS, INC.; WBS CARBONS ACQUISITION CORP.
To: MVC CAPITAL, INC.
Reel/Frame 020654/0068 →
SECURITY AGREEMENT Recorded Mar 3, 2008
From: SUMMIT RESEARCH LABS, INC.; SUMMIT RESEARCH LABS HOLDING COMPANY; REHEIS, INC.; WBS CARBONS ACQUISITION CORP.
To: CHURCHILL FINANCIAL LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 020582/0553 →
RELEASE OF SECURITY INTEREST AT REEL/FRAME NO. 15747/0564 Recorded Mar 26, 2007
From: GOLDMAN SACHS CREDIT PARTNERS L.P.
To: REHEIS, INC.
Reel/Frame 019063/0612 →
SECURITY AGREEMENT Recorded Mar 8, 2005
From: REHEIS, INC.
To: GOLDMAN SACHS CREDIT PARTNERS L.P., AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 015747/0564 →
SECURITY AGREEMENT Recorded Mar 7, 2005
From: REHEIS, INC.
To: BANK OF AMERICA, N.A., AS FIRST LIEN COLLATERAL AGENT
Reel/Frame 015740/0445 →
RELEASE OF SECURITY INTEREST AT REEL/FRAME NO. 14815/0803 Recorded Mar 4, 2005
From: BANK OF AMERICA, N.A., AS AGENT
To: REHEIS, INC.
Reel/Frame 015732/0250 →
RELEASE OF SECURITY INTEREST IN PATENT RIGHTS Recorded May 27, 2004
From: BNY ASSET SOLUTIONS LLC, A DELAWARE LIMITED LIABILITY COMPANY
To: REHEIS, INC., A CORP. OF DELAWARE
Reel/Frame 014675/0192 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 3, 2004
From: LI, ZIJUN; PAREKH, JAWAHAR
To: REHEIS INC.
Reel/Frame 015032/0272 →
SECURITY AGREEMENT Recorded Jan 28, 2004
From: REHEIS, INC. (DE CORPORATION)
To: BNY ASSET SOLUTIONS LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 014289/0030 →
ASSIGNMENT FOR SECURITY Recorded Dec 19, 2003
From: REHEIS, INC.
To: BANK OF AMERICA, N.A., AS AGENT
Reel/Frame 014815/0803 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 22, 2003
From: LI, ZIJUN; PAREKH, JAWAHAR
To: PLANTAMURA, ARTHUR J.
Reel/Frame 014338/0234 →