Drug – bio-affecting and body treating compositions – Anti-perspirants or perspiration deodorants
Reexamination Certificate
2000-10-20
2002-04-23
Dodson, Shelley A. (Department: 1616)
Drug, bio-affecting and body treating compositions
Anti-perspirants or perspiration deodorants
C424S066000, C424S068000, C424S400000, C424S401000
Reexamination Certificate
active
06375937
ABSTRACT:
FIELD OF THE INVENTION
This invention relates to a class of antiperspirant salts that may be used to formulate antiperspirants with enhanced efficacy.
BACKGROUND OF THE INVENTION
A variety of art is available that describes various salts and methods of making them. U.S. Pat. No. 4,331,609 to Orr teaches an antiperspirant active comprising aluminum and zirconium made with separate aluminum and zirconium compounds as well as a neutral amino acid wherein the molar ratio of neutral amino acid to total metal is from about 0.90 to about 0.24. The total metal:chlorine ratio in the complex that is formed is less than 1.30.
EP publication number 0 047 650 describes aqueous solution-stable antiperspirant complexes comprising an aluminum compound, a zirconium or hafnium compound, a water soluble neutral amino acid and an inorganic acid. The molar ratio of neutral amino acid to total metal is from about 0.90 to about 0.24 in an aqueous system, and the molar ratio of neutral amino acid to total metal is from about 0.90 to about 0.75 in a non-aqueous system. The total metal:chlorine ratio in the complex that is formed is less than 1.30.
United Kingdom Patent Application GB 2,076,289 describes an antiperspirant compositions comprising a combination of an aluminum chloride and an aluminum zirconium hydroxychloride in a synergistic mixture. The metal:chloride ratio is less than 0.9.
Canadian Patent 1,153,313 describes an antiperspirant composition which contains a buffering agent such as glycine with a synergistic mixture of aluminum chlorohydrate, aluminum chloride or aluminum zirconium polychlorohydrate complex. The molar ratio of aluminum to chloride is in the range of 0.78:1 to abut 1.95:1. Various salts are described which have a metal:halide ratio of 2.1:1-0.9:1. The glycine:zirconium ratio is much less than 1:1.
U.S. Pat. No. 4,871,525 to Giovanniello et al describes a solid powder of aluminum zirconium hydroxyl halide glycinate complex having improved antiperspirant activity wherein the glycine is used to prevent gel formation. The ratio of Zr to glycine is less than 1:1.
U.S. Pat. No. 6,126,928 to Swaile describes antiperspirant compositions wherein the molar ratio of neutral amino acid to total metal (aluminum•zirconium) is from about 0.90 to about 0.24, and the mole ratio of (aluminum•zirconium):chlorine is less than about 1.30:1.
U.S. Pat. No. 6,066,314 to Tang describes the use of post added glycine to aluminum zirconium salts in an amount in the range of 1:1.2-1:5 of zirconium:amino acid on a weight:weight basis.
None of the above cases described the combination of metal to chloride in combination with the glycine to zirconium ratio as found in the instant invention. Thus, it is surprising that the antiperspirant actives described in this invention provide more efficacious cosmetic products.
BRIEF SUMMARY OF THE INVENTION
This invention comprises aluminum zirconium salts which have a metal to chloride molar ratio in the range of 0.9-1.2:1 and a glycine:zirconium molar ratio greater than 1.3:1, particularly greater than 1.4:1.
DETAILED DESCRIPTION OF THE INVENTION
This invention comprises an aluminum zirconium tetrachlorohydrex glycine salt having a metal to chloride ratio in the range of 0.9-1.2:1 (especially in the range of 0.9-1.1:1 and, more particularly in the range of 0.9-1.0:1); and a glycine:zirconium ratio greater than 1.3:1, particularly greater than 1.4:1.
The salts of this invention may be made in a variety of ways:
Method A:
An aluminum chlorohydrate (ACH) solution of ACH salt in water of suitable concentration is mixed with an aqueous solution of zirconyl chloride (ZrOCl
2
) of suitable concentration and powdered glycine. The mixture is stirred at room temperature to obtain the salt.
Method B:
A suitable commercially available aluminum zirconium tetrachlorohydrex glycine salt is obtained and mixed with a sufficient amount of an aqueous aluminum chloride (AlCl
3
) solution and powdered glycine. The mixture is stirred at room temperature to obtain the salt.
When Method B is used, a suitable salt to use as a starting material includes various types of tetra salts such as aluminum zirconium tetrachlorohydrex gly, aluminum zirconium tetrachlorohydrex gly propylene glycol complex aluminum zirconium tetrachlorohydrex gly dipropylene glycol complex, and mixtures of any of the foregoing.
Method C:
An aqueous aluminum chlorohydrate (ACH) solution made from an activated ACH salt of suitable concentration is mixed with an aqueous solution of zirconyl chloride (ZrOCl
2
) of suitable concentration and powdered glycine. The mixture is stirred at room temperature for a short period of time and then spray dried to obtain the salt in powder form.
If the product is used as a solid powder, the size of the particles of antiperspirant active of the invention currently does not appear to be critical and may include conventional sizes such as greater than 2 to 100 microns, with selected grades having an average particle size of 30-40 microns; finer sized grades having an average particle size distribution from 2-10 microns with average size of about 7 microns as made by a dry-grinding method; and micronized grades of the type described in a co-pending patent application U.S. Ser. No. 9/579,322 having an average particle size of less than or equal to 2 microns, particularly less than or equal to 1.5 microns.
The enhanced salts of this invention may be used to formulate antiperspirants having improved efficacy. Such antiperspirants include solids such as sticks and creams (creams sometimes being included in the term “soft solid”), gels, liquids (such as are suitable for roll-on products), and aerosols. The forms of these products may be suspensions or emulsions.
It is preferred that the glycol content of the formulations be kept to a minimum.
Examples of suitable formulations include the following.
Sticks
Stick products may be made with conventional gelling agents such as stearyl alcohol and dibenzylidene sorbitol. A sample formulation is as follows:
40-55% (particularly 45%) cyclomethicone (especially D5 cyclomethicone)
20-30% (particularly 21%) stearyl alcohol
7-15% (particularly 10%) talc
15-22% (particularly 22%) antiperspirant active in powder form
1-3% (particularly 2%) fragrance
Roll-Ons
45-65% (particularly 55%) cyclomethicone (especially D5 cyclomethicone)
0.1-10% (particularly 3%) cyclomethicone/dimethicone copolyol (such as Dow Corning 2-5185 C)
10-25% (particularly 20%) antiperspirant active in solution form (25-45% actives on an anhydrous basis in water)
5-30% (particularly 20%) water
1-3% (particularly 2%) fragrance
Soft solids
Soft solids may be made with formulations described in co-pending patent application (U.S. Ser. No. 9/273,152 and PCT Publication number WO 99/51192. A sample formulation is as follows:
40-70% (particularly 50%) elastomer in cyclomethicone (KSG-15 from Shin-Etsu)
5-15% (particularly 6%) polyethylene (for example, beads having a density in the range of 0.91-0.98 g/cm
3
and an average particle size in the range of 5-40 microns)
10-20% (particularly 15%) C12-15 alkylbenzoate (Finsolv TN from Finetex)
0.1-25%% (particularly 22%) antiperspirant active in powder form
1-15% (particularly 5%) dimethicone (100 centistokes)
1-3% (particularly 2%) fragrance
Gels
Gels may be made with a variety of formulations such as
5-50% (particularly 29%) cyclomethicone (particularly D5)
0.1-10% (particularly 3%) cyclomethicone/dimethicone copolyol (such as Dow Corning 2-5185 C)
0-10% (particularly 5%) hydrogenated polyisobutene 250
0-10% (particularly 5%) C12-15 alkylbenzoate (Finsolv TN from Finetex)
0-10% (particularly 5%) dimethicone (100 centistokes)
0.1-25% (particularly 20%) antiperspirant active in powder form or 10-25% (particularly 20%) of active in solution (25-45% actives on an anhydrous basis)
5-50% (particularly 30%) water
1-3% (particularly 2%) fragrance
Note that in the explanation of the invention, where water is listed it is intended to count the contribution of the water present in the antiperspirant solution as part of the overall water content. Th
Chopra Suman
Hilliard, Jr. Peter
Tang Xiaozhong
Colgate-Palmolive Company
Dodson Shelley A.
Miano Rosemary M.
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