Antiperspirant Active Compositions and Manufacture Thereof

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) exhibiting an 27 Al NMR spectrum with a species distribution including at least 90% A130 polyhydroxyoxoaluminum cation as the predominant species detectable by 27 Al NMR within the aluminum salt. The composition can optionally include zirconium. Also disclosed are a method of making an antiperspirant active composition and the use of a heating step at elevated temperature to convert Al 13 polyhydroxyoxoaluminum cations in the species detectable by 27 Al NMR within an aqueous aluminum salt solution into Al 30 polyhydroxyoxoaluminum cations in the species detectable by 27 Al NMR without increasing a SEC Peak 3 area in the SEC chromatogram of the aluminum salt.

1 . 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) exhibiting an  27 Al NMR spectrum with a species distribution including at least 90% Al 30  polyhydroxyoxoaluminum cation as the predominant species detectable by  27 Al NMR within the aluminum salt, wherein the 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 
     
     
         2 . The antiperspirant active composition of  claim 1 , wherein the  27 Al NMR spectrum has a species distribution including at least 95% Al 30  polyhydroxyoxoaluminum cation as the predominant species detectable by  27 Al NMR within the aluminum salt. 
     
     
         3 . The antiperspirant active composition 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 aluminum salt. 
     
     
         4 . The antiperspirant active composition of  claim 3 , wherein the  27 Al NMR spectrum has a species distribution including no Al 13  polyhydroxyoxoaluminum cation in the species detectable by  27 Al NMR within the aluminum salt. 
     
     
         5 . The antiperspirant active composition of  claim 1 , wherein the  27 Al NMR spectrum has a species distribution including at most 5% Al m , Al m  comprising an aluminum- and chloride-containing monomer, in the species detectable by  27 Al NMR within the aluminum salt. 
     
     
         6 . The antiperspirant active composition of  claim 1 , wherein the aluminum salt has an OH to Al ratio of at most 2.6:1. 
     
     
         7 . The antiperspirant active composition of  claim 5 , wherein the aluminum salt has an OH to Al ratio of 2:1 to 2.5:1. 
     
     
         8 . The antiperspirant active composition of  claim 1 , further comprising a buffer, wherein a molar ratio of buffer to aluminum is at least 0.1:1. 
     
     
         9 . The antiperspirant active composition of  claim 8 , wherein the buffer is at least one buffer chosen from an amino acid and betaine. 
     
     
         10 . The antiperspirant active composition of  claim 9 , wherein the buffer is an amino acid and a molar ratio of amino acid to aluminum is at least 0.1. 
     
     
         11 . The antiperspirant active composition of  claim 10 , wherein the amino acid is glycine. 
     
     
         12 . The antiperspirant active composition of  claim 1 , wherein the composition 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. 
     
     
         13 . The antiperspirant active composition of  claim 1 , wherein the composition 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. 
     
     
         14 . The antiperspirant active composition of  claim 13 , wherein the composition has no SEC Peak 3 area in the SEC chromatogram. 
     
     
         15 . The antiperspirant active composition of  claim 1 , wherein the composition 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. 
     
     
         16 . The antiperspirant active composition of  claim 15 , wherein the composition has no SEC Peak 5 area in the SEC chromatogram. 
     
     
         17 . The antiperspirant active composition of  claim 1 , wherein the composition has a SEC Peak 4 area of 95 to 100%, no SEC Peak 3 area, and a SEC Peak 5 area of from 0 to 5% of a total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram. 
     
     
         18 . The antiperspirant active composition of  claim 1 , wherein the composition further comprises zirconium. 
     
     
         19 . The antiperspirant active composition of  claim 18 , wherein a molar ratio of aluminum to zirconium is 5:1 to 10:1. 
     
     
         20 . 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, wherein the buffer is an amino acid or betaine and a molar ratio of buffer to aluminum is at least 0.1:1, 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 salt solution having an OH:Al molar ratio of at most 2.6:1, and a pH of 2 to 5;   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 a third aluminum salt exhibiting an  27 Al NMR spectrum with a species distribution including at least 90% Al 30  polyhydroxyoxoaluminum cation as the predominant species detectable by  27 Al NMR within the third aluminum salt; and   IV) 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.   
     
     
         21 . The method of  claim 20 , wherein the 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. 
     
     
         22 . The method of  claim 20 , wherein the buffer is glycine. 
     
     
         23 . The method of  claim 19 , 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. 
     
     
         24 . The method of  claim 23 , wherein the inorganic base is calcium hydroxide. 
     
     
         25 . The method of  claim 19 , wherein the second pH adjusted aluminum salt solution has an OH to Al molar ratio of 2:1 to 2.5:1. 
     
     
         26 . The method of  claim 19 , wherein the first aluminum salt is an aluminum chloride compound chosen from aluminum trichloride, aluminum chlorohexahydrate, and aluminum dichlorohydrate. 
     
     
         27 . The method of  claim 19 , wherein the composition further comprises zirconium and step IV) is present in the method. 
     
     
         28 . The method of  claim 27 , wherein the zirconium compound is ZrOCl 2 .8H 2 O. 
     
     
         29 . The method of  claim 19 , wherein the  27 Al NMR spectrum has a species distribution including at least 95% Al 30  polyhydroxyoxoaluminum cation as the predominant species detectable by  27 Al NMR within the third aluminum salt. 
     
     
         30 . The method of  claim 19 , 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 third aluminum salt. 
     
     
         31 . The method of  claim 30 , wherein the  27 Al NMR spectrum has a species distribution including no Al 13  polyhydroxyoxoaluminum cation in the species detectable by  27 Al NMR within the third aluminum salt. 
     
     
         32 . The method of  claim 19 , wherein the  27 Al NMR spectrum has a species distribution including at most 5% Al m , Al m  comprising an aluminum-and chloride-containing monomer, in the species detectable by  27 Al NMR within the third aluminum salt. 
     
     
         33 . The method of  claim 19 , wherein the third 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. 
     
     
         34 . The method of  claim 19 , wherein the third 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. 
     
     
         35 . The method of  claim 34 , wherein the third aluminum salt has no SEC Peak 3 area in the SEC chromatogram. 
     
     
         36 . The method of  claim 19 , 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. 
     
     
         37 . The method according to  claim 19 , wherein in step III) the period of time is at least 12 hours. 
     
     
         38 . The method according to  claim 19 , wherein a molar concentration of aluminum is greater than 0.2M up to 2.5M. 
     
     
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         55 . An antiperspirant active composition including an aluminum salt produced by the method of  claim 20 .