Zirconyl chloride (basic zirconium chloride or zirconium oxychloride) and zirconyl hydroxychloride solution are commercially available. Rotary vacuum drying at a maximum temperature of about 40°C and about 15 millimeters of mercury has been particularly satisfactory, but spray drying is probably the most practical and economical from a commercial standpoint. The product dissolved in anhydrous SDA-40 in about an hour to form a 30% solution with a CCl4 compatibility of 198 cc. and about 15 mm Hg to give 44 gm product. After overnight stirring, 95.2 gm of the solution was dried in a rotary vacuum evaporator at 30°C. For example, the zinc chloride (Zn Cl2) or zinc bromide (Zn Br2) may be added in their dry crystalline form or as an aqueous solution. 29.8 gm of zirconyl bromide (13.3% Zr) was added to 64.1 gm of 50% basic aluminum bromide (11.3% Al) giving an Al/Zr ratio of 5.5:1. Privacy Policy The product dissolved in anhydrous SDA-40 in 35 minutes to form a 30% solution with a compatibility of 197 cc. 88,206 of John L. Jones and Andrew M. Rubino, filed Nov. 9, 1970, for "Basic Aluminum Bromide Compositions," and assigned to the same assignees as the present invention. The solution was dried in a rotary vacuum evaporator at 30°C. In the case of the zirconyl compounds there is a continuous range of possible values of hydroxy and halide (X) proportions, ranging from zirconyl halide (X/Zr = 2.0) to zirconyl hydroxyhalide (X/Zr = 1.0), since the starting zirconium material is not necessarily a pure compound. The addition of the zinc or zirconium compound to the aqueous basic aluminum bromide solution is by simple mixing, and contrary to the methods described in U.S. Pat. You can disable the usage of cookies by changing the settings of your browser. The above and other objects are achieved by the complexes of the present invention which are prepared by providing an aqueous solution of five-sixths basic aluminum bromide; mixing with the aqueous solution a compound selected from the group consisting of zinc chloride, zinc bromide, zirconyl chloride, zirconyl bromide, zirconyl hydroxychloride, zirconyl hydroxybromide, and mixtures of these compounds; and drying the resulting mixture to produce the complex in the form of a substantially friable solid. Almost any of the usual drying methods known in the art are acceptable, such as air drying at atmospheric temperature and pressure, vacuum drying, freeze drying and spray drying. Analysis: 14.1% Al, 8.2% Zr, 27.3% H2 O by Karl Fischer. Preferred aluminum to zirconium or aluminum to zinc mol ratios (hereinafter referred to as Al/Zr and Al/Zn ratios) range between about 3 and 20 (i.e., y in the previously discussed formulas equal about 3 to 20). 88,206 are comparable to or slightly higher than the values for the zinc complexes. [citation needed] ZnCl 2 itself is hygroscopic and even deliquescent. This was broken up by heating for about 2 hours. The basic aluminum bromides used in the present invention may be prepared in a manner analogous to the conventional production of aluminum chlorhydroxide by reacting aluminum metal with the hydrobromic acid in water solution, or by reacting aluminum metal with a water solution of aluminum bromide. 28 gm of zirconyl bromide (13.3% Zr) was added to 100.2 gm of 50% basic aluminum bromide (11.3% Al) giving an Al/Zr ratio of 9.1:1. Aseptically add 0.5 mL of Inoculumto each tube so pre- pared, except two of the four containing no Standard Cya- nocobalamin Solution(the uninoculated blanks). Although heating to a temperature near reflux (100° C), as in Example VII, may be used where desired, most gelatin problems which may occur where the zirconium compounds are added may generally be avoided by dilution of the mixture with water. 3. Still further objects will appear hereinafter. entitled "Zirconium Complexes Of Basic Aluminum The complexes produced according to the above patents suffer from the disadvantage of being in aqueous solutions. After the addition of the desired zinc or zirconium compound, the resulting solution mixture is dried to form a friable solid complex having the desired water content. Thus, the zirconium complexes generally have CCl4 compatibilities in the range of about 150 to 250 or more, while the zinc complexes generally have CCl4 compatibilities of about 100 to 200. and about 15 mm Hg to 60 gm. To 1,282 gm of 50% basic aluminum bromide (10.7% Al) was added 114.4 gm of zinc bromide giving an Al/Zn ratio of 10.0:1. The zinc salts are miscible under all conditions, but there is usually a decrease in pH on standing or heating. The solution was spray dried at an outlet temperature of 180°F. ZrO (OH)2-z Xz. generation, Metal-aluminum inorganic-organic complexes and methods of preparing same, Zirconyl and aluminum halohydroxy complex, Zirconyl hydroxy chloride antiperspirant compositions, <- Previous Patent (Zinc complexes of ba...). This application is a division of our It is more complex and time consuming than those used to measure radiolabeled zinc levels. and about 15 mm Hg to give 46.8 gm product. Privacy Policy © 2004-2020 FreePatentsOnline.com. 2,906,668 for "ZIRCONYL AND ALUMINUM HALOHYDROXY COMPLEX" issued to Stewart M. Beekman, which discloses aqueous solution complexes of zirconyl halides with aluminum hydroxyhalides and a method for maintaining a high solution pH and preventing gelling. Nevertheless, the present invention represents further attempts to produce even better astringent aluminum compounds. 2,906,668 and 3,405,153, discussed previously. Alcohol soluble complexes of basic aluminum bromides may be prepared by adding zirconyl or zinc bromide or chloride, or zirconyl hydroxychloride or hydroxybromide, or mixtures of the above chlorides and bromides to an aqueous solution of five-sixths basic aluminum bromide, and drying the resulting mixture to a substantially friable solid, such as by vacuum or spray drying. Alternatively, the aqueous basic aluminum bromide solution could be prepared from a solid basic aluminum bromide having the desired Al/Br mol ratio, since such solids are readily soluble in water. & Terms of Use. The product dissolved in anhydrous SDA-40 in less than 0.75 hour to form a 30% solution with a CCl4 compatibility of 232 cc. It is also known that zinc salts and zirconium salts, such as zirconyl chloride (ZrOCl2 or zirconium oxychloride) are capable of preventing or retarding the exudation of perspiration from the skin and have been used or suggested for use in antiperspirant compositions. Thus, in order to be commercially acceptable for use in present day aerosol antiperspirant compositions, it is generally necessary that the astringent compositions meet the following requirements: 1. The alcohol soluble zinc and zirconium complexes of basic aluminum bromides and the methods of making the solid complexes of the present invention will now be described in more detail with reference to the following specific, non-limiting examples: 404 gm of zirconyl hydroxybromide (21.7% Zr) was added to 1,428 gm of 50% basic aluminum bromide (10.9% Al) giving an Al/Zr ratio of 6.0:1. The preferred solid complexes of the present invention will have a water content (both free and bound water) of about 15 to 30 weight percent based on the total weight of the solid and determined by Karl Fischer titration. A high performance liquid chromatographic (HPLC) method with spectrophotometric detection is presented for the assay of undecylenic acid, undecylenates (calcium, zinc), and the combination undecylenic acid-zinc undecylenate in commercial antifungal products. In particular, the pH's of the complexes of the present invention are generally inversely related to the halohydrocarbon compatibility. Thermo Fisher Scientific India Private Limited. Analysis: 16.4% Al, 9.7% Zn, 15.5% H2 O by Karl Fischer. Of course, due to the excellent carbon tetrachloride compatibilities of the complexes of the present invention, even higher concentrations may be used, thus yielding higher concentrations of the active ingredients.