GB2191184A

GB2191184A - Activated aluminum-hydrogen- oxygen complex and process of preparation and use

Info

Publication number: GB2191184A
Application number: GB08711267A
Authority: GB
Inventors: Fred B Bernat
Original assignee: UNITED STATES RES CORP
Current assignee: UNITED STATES RES CORP
Priority date: 1986-05-13
Filing date: 1987-05-13
Publication date: 1987-12-09
Also published as: CN87104316A; NL8701149A; DE3715963A1; AU7279887A; SE8701946L; JPS6325218A; ES2005573A6; KR870011043A; GB8711267D0; IT8720486A0; PH24020A; FR2598700A1; FI872098A0; FI872098A; IT1204594B; SE8701946D0

Description

GB 2 191 184 A 1

SPECIFICATION

Activated aluminum-hydrogen-oxygen complex and process of preparation and use The present invention relates to novel aluminum-hydrogen-oxygen complexes and processes for the 5 preparation of those complexes. In particular, the complexes contain aluminum, oxygen and hydrogen in certain proportions and forms such that the complexes are capable of use in compositions to control breakdown of organic material, for example, acne lotions, bleach creams, deodorants, depilatory composi tions and treatment of biological materials.

Commercially available non-prescription products which may be applied to the skin, such as cosmetics, 10 beauty aids, antiseptics, medicaments, deodorants, etc., work on the basis of either dilatant or astringent action on the skin pores. Neither is satisfactory with respect to the cure of acne.

Those compounds which utilize dilatant action may clear the skin of existing impurities but, as a result, the skin pores remain dilated for a considerable period of time, and thus are particularly susceptible to entrance of air pollutants such as sulfur dioxide and tar. The long term result of using such dilatant-action containing 15 products is that, after a short term "success" a worsened skin condition usually occurs.

Those compositions which utilize astringent action are usually applied after the cleaning of the skin with hydrogen peroxide or other strong oxidizing agents. While the oxygen from the hydrogen peroxide acts effectively and immediately, the subsequent action of the astringent prevents a "deep" cleaning of the skin.

Furthermore, compositions which are used on the skin must help eliminate unpleasant and offensive odors, 20 reduce skin irritations and dry oxygen lacking impurities on the skin, such as commidones (e.g. blackheads) or acne, depending upon the intended utility of these compositions. Because these compositions are to be used on the skin, they must also be bacteriostatic, non-toxic, non-irritant and completely safe.

The search has continued for new and improved compounds useful in compositions which are applied to the skin such as depilatory compositions, acne lotions, roll-on deodorants and bleach creams. This invention 25 was made as a result of that search.

Objects and summary of the invention

Accordingly, it is a general object of the present invention to avoid or substantially alleviate the above-discussed problems of the prior art. 30

More specifically, this invention provides an aluminum-hydrogen-oxygen complex which is capable of use in compositions which may be applied to the skin, and a process for preparing this aluminum-hydrogen oxygen complex. The new aluminum-hydrogen-oxygen complex may be applied to the skin in the form of solid or semi-solid compounds or in combination with one or more fluids. The new product may be used in the control of breakdown of biological material. 35 The present invention provides, in one aspect, a process for preparing an activated powder. This process consists of:

(a) contacting aluminum metal having a purity of at least about 99.94% by weight and containing at least trace amounts of silicon with a source of an acid of a type and concentration which will both remove and inhibit the formation of oxide on the metal; 40 (b) contacting the acid-treated aluminum metal with a source of mercury in an oxygen-containing atmosphere; and (c) partially immersing the mercury contacted aluminum in a hydrogen halide solution for sufficient time to begin the growth or formation on the mercury-contacted aluminum of a crystal like substance which is the activated powder. 45 In another aspect, the present invention provides the product produced bythis process.

In yet another aspect, the present invention provides a process for preparing a suspension of the aluminum-hydrogen-oxygen complex which is capable of releasing oxygen and hydrogen in the presence of a halogen-containing compound. This process consists essentially of:

a. contacting aluminum metal having a purity of at least about 99.94% by weight and containing at least 50 trace amounts of silicon with a source of an acid of a type and concentration which will both remove and inhibit the formation of oxide on the metal; b. contacting the acid-treated aluminum metal with a source of mercury in an oxygen-containing atmosphere; c. partially immersing the mercury contacted aluminum in a hydrogen halide acid solution for sufficient 55 time to begin the growth of a complex on the mercury-contacted aluminum; d. at least partially redissolving the complex in a hydrogen halide acid solution to form a suspension; e. cooling the suspension; and f. increasing the pH of the suspension to from about 5.0 to about 5.8.

The present invention also provides the suspension produced by this process. 60 Brief description of the drawings

For a better understanding of the invention, reference will be made to the accompanying drawings, wherein:

Figure 1 is a schematic sectional elevational view of an embodiment of the apparatus and ingredients used 65 2 GB 2 191 184 A 2 in the first two steps of the process of the present invention.

Figure 2 is a schematic view similar to Figure 1 showing a different embodiment of the first two steps of the process of the present invention.

Figure 3 is a schematic view similar to Figure 1 showing the formation of aluminum-hydrogen-oxygen complex on a non-immersed metal surface in a hydrochloric acid bath, which takes place during the third step 5 of the process of the present invention.

Figure 4 is a schematic representation of a Soxhiet apparatus in which is carried out the partial redissolution of aluminum-hydrogen-oxygen complex formed on a non-immersed metal surface.

Detailed description of the preferred embodiment 10

The aluminum-hydrogen-oxygen complex of this invention is a light, amorphous, super-oxygenated material, containing aluminum, oxygen, hydrogen and at least trace amounts of unassociated halogen. It is a critical limitation that the aluminum metal from which this aluminumhydrogen-oxygen complex is formed contain trace amounts of silicon in hexagonally structured form. The aluminum-hydrogen-oxygen complex does not burn and it is not explosive. 15 This aluminum-hydrogen-oxygen complex, which will be further described below, is believed to be A112(H20AlsH6 a blue-green amorphous material and forms a non-immersed metal surface during the process of this invention. This aluminum-hydrogen-oxygen complex initially is designated BB-1.

The term "activated aluminum- used to describe the aluminum from which the BB-1 is prepared means aluminum metal which has been treated with a source of mercury and subsequently exposed to partial 20 immersion in hydrohalic acid attemperatures of between about ambient and not more than about WC. In this "activated" state, the aluminum metal on the non-immersed surface remains in its elemental form, but is "clathratic" in that it entraps or confines therein "free" chlorine (or other halogen) in trace amounts.

Furthermore, the clathratically entrapped free chlorine enables the present aluminum-hydrogen-oxygen complex to release oxygen and hydrogen. 25 The structure of the trace silicon which is required to be contained in the aluminum metal used in this invention is two forms. The usual form is a spherical or cylindrical form but a small portion of the silicon is in a second form which is hexagonal in silhouette. In most instances throughout this description the silicon is measured as a total without regard to silicon structure. However, the presence of hexagonal silicon is believed to be critical, in order to attain the desired properties of the aluminumhydrogen-oxygen complex of the 30 present invention. Affixing a ratio of the two forms of silicon has been exceedingly difficult. it appears that in commercially available aluminum containing traces of silicon, the hexagonal silicon represents less than about 1 % of total silicon.

The aluminum-hydrogen-oxygen complex of this invention may be prepared by a multi-step process. The process will be described in connection with the drawings. 35 Utilizing the apparatus of Figure 1, an aluminum bar or rod (1) is placed in a vessel (2) which is made preferably of glass or other acid resistant material. A thin layer of a hydrohalic acid, preferably hydrochloric acid (3), is placed into the vessel such that the aluminum is slightly covered. The shape of the aluminum is not critical, although a bar or rod shape is generally preferred.

The purpose of the acid treatment is to remove any oxide from the aluminum surface, and to inhibit any 40 further development of oxide on the surface. The aluminum should be pure, generally at least about 99.94%, typically at least about 99.98%, and preferably at least about 99.99% pure. The purity of the aluminum may readily be empirically determined since the presence of oxides is demonstrated by an abrupt rise in temperature of the acid solution.

The aluminum metal should not be 100% pure, however. It is necessary that some silicon, generally from 45 about 30 to about 100, typically from about 45 to about 95, and preferably from about 60 to about 90 parts per million ("ppm---) total silicon be present in the aluminum. The use of less than about 30 ppm total silicon will lead to a complex which will not contain sufficient hydrogen and oxygen for the desired purpose. However if aluminum metal containing greater portions of hexagonal silicon were available than are now available lower total silicon content aluminum would be useful in this invention. The use of more than about 100 ppm total 50 silicon will result in process difficulties since silicon tends to heat up the solution and drive off the desired hydrogen and oxygen gases.

Other impurities, such as iron, may be present in the aluminum to the extent discussed above. The amount of iron present in the aluminum should generally be less than about 50, typically less than about 40, and preferably less than about 30% by weight of the silicon. It is desired to keep the iron content to a minimum 55 because iron tends to react with, and thus deplete, the oxygen in the system.

After immersion in the acid solution, the aluminum is then contacted or coated with a source of mercury, preferably by placing the aluminum in a bath or similar type of apparatus. This step is carried out in the presence of an oxygen gas-containing atmosphere, such as air. The mercury acts as a catalyst which effects a change in the aluminum structure. 60 The temperature at which these first two steps are carried out is not critical, but should not be such as to encourage oxide andlor chlorine gas formation. A temperature range of generally from about 10 to 45, typicallyfrom about 15 to about 35, and preferably from about 20 to about 30,'C may be used.

If desired, the acid and mercury contact may be made simultaneously as shown in Figure 2, where aluminum rod (1) is immersed in acid bath (3) and the heavier mercury bath (4). 65 3 GB 2 191 184 A 3 Regardless of whether the apparatus of Figures 1 or 2 or other suitable apparatus is used, the length of time of contact with the mercury may be relatively short, although longer contact is not detrimental. A time of generally at least about 15, typically from about 15 to about 60, and preferably from about 15 to about 30, seconds may be employed.

The mercury acts as a catalyst which effects a change in the aluminum structure. 5 The mercury contacted aluminum thus formed is then partially immersed in a hydrogen halide acid solution. A particularly preferred halogen forthis purpose is hydrochloric acid. This step results in the growth orformation on the non-immersed surface of the mercury contacted aluminum of the aluminum-hydrogenoxygen complex of blue-green amorphous material which is believed to be A11AH202)181-16.

The aluminum-hydrogen-oxygen complex appears as a growth or formation BB-1 -which is collected as a 10 powder-like substance and maybe utilized directly. Optionally, this material maybe further processed by the steps of (a) at least partially redissolving the complex in a hydrogen halide acid solution to form a suspension; (b) cooling the suspension; and (c) increasing the pH of the suspension to from about 5.0 to about 5.8 (131311 suspension).

The BB-1 complex maybe formed in a number of ways and the method thereof is not critical in and of itself. 15 For example, after contact with mercury, the thus treated aluminum rod or bar maybe partially immersed in another vessel, containing a bath of hydrochloric acid having a concentration which maybe empirically determined but which is generally from about 1 to about 2 normal. A blue-green amorphous material is then formed as the non-immersed metal surface. This growth is shown in Figure 3 wherein the complex (5) is denoted as forming above the acid bath on the non-immersed surface which when dried becomes a powder of 20 the BB-1 complex.

The temperature atwhich this complex is formed should generally be from about 5 to about 40, typically from about 20 to about 30, and preferably from about 22 to about 25,'C. A sudden adverse rise in temperature of the reaction environment atthis point may result if the aluminum starting material were not sufficiently pure. The temperature should not exceed 40' C because the desired hydrogen and oxygen gases of the BB-1 25 complex will be released at these higher temperatures. Temperatures less than 5' C are not desirable because the reaction rate is not usually commercially feasible at these temperatures.

In any embodiment, the complex is formed by treating oxide-free aluminum with mercury to change the structure of the aluminum and to effect its activation, and then contacting (or continuing to contact) the thus treated aluminum with hydrochloric acid by partial immersion to cause the formation of an aluminum- 30 hydrogen-oxygen complex on the exposed metal surface. The contacting step is carried out for preferably from about 75 to about 100 minutes. A blue-green BB-1 complex is the product of this step.

The BBA complex is then dried either at ambient temperature, or preferably in a convenient drying oven.

The heat applied must not be so high that chlorine gas is liberated. The temperature should be generally from about 5 to about 50, typically less than about 40, and preferably from about 20 to about 40' C. The relative 35 humidity should be preferably about 30%.

The length of time needed for drying may be empirically determined since it depends upon the thickness of the layer of complex and also upon the size of the drying oven. Usually drying requires generally from about to about 150, typically from about 50 to about 125, and preferably from about 75 to 100 minutes. A blue-green powder, BB-1, is the product of this drying step. 40 To form the BB-1 suspension the BB-1 powder is introduced into thimble (11) of a Soxhiet apparatus (12) as shown in Figure 4 Flask (13) of Soxhiet apparatus (12) is filled with a solution of a hydrohalic acid, preferably hydrochloric acid (14), which is preferably about 3 normal. Flask (13) is then heated by conventional means to the boiling point. The hydrogen chloride vapors penetrate Soxhiet apparatus (12) and, after condensation upon water cooled condenser (15), partially dissolve the powder within thimble (11), and are recirculated 45 within flask (13). This procedure maybe repeated until thimble (11) of Soxhiet apparatus (12) is empty.

The amount of time needed to carry out this partial redissolution step may be empirically determined, although generally from about 30 to about 200, typically from about 50 to about 150, and preferably from about 70 to about 120, minutes may be employed. The BB-1 powder is then recycled in a string acidic liquid such as hydrochloric acid. It is recycled partly in the form of a solution and partly in the form of a fine cloudy 50 suspension and is referred to collectively as BB-1 suspension.

After the suspension is cooled to a temperature of generally less than about 50, typically from about 15 to about 40, and preferably from about 20'to about 30' C, the pH of the complex is increased to generally from about 5.0 to about 5.8, typically from about 5.2 to about 5.6, and preferably from about 5.3 to about 5.5.

The pH maybe increased by treating it with a strong hydroxide such as sodium hydroxide or potassium 55 hydroxide. The concentration of the hydroxide is not critical and maybe generally from about 1 to about 4, typically from about 1.5 to about 3.5, and p referably from about 3 to about 4 normal.

This increase in pH may be monitored with a conventional pH meter.

The BB-1 suspension resulting from this process may be used in various formulae in the field of cosmetics, beauty aids, medicants, deodorants, etc--- in various percentages which may readily be determined 60 empirically.

This BB-1 suspension, even in small amounts, has the unique ability (in the presence of halogen salts) of releasing oxygen and hydrogen when used in an oxygen and hydrogen- containing composition, such as cosmetics, medicants, beauty aids, deodorants, etc. These compositions are frequently utilized on skin. It is to be understood that halides normally are present on skin, generally as a result of normal physiological 65 4 GB 2191184 A 4 processes, thus activating the BB-1 suspension.

The BB-1 suspension may be used in the following percentages by weight of the total composition depending upon end use: acne cream or lotion (about 3%), depilatory composition (about 4.5 to 5%), face cream (about 5%), underarm deodorant (about 3M.

The present invention is further illustrated by the following examples. All parts and percentages in the 5 examples as well as the specification and claims are by weight unless otherwise specified.

Example 1

This example illustrates the preparation of BB-1. Five hundred grams of aluminum metal rod, having not morethan 0.02% of impurities including about30 to 10Oppm silicon is placed in a 36 inch long shallow glass 10 vessel as shown by Figure 1. The aluminum is contacted with 3N hydrochloric acid at 20' C in amounts sufficient to coverthe aluminum rod. Thereafter, the aluminum rod is removed from the acid bath and immersed in a mercury bath for approximately 10 minutes under moist (relative humidity of about 30%) air-atmospheric conditions.

The mercury contacted aluminum rod is then partially reimmersed in a bath of 2N hydrochloric acid. A 15 growth is observed on all non-immersed portions of the surface of aluminum and the aluminum bar begins to dissolve in the hydrochloric acid bath on the immersed surface.

The blue-green amorphous material which begins to form on the nonimmersed surface is the aluminumhydrogen-oxygen complex referred to as BB1.

This material is collected and either used directly in deodorants, bleaches, depilatories, biological material 20 treatment, or is indirectly used in making complexes.

Example 2

This example illustrates an alternative method of preparing BB-1. The same procedure of example 1 is utilized however the starting material is an aluminum metal rod having not more than 0.02% of impurities and 25 from about 0.3 to about 1 ppm hexagonal silicon impurity therein.

Example 3

This example illustrates the preparation of BB-1 suspension. One hundred grams of the BB-1 complex of Example 1 is introduced into thimble (11) of SoxhIet (12). Flask (13) is filled with 1000 milliliters of 3N 30 hydrochloric acid (14) and heated to the boiling point. The hydrochloric acid continues to boil and then acidic liquid is recycled four times during a period of about 90 minutes. At that point, thimble (11) of Soxhiet apparatus (12) is empty, and the liquid in flask (13) of the Soxhiet apparatus contains a fine cloudy solution or suspension. After the suspension is cooled to about 20' C, a 3N potassium hydroxide solution is slowly added, until the pH increases to about 5.4. This pH increase is monitored with a Beckman pH-meter. At that point the 35 product - BB-1 suspension - may be used in specific cosmetic, deodorant, medicant and other formulations.

Example 4

The following example illustrates the use of the BB-1 suspension of the present invention in preparing a lotion useful fortreating skin conditions acne, in particular, the ingredients listed in Table 1 were used in the 40 weight percentages listed therein:

TABLE 1

Ingredient Percentage by weight 45 Deionized Water 65.419 BB-1 Suspension 3.000 MBS Special Richonate 6122 (Sodium Dodecylbenzene Sulfonate) 1.800 50 Potassium Xyiene Sulfonate 3.550 Citric Acid (Anhydrous USP) 0.366 Antifoam AF (Dow Corning) 0.005 SalicylicAcid 0.500 Perfume 0.050 55 Ethyl Alcohol 95% 23.000 Sodium Carbonate (Anhydrous) or Potassium Hydroxide 0.060 Supercel (Filter Aid) (Rohm & Haas) 0.250 Triethanolamine 2.000 60 100.000% The lotion is prepared by running the deionized water into a glass lined or stainless steel tank. The BB-1 suspension, sodium dodecyl benzene sulfonate, potassium xylene sulfonate, citric acid, and Antifoam AF are 65 GB 2 191 184 A 5 then added to the water.

The salicylic acid and the perfume are dissolved in part of the alcohol sufficient for solubility. The rest of the alcohol is run into the reaction tank. Then the solution of salicylic acid, perfume, and alcohol is then added to the tank.

The pH is adjusted to 3.0 using the sodium carbonate. The triethanolamine is then added. 5 The mixture is filtered at room temperature. Afilter aid is prepared by mixing a part of the Supercel with a part of the liquid mixture, and passing the concentrate through the filter until clear. The filter bed may be changed if necessary. Aging is not necessary.

If the reaction tank is stainless steel, the mixture is transferred to a glass lined storage tank or to drums if long storage is anticipated. 10 Example 5

This example illustrates the application of a complex of this invention in the field of health and beauty-aids, particularly the preparation of an acne-removing formulation:

The following ingredients set forth in TABLE 2 are mixed together in a blender until a homogeneous 15 composition is obtained.

TABLE2

Ingredient Percentage by weight 20 Deionized Water 65.419 BB-1 3.000 Sodium Dodecylbenzene Sulfonate 1.800 Potassium Xylene Sulfonate 3.550 25 Citric Acid (Anhydrous LISP) 0.366 Antofoa m AF 0.005 Sal icylic Acid 0.500 Alpine Perfume 6321 0.050 Ethyl Alcohol 95% 23.000 30 Sodium Carbonate (Anhydrous) 0.060 Supercel (Filter Aid) 0.250 Triethanolamine 2.000 100.000% 35 By Weight Of Total Composition This composition may be applied directly to skin containing acne lesions.

The BB-1 of this invention is believed to work in a manner substantially different from that of prior art 40 compositions. While it is slightly astringent, the present complex neither closes nor dilates the pores. Since it is rich in readily liberated oxygen and since it is activated by halogen salts such as sodium chloride (present in perspiration from the surface of the skin), this complex releases a constant and steady flow of oxygen.

Commidones (blackheads) are immediately attacked by this released oxygen. Since commidones are isolated foreign materials, which have no oxygen supply like the rest of the skin, it is thought that they become 45 11 oxygen-hungry". The oxygen from the complex penetrates the commidones readily and efficiently and dries them out, while the rest of the skin is unaffected. By using an oxygen carrier-compound such as described above the acne-removing formula, the affected skin is under control during the period of development of the acne.

This complex may be used in other compositions which are used on the skin. One such composition is an 50 underarm deodorant. Problems are encountered with prior art underarm deodorants in applying the correct amount to the underarm area. Too little will not be effective. Too much might irritate. The present complex, however, is non-irritating to the skin. Furthermore, the salt in perspiration triggers the release of hydrogen and oxygen. When the perspiration stops, the action of the aluminum- hydrogen-oxygen complex also stops.

When perspiration re-commences, the action of the complex also recommences. 55 Example 6

This example illustrates the preparation of a roll-on deodorant using the suspension of the present invention. The ingredients used in this example are set forth in Table 3 with the corresponding percentages by weight: 60 6 GB 2191184 A 6 TABLE3

Ingredient Percentage by weight Water For Vessel 13.00 5 Veegum (R.D. Vanderbilt) 0.43 Disodium Sequestrene No. 2 0.10 Water 37.23 Kisscowax-A-33 (McKesson & Co.) (PEG 400 MS) 2.89 Dupanol WA Paste (Dupont) (Mapsofix WA) 0.56 10 Allantoin 0.05 Glycerin 4.50 Isopropyl. Alc. 15.04 Tween 20 [Polyoxyethylene (20) sorbitan monolouratel 0.69 15 Methyl Parabene (Atlas) 0.17 Perfume W&J 6398) 0.15 BB-1 Suspension 25.00 Colors 20 Thewater isfirst added to a stainless steel steam tank. The methyl parabene isthen mixed until it is dissolved. Heating may be necessary to complete the solution.

The mixture is then cooled, and the Veegurn is sprinkled on the surface of the liquid mixture while mixing for about 15 minutes. After addition of the Veegum, the composition is mixed for another hour and the mixture is allowed to stand overnight. On the following day, the composition is mixed together with disodium 25 sequestrene No. 2, kisscowax, dupanol, allantoin and glycerin at 76' C until it is melted. The Veegurn solution is then heated to 710 C while stirring until a homogenous phase is formed. This homogeneous phase should be combined with the mixture of the other ingredients after mixing for 112 hour. The mixture is then cooled to 24' C. 30 A separate solution of isopropyl alcohol, Tween 20 and perfume (J&J 6398) is prepared. The mixture should 30 bestirred until clear and the clear mixture should then be added to the batch, at which time the BB-1 suspension should be added to the mixture over a period of about three hours. Q.S. to final volume with deionized water and colorthe batch to match the standard. Lab samples may be obtained after draining out two to three gallons of the mixture. The product generally keeps well for about one month after laboratory approval if stored in tightly sealed polyethylene bags or 35 stainless steel containers.

Example 7

The following example illustrates the use of BB-1 of the present invention in preparing a skin bleaching agent. The ingredients listed in Table 4 were used in the weight percentages listed therein: 40 TABLE4

Ingredient Percentage by weight 45 Hexamul AS (Hoechst) 12.0 Cetyl Alcohol 5.0 Propyl Parabene 0.1 Methyl Parabene 0.2 Citric Acid 0.3 50 Water 79.7 BB-1 Powder 2.0 Sodium Sulfide 0.3 Sodium Metabisulfite 0.2 Stannous Chloride 0.1 55 Dontill 200 (Dow Chemical) Include excess to allow for evaporation.

The water is added to the mixing vessel and heated to 82' C. Next, the methyl parabene is mixed in thoroughly, after which the stannous chloride is mixed in. 60 The heated mixture is reduced in temperature to 80' C and the hexamul AS, cetyl alcohol, citric acid and propyl parabene and methyl parabene mixed in.

The resulting mixture is cooled to 50' C and BB-1, sodium sulfide, sodium metabisulfite and Donflil 200 are thoroughly mixed in.

The resulting lotion is thus prepared and ready for application to skin. 65 7 GB 2 191 184 A 7 In a further application sewage maybe deodorized and the alkalinity reduced in concert with an oxygen enrichment that facilitates sewage breakdown.

This maybe accom p] ished by the addition of BB-1 to sewage. Due to the variable nature of sewage and the degree of deodorization or reaction rate desired specific ratios of BB-1 to sewage must be fixed with regard to the specific material being treated, temperature and other considerations obvious to those skilled in 5 the art. As a general range from about 1 gm to about 20 gms BB-1 per liter of sewage will prove satisfactory with about 2 gms to about 12 gms per liter being preferred.

While the scientific phenomena upon which this invention is based is notfully understood, and 1 do not wish to be bound by any particular theory, it is believed that the subgrain structure of aluminum appears to undergo profound changes when under chemical and electrochemical attack. 10 It is believed that the spheroidal shape of the silicon trace material in aluminum changes to the hexagonal shape as a result of the 'Wee chlorine" of the complex, and due to the interaction of the mercury-treated aluminum with the hydrochloric acid solution. One may observe hexagonal holes in the aluminum-hydrogenoxygen complex of this invention similar to the outline of the hexagonal silicon crystals. The properties of B13-1 are also believed to be related to a phenomenon which enables the complex of this invention to release 15 oxygen and hydrogen in presence of a catalyst.

Furthermore, when ordinary aluminum is introduced into an hydrochloric acid solution, e.g., 1 N or 2N, the production of aluminum chloride (and water) takes place. However, when the mercury treated aluminum which is used in the process of this invention is partially immersed in hydrochloric acid the behavior is quite different. While there still results the formation of aluminum chloride as well as other aluminum compounds, 20 after the passage of from about 8 to about 72 hours complex which begins as a blue-green amorphous material is formed on the non-immersed surface.

The principles, preferred embodiments, and modes of operation of the present invention have been described in the foregoing specification. The invention which is intended to be protected herein, however, is not to be construed as limited to the particular forms disclosed, since these are to be regarded as illustrative 25 rather than restrictive. Variations and changes may be made by those skilled in this art without departing from the spirit of the invention.

Claims

30 1. A process for preparing an aluminum-hydrogen-oxygen complex which comprises:

(a) contacting aluminum metal having a purity of at least about 99.94% by weight and containing at least trace amounts of silicon with an acid of a type and concentration which will both remove and inhibit the formation of oxide on said metal; (b) contacting said acid-treated aluminum metal with a source of mercury in an oxygen-containing 35 atmosphere; and c) partially immersing said mercury contacted aluminum in a hydrogen halide acid solution for sufficient time to beging the growth of the aluminum-hydrogen-oxygen complex on said mercury contacted aluminum.
2. The process of Claim 1 wherein said aluminum is at least about 99.99% pure and contains from about 30 to about 100 ppm silicon and less than about 40% by weight iron based upon the weight of said silicon. 40
3. The process of claim 1 wherein said aluminum is at least about 99.99% pure and contains from about 0.3 to about 1 ppm hexagonal silicon.
4. The process of claim 1 wherein said aluminum metal has a purity of at least 99.99% by weight, and contains from about 60 to about 90 ppm silicon and less than about 30% by weight iron based on the weight of said silicon; and the acid used is hydrochloric acid. 45
5. The process of any of Claims 1 to 4 wherein step (c) is carried out at a temperature of from about 5 to about 400C.
6. The process of claim 5 wherein step (c) is carried out at a temperature of from about 20'C to about 30'C.
7. The process of any of claims 1 to 6 which comprises also:

(d) at least partially redissolving said complex in a hydrogen halide acid solution to form a suspension; 50 (e) cooling said suspension; and (f) adjusting the pH of said suspension to from about 5.0 to 5.8.
8. The process of claim 7 in which said complex is at least partially redissolved in a hydrogen chloride acid solution; the resulting product is cooled to a temperature less than about 50OC; and the pH of said cooled product is adjusted to from about 5.3to about 5.5. 55
9. The process of any of claims 1 to 8 wherein the said aluminum-hydrogen- oxygen complex forms on, and is collected from, the non-immersed portion of the mercury contacted aluminum.
10. The process of claim 1 substantially as hereinbefore described.
11. The productof the process of anyof claims 1 to 10.

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Published by The Patent Office, 25 Southampton Buildings, London WC2A lAY, from which copies may be obtained.