DE2036625A1 - Oxygenated aluminum complex, process and apparatus for making the same - Google Patents

Description

July 25, 1970 "R-55772

George Gergely MEEKL, 517 Boulevard, New Milford, N.J., V.St.A.

"Oxygenated Aluminum Complex, Process and Apparatus to make the same "

The present invention relates to an oxygen-containing one Aluminum complex and method and apparatus for producing the same. The complex contains oxygen in an atomic ratio of aluminum to oxygen greater than 2: 3 and more up to about 85% by weight of oxygen 15 wt .- $ aluminum. The complex is made by reacting aluminum of selected purity with mercury and hydrogen chloride acid reacted in the presence of an oxygen-containing atmosphere in a plant, the devices for temperature control of the reaction and devices for continuous removal of the complex from the reaction zone owns.

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It is known that aluminum is only monobasic oxide, p forms in different hydration states. There is no known aluminum oxide that has oxygen in an atomic ratio of aluminum to oxygen greater than 2: 3. The classic approach therefore assumes that Aluminum can reach a maximum oxidation level of +3.

The present invention relates to an aluminum-oxygen complex in which there is up to about 85 wt .- ^ oxygen to 15 wt .- $ aluminum. The atomic ratio of aluminum to oxygen is therefore far above the ratio of 2: 3.

If one were to postulate an aluminum oxide for this, the aluminum would have to have a valence state well above +8. Such a postulate would violate all recognized rules of atomic theory in chemistry. In addition, it has been found that the complex described here ^{emits gaseous oxygen when heated above 100 °} C. and X-ray and electron diffraction studies show a non-crystalline, amorphous structure. One is therefore compelled to conclude that something other than a simple combination of aluminum and oxygen is being disclosed here.

It does not contradict the analysis of the complex claimed here and a theoretical evaluation of the reaction process to draw the conclusion that it is a aluminum clathrate containing oxygen.

While organic clathrates are relatively common, inorganic clathrates are rare and have previously been considered chemical oddities viewed. There are no inorganic

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just see through clathrates. Use of extremely high temperatures and prints made. There are no known methods for the industrial production of inorganic clathrates of technical merit. The present invention relates to processes for relatively inexpensive, technical production an oxygen-containing aluminum clathrate of significant technical usefulness.

A clathrate represents an expanded atomic lattice of a Element or a compound, in which another element or another compound is included is. There are complex forces of attraction that hold the trapped substance back in the basic lattice. In the case of a trapped gas, however, an increase in temperature generally creates conditions which favor the escape of the trapped substance.

The present oxygen-containing aluminum complex appears as an extremely light, porous, structurally self-supporting but relatively fragile, bluish-white plague substance with a low density. Starting generally about 10O ⁰ C at atmospheric pressure, the complex emits oxygen serving as gaseous diatomic oxygen appears in the immediate vicinity of the complex, with a very high purity, ultra-high-purity alumina remains. ·

The complex has many uses, for example as a source of gaseous diatomic oxygen, as Gas separating agent, as liquid cleaner, cosmetic Porters, porters and additional oxygen provider for flammable compounds, drug for burns, i'iltermittel, Intermediate product for the production of crystalline gases and many others too numerous to be they could be cataloged.

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The process for preparing the complex basically involves the reaction of metallic aluminum of high purity and free from surface oxides with mercury and hydrochloric acid in the presence of gaseous oxygen.

The oxygen-containing aluminum complex claimed here is made of exquisite purity with the conversion of aluminum liquid mercury and hydrochloric acid in the presence of gaseous oxygen under controlled conditions Temperature conditions established

The assumption that the oxygen-containing complex by changing the usual crystal lattice of metallic Aluminum, opening the lattice to absorb and hold oxygen ions, is formed, does not violate observation and reaction analysis. The change in the aluminum grid is due to high-energy short-wool UV radiation of the order of 1,000 angstroms reaches which either leads to a dissolution or reorientation of the aluminum-hydro-aluminum crystal bonds

At the same time it ionizes. the same radiation as the surrounding oxygen _; which is present as gaseous, diatomic oxygen in the atmosphere in which the metallic aluminum is located. As soon as the aluminum crystal lattice changes, ionized oxygen enters and is held in place with the formation of an aluminum clathrate.

In the preferred embodiment of the present invention, the UV radiation originates from excited atoms of the liquid mercury in resonance with chlorine derived from hydrochloric acid.

The process for preparing the aluminum complex can be

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take any alternative forms and include the preferred methods and procedures set forth below a, '■'

The choice of aluminum.

us it was found that the presence of impurities in metallic aluminum either the production of aluminum oxide favored at the expense of the desired complex or reduced the yield of the complex in some other way » It has been found that the resonance between mercury and chlorine for generating UV radiation is correct Energy of the amount of hydrogen ions or proton absorption depends on the mass of the metallic aluminum. Those impurities in the aluminum which the rate and extent of absorption or diffusion of hydrogen ions or protons in the mass lowering the aluminum, therefore lowering the yield of the aluminum complex in favor of the formation of ordinary Aluminum oxide, these impurities are chromium, copper, iron, silver, molybdenum, nickel, and tungsten Cobalt.

Conversely, certain metals promote the diffusion of hydrogen ions or protons into the aluminum mass. Dissolvable metals are cesium, vanadium, zirconium, thorium, lanthanum, Hafnium, titanium, thallium, palladium and columbium.

Aluminum rods or wires with about 5 wt .- $ copper and Magnesium impurity 2 wt .-% are readily available commercially and are used to produce useful amounts of the Aluminum-oxygen complex. When using However, complexes made of aluminum of such purity contain significant amounts of trapped nitrogen. Nothing-

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nevertheless greater Augbeuten aluminum complex, no significant amounts of nitrogen may contain and unge ferry 85 wt .- # oxygen to 15 wt .- $ Aluminum has be produced by the use of aluminum containing less than 0.01 i "impurities . The aluminum complex produced with such extremely high-purity aluminum is physically more self-supporting and has a higher degree of stability with regard to spontaneous breakdown and conversion to aluminum oxide.

For example, if the magnesium is in amounts greater than 0.02 # occurs, the final product complex has a tendency to completely disintegrate in the course of a relatively short period of time and transform into alumina. It is believed that magnesium even in such relatively small amounts causes a disintegration of the oxygen inclusion created by the aluminum grid, as a result of Excitation of the magnesium pollution generated radiation.

The allowable amount of a given impurity or combination of impurities must be determined in terms of their influence or their total or combined influences, if any, ' on the yield ^ by favoring the formation either of aluminum oxide at the expense of the complex or due to the formation of the complex in unstable form or with undesirable large amounts of nitrogen.

The above-mentioned metals which promote the diffusion of hydrogen ions or protons can be used in Amounts from 0.05 to 1.0 wt. $ Can be used. One should also note that the presence of metals which do this; tend to diffusion of hydrogen ions or To inhibit protons, intentionally in relatively low levels

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Quantities can be used to speed up the reaction as long as their use does not unduly adversely affect the yield or quality of the final product complex. Metals or impurities which tend to inhibit the diffusion of hydrogen ions or protons, to be used in amounts of more than 5 wt .- ^.

“The physical form of the aluminum metal must match that other reaction events are consistent. In a preferred embodiment of the method, this is aluminum partially immersed in a bath of liquid mercury. From the point of view of operational expediency, In contrast to chemical necessity, it is therefore preferable to use self-supporting rods or the like to choose, as opposed to loose powder. In addition, with loose powder, the surface of the Aluminum is enlarged so much that the reaction rate is too great. If the reaction speed increases excessively, the effective or increases The internal temperature of the reaction increases so much that the yield of aluminum complex is reduced. It was found, that aluminum rods meet all the requirements mentioned above and technically in the required purity obtainable to relatively high yields of the aluminum complex, the maximum. Amounts of oxygen and minimal: Contains amounts of nitrogen.

Manufacture of aluminum . _#

The implementation depends on how much the liquid mercury penetrates the aluminum rod. The surface of the Aluminum should therefore be free of oxides, which tend to reduce both the absorption of mercury and the To hinder hydrogen ion absorption. Experience showed

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that no complex formed over the parts of the stick, those because of an oxide layer or because of the presence of other foreign substances not from a mercury film were covered.

Under normal circumstances, aluminum, when exposed to air, quickly takes on a relatively thin but uninterrupted surface oxide film in the form of Al ₂ O. The AloO can be removed from the aluminum by any of a number of well known methods. In a preferred embodiment of the present invention for preparing the complex, hydrochloric acid is used for this purpose. Although AlpO, is not soluble in hydrochloric acid, it penetrates the oxide layer down to the aluminum and causes delamination of the oxide and effective deoxidation of the surface of the aluminum.

In addition, hydrochloric acid can be effective as oxide stripping reagent as it acts as a Reactant is used, which interacts with the mercury and aluminum to generate to stimulate and entertain by UV radiation of suitable wavelengths in order to change the aluminum crystal lattice to effect.

The reaction vessel:

The reaction is preferably carried out in a device which is described in more detail later. Nonetheless the reaction vessel must be chemically inert to attack by any reagent, in particular to liquid mercury and hydrochloric acid. It has been found that many metals, ferrous metals, Aluminum, copper or copper alloys and the like

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be attacked by the respondents. In addition, most plastics contain impurities, which can be leached from the plastic and which tend to poison the implementation.

In addition, it is desirable to use a reaction vessel which as much of. the relatively high-energy and short-wave UV radiation that reflects through the implementation is generated.

With these desires in mind, it has been found that inexpensive, ordinary glass vessels are most suitable. Such Vessels are not attacked by the reagents nor do they introduce impurities or poisoning substances through absorption or leaching and they tend to reflect UV radiation.

Theoretical-chemical and nuclear-chemical reactions:

The following chemical and nuclear-chemical reactions are theoretically probable and agree with the observations match. Nonetheless, the mechanism of the reaction is not yet clear enough to be asserted with certainty to be able to ensure that the following reactions actually take place as they are postulated. However, it is believed that the following reactions take place and they serve for a general explanation of the reaction process.

It has been found that the aluminum is relatively free of surface oxides have to be. It has also been found that hydrochloric acid is the only acid suitable for both removing the surface oxides as well as bringing about the reaction to produce the aluminum complex.

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Hydrochloric acid removes the surface oxides Aluminum by a relatively well known process. Although aluminum oxide is not soluble in hydrochloric acid the vapor pressure of hydrochloric acid is sufficient large to penetrate the oxide and thus attack the metallic aluminum underneath. The hydrochloric acid attack on the aluminum under the surface oxide film causes the film to peel off and thus be eliminated the surface oxides. The reaction between aluminum and hydrochloric acid is carried out by the following known equation shown:

A1 + HC1 Al ⁺³ + Cl ~ + H ₂ (1)

The reaction between aluminum and hydrochloric acid is exothermic. The heat of this exothermic reaction initiates at least the process by which UV radiation is generated to change the aluminum crystal lattice. Nonetheless, the greater part of the whole seems Heat of reaction does not come from the reaction between aluminum and hydrochloric acid. On the contrary, it seems as if the greater part of the heat is generated 'after the reaction has been initiated' and how it is seems, it comes from the bulk of the aluminum itself. From a thermodynamic point of view, the transformation of the aluminum crystal lattice seems to be exothermic

Nevertheless, it has also been found that the reaction zone comprises both an exothermic reaction and an endothermic one, which is described in more detail below in the discussion of the thermodynamics of the implementation.

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In order to produce the aluminum complex claimed here "is it is necessary to bring liquid mercury into contact with the surface of the aluminum rod. aluminum is not easily wetted by mercury. Aids can be applied, including using of compounds containing mercury. Y / enn e.g. mercury-II-oxide is used as a mercury-containing compound, it can be assumed that liquid mercury by simple decomposition of the Queek Silver II oxide in Presence of ordinary light is generated as it is is shown in the equation below:

HgO H _g + 0p (2)

It has also been found that the aluminum goes with the mercury can be related by first treating the surface oxides by using hydrochloric acid removed and immediately poured liquid mercury over the surface of the rod or the Immersed rod in a mercury bath.

Experience has shown that the change in the aluminum crystal is caused by the conversion of high-purity aluminum with Mercury and hydrochloric acid in the presence caused by an oxygen-containing atmosphere.

It is believed that the change is at least partially caused by high-energy, short-wave UV radiation will. UV radiation with a wavelength on the order of 6000 angstroms is relatively ineffective at to produce significant yields of the complex, and in the Indeed, it can happen under the circumstances that

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no complex disfigured at all. Significant yields of complex are believed to occur only when the UV radiation has a wavelength on the order of 3000 angstroms or less. On the basis of theoretical calculations, an optimal wavelength of approximately 1000 angstroms has been postulated. It is also assumed that wavelengths less than 700 angstroms / duktauf cost of oxygen significantly increase the relative amount of nitrogen in the Endpro- wherein the nitrogen in amounts of from 10 ° / o or more occurs.

It is believed that the UV radiation is "generated" in the following manner. The reaction between aluminum and hydrochloric acid is exothermic, causing mercury atoms to become so strongly excited that their electrons are in the outer Orbital can be raised to a higher energy level. Such mercury atoms are unstable and fall spontaneously back to the original level. During the relapse, the electrons of the outer orbital go back to its normal energy level ^ and it becomes UV radiation of the desired wavelength range of approximately 700 to 3000 angstroms are generated depending on the temperature conditions in and around the reaction zone. These Response can be represented by the following equation:

0 + ο

Hg + DH Hg Hg + 8 (3)

wherein Hg is mercury in the unexcited state;

DH the exothermic energy or the conversion between. Represents aluminum and hydrochloric acid;

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Hg means mercury in the excited state; 8 represents UV radiation.

It is believed that there is a resonance between the above reaction of mercury and l · a chloride ion and Hydrogen gas occurs in the following manner. The chloride ion from the hydrochloric acid is absorbed to a limited extent Amounts of UV radiation from the mercury returning to its ground state. The chloride ion is absorbed by the UV radiation is excited, causing its electron in the outer orbital to a higher energy level is raised. As in the case of mercury, the excited chloride ions spontaneously revert to the ground state, producing photons, which can be represented by the following equation;

ο +0

Cl + 8 Cl Cl + 0 (4)

wherein Cl "represents a chloride ion in the unexcited state;

Cl represents an excited state chloride ion; and

j # means photons.

Similarly, hydrogen gas is released by the reaction between hydrochloric acid and aluminum. It was observed that the conversion of aluminum to the complex is greatly promoted when hydrogen gas is passed over the aluminum

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minium in contact with hydrochloric acid conducts. It will therefore assumed that hydrogen atoms are also caused by UV radiation from mercury which has returned to its ground state are excited in the same way as the chloride ions. When the excited hydrogen atoms fall back more photons are emitted, as shown in the following equation:

ο +

Hg + 8 H ₂ H ₂ + JZi (5)

wherein H _{2 is} hydrogen in the unexcited state;

H _{2 represents} hydrogen in the excited state.

Photons produced by the relapse into the ground state of both excited chloride ions and excited hydrogen atoms are absorbed by the mercury atoms, with the electrons in the outer orbital be raised to a higher energy level. The mercury atoms spontaneously revert to their basic state, with additional UV radiation being emitted until resonance occurs between the atoms of mercury, chloride ions and hydrogen. When there is resonance, you have a sufficient sustained source of UV radiation of the desired wavelength to completely convert the To effect aluminum in the converted complex.

As is well known, the unchanged aluminum crystal contains about 12 electrons at the junctions of the aluminum

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minium atoms. The exact course of the transformation is not entirely clear. The assumption that the UV radiation with a wavelength of about 1,000 Angstroms ionizes oxygen atoms in the immediate vicinity of the aluminum and removes at least 2 electrons, however, does not contradict the observed finding. At the same time, the bond between one or more aluminum atoms in the crystal is either broken or distorted to such an extent that the usual crystal lattice structure opens up. When the crystal lattice is opened, oxygen ions penetrate the interatomic spaces and a new structure is formed. In the new structure, which is amorphous, electrons that originated either from the oxygen atoms during ionization or from the bond between aluminum atoms _; trapped in the altered structure in the same way as the oxygen ions.

It has been found that if the reaction is allowed to proceed rapidly, the exothermic phase of the reaction predominates, with the result that the effective reaction temperature rises. If the effective reaction ^{temperature is above approximately 100 °} C., the nitrogen present in the surrounding air is also included with the oxygen in the end product complex. Lower temperatures favor oxygen more as an enclosed gas than as nitrogen. Theoretically, this phenomenon can be explained by the more energetic UV radiation that is generated at higher temperatures.

It has also been found that other gases present in the surrounding atmosphere can be trapped by the Generation of UV radiation in the ionization region of these gases.

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Although the present invention is particularly concerned with the production of the oxygen-containing Concerning the aluminum complex, other interesting reactions leading to the production of by-products were observed led. In one embodiment of the method, an aluminum rod approximately 19.05 mm in diameter is used (3/4 inch) bent into a circle lying in one plane. The bent rod is put in a flat jar and so on a lot of mercury added so that about half the surface of the aluminum rod is immersed. About the mercury hydrochloric acid is poured out, which is in contact with the aluminum. The usual procedures those with reference to the removal of surface oxide are reproduced in detail below, and the temperature control is followed.

In this embodiment of the method, the oxygen-containing one occurs Aluminum complex as a curtain that rises from the treated upper surface of the aluminum rod and expands rapidly upwards as a ring-shaped curtain. However, there seems to be another reaction beneath the surface of mercury to take place. It was found that during the reaction a solid by-product, apparently in crystalline form, is deposited on the bottom of the vessel near the aluminum rod. This solid by-product gives off ammonia gas when heated and is believed to be an ammonium complex acts, although its exact composition is not determined became.

It was also found that the implementation, which the oxygen-containing aluminum complex supplies, is exothermic. However, the reaction that supplies the ammonium compound is endothermic.

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A quantitative core activation analysis of a representative Sample of the oxygen-containing aluminum complex leads to the following result: ■

Ingredient wt .- $

Aluminum 15

Oxygen 83-75

Nitrogen 1-2

The pure end product complex does not contain any other components, but traces of mercury are usually found and chlorine mechanically included in the test sample. In addition, with decreasing aluminum purity increasingly larger amounts of alumina found shortly after the reaction, either during the Conversion formed or resulted from the conversion of unstable final product complex to aluminum oxide. The above analysis is representative of the final product complex consisting of an aluminum rod with $ 99.99 Purity stems from ..

It has also been found that the use of highly concentrated hydrochloric acid, more concentrated than two normal, promotes a greater yield / time ratio and produces a considerably more stable end product which is resistant to spontaneous conversion to alumina. The use of hydrogen gas in the reaction also increases the yield / time ratio and promotes the stability of the end product. The final complex is diatomic oxygen starting from about 100 ⁰ C. In the range of 100 ⁰ C there is an instantaneous loss of about 30 wt .- ^ in the form of gaseous, diatomic acid

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fabric on. When heated to approximately 80O ⁰ C, an additional release of 25 wt .- ^ takes place.

Analysis of the final product complex is consistent with the conclusion that there is a ratio of at least 5 oxygen atoms to one aluminum atom, and in some cases an even greater ratio. It is therefore reasonable to conclude that oxygen is not bound to the aluminum, as is the case with classical aluminum oxide with ionic bonds. Otherwise the aluminum would have a valence level of at least +10 and even higher. Such a valence state is at least extremely unlikely, if not impossible. Under conditions which favor the inclusion of nitrogen, one has a ratio of nitrogen atom ¹ to aluminum atom greater than that which would be consistent with the formation of aluminum nitride complexes. So one is led to the conclusion that nitrogen is also included as a nitrogen ion in the aluminum lattice. The ionization potential of nitrogen is known to be higher than that of oxygen, so experience has shown that it is compatible with observation to conclude that the generation of UV radiation with a shorter wavelength favors the inclusion of nitrogen at the expense of oxygen. Other gases can be included in a similar manner.

Response parameters

Stoichiometry; _t

It was found to be less than the stoichiometric Amounts of hydrochloric acid and mercury, ent

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used neither as liquid mercury nor as a mercury-containing compound in relation to converted aluminum can be. As for hydrochloric acid, there is the stoichiometric criterion is that the chlorinated water The amount of acid is just sufficient to essentially bare the surface oxides from the aluminum and sufficient heat is generated to cause continued animal UV radiation to be generated Introduce aluminum, mercury and hydrochloric acid. It is clear that if the aluminum has been previously stripped of the surface oxides, then less hydrogen chloride will be used acid must be used.

Very small amounts of hydrochloric acid appear compared to aluminum, sufficient. Also is the concentration of hydrochloric acid itself is not decisive for the formation of the final product complex, but it is crucial with regard to the yield / time ratio and the stability of the final product complex. In practice the hydrochloric acid should not be below 0.1 normal. Using 'a more concentrated Hydrochloric acid increases the yield / time ratio and the stability of the product.

For example, it has been found, but not limited to, that about 100 grams of aluminum wire are in An acceptable end product can be converted by using approximately 28.35 to 141 »7 grams (1 to 5 ounces) of 2N hydrochloric acid used. With regard to mercury, it is seen from the point of view of stoichiometry desirable to use an amount just enough to cover the surface of the aluminum to be converted cover. However, a lower amount of mercury does not limit the conversion reaction itself, but rather

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only a limitation of the reaction yield. That stoichiometric criterion for mercury is that just as much mercury, either as liquid Mercury or as a mercury-containing compound, is present that the desired amount of aluminum in the final product complex is converted.

For example, those mentioned above can be treated with 28.35 to 141.7 g (1 to 5 ounces) of 2N hydrochloric acid 100 g of aluminum wire can be practically completely converted into the complex if one uses about 10 g Mercury-II-Oxide mixed. The Mercury II Oxide is placed as a powder in the reaction vessel and the Reaction vessel stirred until the powder appears to "substantially" cover the aluminum wire. Nevertheless, it is desirable swerter, the mercury than the mercury bath in which an aluminum rod is placed on the side to apply to the aluminum. In this case it should be so much Mercury are added so that the rod is immersed practically to its center. Besides that. will mercury in the preferred embodiment of the present method for heat dissipation used, which will be explained in more detail later is described.

With respect to both mercury and hydrochloric acid, it must be remembered that both are Aid for generating UV radiation of a suitable wavelength, preferably in the bulk of the aluminum itself, can be used. Nevertheless, the aluminum conversion process takes place under radiation conditions, as above mentioned, takes place on the surface of the aluminum, which does not withstand the source of the origin of the radiation, In addition, the aluminum can be mechanical or chemical any other expedient means of removal

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the surface oxides are pretreated than by the use of hydrochloric acid. Nevertheless, the use of hydrochloric acid and mercury leads to a fairly simple and efficient conversion process with an end product of high purity. In addition, the hydrochloric acid provides the chloride ions required to resonate with the mercury and protons, thus creating a permanent source of UV radiation.

Under ordinary circumstances, when the implementation in air atmosphere is carried out, the oxygen stoichiometry is not a problem. Oxygen gets into the air from the air absorbed by the conversion process determined amounts. It is clear that if the proceedings are carried out in an open, a vessel accessible to air is carried out, a large excess of oxygen is available. Lack of oxygen and the effect of oxygen starvation was therefore not observed. Since it was found that the A complex can absorb about five times as many oxygen atoms as there are aluminum atoms such excess oxygen must be achievable to make maximum use of the conversion process. A stoichiometric criterion for sufficient oxygen to remove the changed aluminum grid under room conditions to completely saturate is therefore desirable but not a chemically limiting factor for the conversion process self.

Thermodynamics of implementation ;

The thermodynamics of the implementation are demanding and can be decisive under given conditions.

The basic reaction involves two sources of exothermic energy:

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The first source is the conversion between aluminum and hydrochloric acid; the second source is the transformation process itself, presumably due to the breaking or reorientation of the bonds between the aluminum atoms in the aluminum crystal.

If the reaction is carried out in a bath of liquid mercury, an endothermic reaction takes place the surface of the mercury, thereby forming a by-product that contains ammonia. The speed of response for the formation of the oxygen-containing Aluminum complex is a puncture the size of the aluminum surface exposed to the atmosphere is. Likewise, the reaction rate for the formation of the by-product is below the mercury level also a puncture the size of the aluminum surface beneath the surface of the mercury.

The reaction temperature immediately adjacent to the aluminum exposed to the atmosphere should (80 to 12O ⁰ P), and preferably at about 37.8 ⁰ C (10O ⁰ P) in the range from 26.7 to 48.9 C ^0. At the upper limits of the temperature range, the inclusion of larger amounts of nitrogen in the oxygen-containing aluminum complex is favored. If the upper temperature range is exceeded significantly, no oxygen-containing aluminum complex is produced. It has been found that the yield at about 65.6 ⁰ C (150 ⁰ P) is negligible. In addition, as the temperature increases above the desired level, larger amounts of simple aluminum oxide are produced. Lower temperatures accelerate the conversion process if it is carried out with aluminum, which is coated with mercury but not immersed in a mercury bath; when the aluminum is immersed in a mercury bath, lower temperatures favor lower temperatures

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Temperatures the formation of the ammonium-containing by-product complex under the surface of the mercury.

If the effective reaction temperature in the range (130 to 135 ⁰ P) of 54.4 bis.57,3 ⁰ C, undergone substantial and significant amounts of nitrogen in amounts of about 15 ⁰ Jo in the oxygen-containing Aluminiumkqmplex.

The rate of reaction, and consequently the rate of generation of exothermic heat of reaction, is also influenced by the purity of the aluminum used. Alloying means, as mentioned before, which the Inhibit proton diffusion in aluminum, reduce the reaction rate and the temperature of the reaction. This contamination affects, but also the yield / time ratio of the final product complex and its oxygen content and stability.

Those alloying agents which promote diffusion promote in aluminum, increase the reaction rate and potentially increase the yield / time ratio. However, if the reaction rate is so fast as to cause excessive temperature rise, so will the overall yield is reduced and the inclusion of nitrogen in the complex is favored.

Therefore, many factors have to be balanced in order to keep the effective reaction temperature within relatively narrow limits to keep the oxygen concentration in the end product complex to a maximum and the yield / To raise time ratio.

It has been found practical that the reaction is most preferably carried out using a relatively thick one

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lying on the side and partly in a mercury bath immersed aluminum rod is carried out. The mercury then serves to dissipate heat and tends to Attenuation of sudden and drastic temperature changes in the reaction. The use of a mercury bath however, it is accompanied by other problems related to the reaction temperature. In the course of the reaction The aluminum absorbs quantities of mercury, which increase its specific weight. As a result, it tends the aluminum, which usually floats in the mercury,

fe to sink deeper into the mercury as the reaction progresses. If the aluminum sinks significantly below its center line, the reaction is dampened and actually stopped. If, however, the electrode is lifted out of the mercury substantially above its center line, the reaction proceeds rapidly as a puncture of the surface of the aluminum rod, with increasing amounts of heat being generated. The yield / time ratio increases up to a point on which the effective reaction temperature is dependent. If the reaction temperature exceeds the optimal level, about 37.8 ⁰ C (100 ⁰ P) to decrease the time ratio, the yield / begins. When the reaction rate is so fast that the temperature increases

™ about 65.6 ⁰ C (15O ⁰ P) increases, the conversion stops. It has also been found that as the reaction temperature rises, the absorbed mercury tends to leak out of the aluminum. In a state where the reaction breaks out, the aluminum rod heats up so strongly that it expels (dries out) significant amounts of mercury, whereby it floats even higher in the mercury due to the decrease in specific weight and thus the temperature rises even further until the Reaction stops.

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Pole nuts if a mercury bath is used. Devices to control the mercury level on the aluminum rod are available. By doing the Queeksilver like that The effective reaction temperature and the yield / time ratio can be controlled on the aluminum rod carefully controlled.

It has also been found that the mechanical hydrogen chloride acid level in and around the aluminum electrode is also important when using a mercury bath. The hydrochloric acid must be an extremely "thin film." on the surface of the mercury covering the aluminum rod. It was found that if the hydrochloric acid film is too strong, it tends to as Y heat drain on the bared surface of the aluminum to act, cool the reaction and wash away the final product complex before it has time to act as to form an upwardly extending curtain. Experience has shown that the thickness of the hydrogen chloride film must be controlled v / earth so that the development of the final product complex as a curtain on the exposed surface of aluminum can take place.

Humidity :.

It has also been found that moisture plays a role in the development of the final product complex. Different as the temperature, the humidity is not critical within such narrow limits. Generally speaking, if the surrounding The atmosphere is excessively dry or excessively humid, the yield / time ratio is adversely affected. It is believed that moisture induces the conversion, transformation reaction through complex and ingenious effects impaired proton diffusion. Nevertheless, experience has shown found that the relative humidity at

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best kept near $ 50, being a relative wide range is permitted.

Preferred reaction technology ;

The preferred reaction technique comprises the following stages:

1. An aluminum rod 1.27 to 2.54 cm (1/2 to 1 inch) in diameter is bent into an in-plane circle. The aluminum should have less than 0.01 ° / o impurities.

2. The aluminum rod is treated with two normal or more concentrated hydrochloric acids to Stripping off surface oxides.

3. The stick is placed in a flat, cheap, flat-bottomed glass bowl that has so much liquid mercury in it is filled so that the aluminum rod is exposed along its entire length above its center remain.

4. The mercury is quickly poured over the bared surface of the aluminum rod until the aluminum rod is completely wetted by the mercury.

5. Two normal or more concentrated hydrochloric acids is poured onto the surface of the mercury next to the aluminum rod, making a relative thin layer of hydrochloric acid is formed, which extends over the rod. which is now wetted with mercury.

6. Allow the reaction to proceed with the temperature of the aluminum rod immediately adjacent to its surface

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maintained at about 37 »8 ° C (10O ⁰ P). Meanwhile, an annular curtain of oxygenated aluminum complex forms on the exposed surface of the aluminum rod and extends upward.

7. The temperature of the reaction can be controlled by measuring the depth of immersion of the aluminum rod in the Mercury controlled.

8. Other devices to control the temperature of the reaction can be installed under the reaction vessel in the form of a heat exchanger.

9. The relative humidity of the ambient atmosphere should be about 50 i "and the air in and around the surface of the aluminum rod must be relatively motionless.

10. The oxygen-containing aluminum complex, which turns out to be If an annular curtain forms on the aluminum, it can be removed periodically if desired.

It is interesting to mention that the aluminum rod symmetrically from above and below the surface of the mercury is eroded so that its cross-section is horizontal obtains an elliptical shape, as shown in FIG is. However, depending on the depth of the aluminum rod in the mercury during the reaction, erosion can result lead vertical-elliptical cross-sectional shape, which is greater than the surface of the mercury above, as shown in FIG.

Careful monitoring of complex formation on the bared Aluminum surface above the mercury bath level shows an area immediately above the surface of the

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R-55772 Jj

Aluminum which does not appear to be in contact with the complex forming thereon; the only apparent contact between the aluminum rod and the complex is on the sides of the rod adjacent the interface with the mercury bath. The curtain of oxygenated aluminum complex appears to form from the bottom and push the top up, but there is no apparent visible contact between the surface of the aluminum rod, or more correctly, the surface of the aluminum and hydrochloric acid which coats the aluminum rod, and the best visible bottom parts of the aluminum complex. Pur generated by the above-mentioned preferred technique, oxygen-containing aluminum complex is characteristic in that it contains approximately 15 i »aluminum to $ 85 oxygen with relatively small amounts of nitrogen. The complex is. chemically stable and mechanically relatively stronger than complexes that are formed from aluminum of lower purity. The complex appears as an extremely light, porous, pale blue-white mass that can be broken into a powder which, apart from given limits, is pressure-resistant. Relatively small amounts of a matt, white, extremely fine powder are also formed, which is known to be a highly pure, fine-grained aluminum oxide which is clearly different in physical appearance and chemical properties from the aluminum complex product. '

Although the above technique from _# many reasons is preferred, many other techniques which produce the aluminum complex may be employed. A number of examples of other working techniques that can be used are given below, but these are not intended to restrict the scope of the present invention.

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R-55772 AS

example 1

(a) 100 g of aluminum wire, either in one piece or on. appropriate V / else divided, with no more than about 0.01 i <> impurities and practically free of Oberflächenoxyd be in air, acid vapors, hydrochloric includes, hanged.

(b) Before surface oxides can form, this will be Aluminum with UV radiation in the wavelength of approximately 1000 angstroms irradiated from a suitable external source.

(c) the temperature is maintained at approximately ⁰ ° C .; the pressure is atmospheric.

(d) The irradiation is continued until the aluminum is practically completely converted to the aluminum complex is.

example

(a) 100 g aluminum rod with no more than $ 0.01 impurities is bent into a ring and placed on the bottom of a flat glass vessel.

(b) Liquid mercury is introduced into the vessel, it covers about half the cross-section of the aluminum rod.

(c) Add 2, On hydrochloric acid to the vessel, that it floats on the mercury and occupies the aluminum rod at all points.

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R-55772 3O?

(d) Stir or immerse the rod in the mercury and hydrochloric acid until the mercury is all Wet rod.

(e) Leave the aluminum rod wetted with mercury in the mercury and hydrochloric acid bath, while the aluminum complex grows up from the top of the rod.

(f) The temperature is around room temperature and fc the pressure is approximately atmospheric pressure.

Example 3

(a) 100g aluminum wire with no more than about 0.01 # Contaminants are placed in a glass jar with the aluminum wire generally upright in it.

(b) About 28 ^ 35 to 141.7 g (1 to 5 ounces) of one approximately 2'On hydrochloric acid is added to the vessel and the jar is shaken vigorously until the aluminum is practically freed of the surface oxides is.

(c) Add approximately 10 grams of powdered mercury oxide, either red or yellow, to the jar and shake it Vessel vigorously until the aluminum wire is essentially covered with the powdered mercury (II) oxide seems to be.

(d) The vessel is left open in the air until practically all of the aluminum has been converted into the finished aluminum complex.

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R-55772 ti '■.

(e) The temperature (7O ⁰ P) held during the conversion at about 21.1 ⁰ C; the pressure remains at atmospheric pressure. ,

Example 4

The procedure described in Example 3 above is followed with the exception that the mercury (II) oxide is replaced by a Amount of about 40 g of mercury (II) chloride is replaced.

example

The procedure described in Example 3 above is followed except that the mercury (II) oxide is replaced by a Amount of approximately 75 g of mercury (II) sulfate replaced will.

Example 6

The method described above in Example 3 was followed except that the aluminum wire with mercuric oxide was coated, and the mercury-II-oxide was reduced to mercury, the temperature was lowered to about 2O ⁰ C, whereupon the reaction strongly accelerated.

Example 7

(a) Approximately 100 g aluminum wire with no more than about 0.01 i "impurity werdai suspended in air.

(b) The aluminum wire is coated with about 2, On chlorinated water

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chemical acid sprayed in an amount just enough to remove the surface oxides from the aluminum wire.

(c) A fine spray of liquid mercury. will appear the aluminum wire is straightened until the aluminum wire is essentially coated with mercury, whereupon one allowing the reaction to proceed to completion.

Example 8

The method according to Example 3 is used, with the Exception that after the addition of the mercury (II) oxide the Aluminum wire with intensive additional UV radiation in the wavelength range of approximately 1000 Angstroms from a suitable one external source is irradiated from.

example

The procedure of Example 3 is used, with the exception that during the conversion and after the addition of mercury (II) oxide, hydrogen gas over the aluminum wire is directed; the hydrogen gas accelerates the conversion.

Example 10

(a) 100 grams of aluminum wire containing no more than about 0.01% contamination, freed from surface oxides, is placed in a generally horizontal tray in a reaction vessel.

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R-557.72 '33

(b) The tub is partially filled with liquid mercury, so that some of the aluminum protrudes above the surface of the mercury and there is an amount of 2.0 normal hydrochloric acid in the vessel that sufficient to cover at least part of the aluminum wire, which protrudes from the mercury to bring into contact with it and part of the aluminum wire with the surrounding oxygen-containing atmosphere in contact. ·

(c) allowing the reaction to proceed, not (12O ⁰ P) and is preferably used at an effective reaction temperature is higher than about 48.9 ⁰ C at much lower temperature until the final product "of the aluminum complex as a light, porous Pestsubstanz to light that grows up on the surface of the aluminum wire into the surrounding air.

Preferred embodiments of a device.

The preferred method of making the complex described herein is preferably in a model device carried out in which temperature, humidity, pressure and atmospheric composition, as well as other parameters, can be carefully controlled. A preferred embodiment of such a device is shown in the drawings illustrates:

Pigur 1 is a side view of a sectional view of an apparatus for generating the oxygen-containing Aluminum complex;

Pigur 2 is an enlarged side view of a sectional view of a reaction vessel, the DAR in Pigur. 1 is set;

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R-55772.

Figure 3 is a side view of a sectional view of a: partially reacted aluminum rod;

Figure 4 is a side view of a cross-sectional view of another aluminum rod that is partially reactive but has under different conditions than the one shown in Figure 3.

Turning now to the details of the drawings: The model apparatus comprises a generally closed one Housing 11 with side walls 12 and 13 and a removable cover 14. The cover 14 is provided with valve openings, to maintain pressure and atmospheric conditions inside the housing 11. The housing 11 contains a plurality of reaction devices in a stacked arrangement, one of which is shown in FIGS 2 illustrates

Each of the reaction devices comprises a generally inverted, truncated, conical, funnel-shaped product container 16 »which is supported by the pillars 17, 17 which are fastened to the bottom 18 of the housing 11. Of the Product container 16 is provided with a circular opening 19 in its bottom. Under the opening 19 is a continuous conveyor belt 20 is attached for emptying, and prepared to receive the oxygen-containing aluminum complex produced in the above apparatus. The continuous discharge conveyor belt 20 does not extend longitudinally through the housing 11 and over one end of it. Although the reaction is generally carried out at atmospheric pressure, it can sometimes it may be desirable to use other than atmospheric pressure. In such circumstances the conveyor belt must 20 go through a conventional airlock, which is not shown.

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R-55772 }

A transverse hanger 21 extends between the side walls 12 and 1.3 in the vicinity of the cover 14 through the housing 11. A supply line as a carrier Large diameter 22 is attached to hanger 21 and is suspended therefrom into housing 11. Die Supply line 22 extends upward through opening 23 in cover 14 and is fitted with a fitting 24 for the connection of the supply lines.

The supply line 22 runs downward from the hanger 21 to near the top of the container 16. A pair of identical reaction stations 25 and 26 are rigidly attached to the supply line 22. Each reaction station 25 and 26 is identical and detailed in FIGS Piguren 3 and 4 shown.

Each reaction site includes a generally annular frame 27 that is rigidly attached to the supply line 22 which extends downward through an opening in the center of this frame. The frame 27 carries an annular Heat exchanger 28 with inner tubes 29 etc. for the circulation of a temperature-controlling fluid. A Reaction vessel 30, which is preferably made of inexpensive glass, is on top of the heat exchanger 28 attached. The reaction vessel 30 is provided with an upright annular baffle plate 31, which an annular basin 32 delimits.

The supply line 22 is with a variety of pipes for bringing various gases and liquids for the reaction carried out in Basin 32 is equipped. A central multipurpose pipe 33 is in the supply line 22 provided for the passage of compressed air. A plurality of radial, generally horizontal, air ducts 34, 35 are connected to the multipurpose line 33

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R-55772

and extends ·. radially outwards through the supply line 22 immediately above the top of the reaction vessel 30. Each of the lines 34 and 35 is connected to a terminal · nozzle 36 or 37, which air that emerges from them at high speed into a narrow, conical stream.

The heat exchanger tubes 29 in the heat exchanger 28 are provided with multipurpose tubes by inlet and outlet tubes 38 and 39, respectively 40 and 41 connected in the multi-purpose line 21. There are also a variety of multi-purpose lines for Feeding of other reactants extending down through line 22. For example, the multipurpose line is 42 is connected to a radially extending line 43 which goes out through the multi-purpose line 22 and ends in basin 32 near its top. "

The radial line 43 is provided with an electrically controlled valve 44.

There are similar general purpose lines 45, 46 and 47 connected to radially extending lines 48, 49 and 50, respectively and each terminate in the basin 32 near its top. Each of the conduits 48, 49 and 50 is connected to a electrically controlled valve 51, 52 and 53 respectively.

The multipurpose line 42 supplies hydrochloric acid into the basin 32 through the electrically controlled valve 44. Similarly, line 45 delivers liquid mercury into basin 32 through electrically controlled valve 51. Multipurpose lines 46 and 47 can be used to bring any reagent of choice into basin 32, E.g. gaseous oxygen, gaseous nitrogen, helium, argon or any other gas that is fed into the Want to include aluminum complex «,

_ 36 10982 0/2268

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A plurality of vertically adjustable electrode or rod supports 54 and 55 are generally in positions in the basin 32 attached from the same distance. Each of the carriers 54 has a vertically movable table 56 which is in the Floor is recessed and carries a ring-shaped aluminum electrode or an aluminum rod, 57 «by an electric Remote signal, the supports 56 can be raised and lowered to the level of the aluminum electrode in the Control basin 32. Mercury is released into the basin 32 through the multipurpose conduit 42 and the control valve 44 guided and forms a pool 58 which extends from the side wall 59 of the reaction vessel 30 to the retaining wall 31,

The housing 11 is also provided with humidity control devices 60 equipped, which are set so that the relative humidity in the housing 11 in the desired range is held, In addition, the walls 12 and 13 are with Pensters 61 and 62 are provided, which can be opened.

Each of the reaction vessels 30 and each reaction station is in operation 25 and 26 of each device are charged with at least one aluminum electrode 57. Though only If an aluminum electrode has been shown, a number of aluminum electrodes can also be in concentric but spatially separated circles exist. Before the electrode 57 is brought into the reaction vessel 30, it is with it With the help of hydrochloric acid freed from surface oxides and preferably after the previously described immersion and casting techniques pre-wetted with mercury. The basins 32 are filled with so much mercury through the utility line 45 and the electrically controlled valve 51 is filled to reach a level at which approximately half the surface of the aluminum electrode 57 is covered. Then a small amount of hydrochloric acid is added to each of the Basins 32 with the help of the multiple line 42 and the elec-

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R-55772

trisch controlled valve 44 initiated. The hydrochloric acid 63 floats on top of the mercury and forms a film over the top of the electrode Then the reaction takes place.

It quickly forms a ring-shaped upright position Curtain 64 of the oxygen-containing aluminum complex, which extends upward to a position generally compared to the nozzles 36 and 37. Then compressed air is introduced through the multi-purpose line 33, which leads to the outside goes through the nozzles 36 and 37 and the relatively fragile Curtain 64 of the aluminum complex to the outside over the upper edge 65 of reaction vessel 30 pale. The parts of the aluminum complex 66 that extend from the top of the curtain 64 blown away, fall down into the conical container 16, go out through the passage 19 and fall onto the conveyor belt 20 ″. The conveyor belt 20 conveys the complex 66 out of the housing 11.

A heat exchange. ©?; -! Medium passes through inlet line 40, enters the pipe 29 of the heat exchanger 28 and goes through the multipurpose line 41 to the outside. The temperature the reaction can be controlled by careful control of the temperature of the heat exchange medium. The level of the aluminum electrode 57 in the mercury bath 58, which is fixed by the movable support 56 can also be used to control the temperature of the reaction will. The reaction temperature can be measured by sensors near the electrode or by visual observation to be determined.

The electrodes erode in the course of the reaction and absorb mercury, especially if the temperature of the Reaction is controlled. The level of electrode 57 must must therefore be constantly monitored and changed in order to

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R-55772 3

term surface area of the electrode above the level of the Mercury bath 58 must be observed. In addition, some of the hydrochloric acid is consumed and its level must can also be maintained in basin 32.

- 39 -

Claims (39)

R- 5 5 77 2 TV _2 5 ._Noye mb e r "19 ZO PATESTAISPHÜCHE: 1. Process for the production of an oxygen-rich Aluminum complex, characterized in that one (a) Aluminum <e purity with as much liquid QuecHf- ^{75 /;} brings silver and hydrochloric acid into contact that the aluminum is essentially wetted and at least partially penetrated by mercury, and in an oxygen-containing atmosphere (b) the temperature is maintained at a temperature no higher than that which will allow the formation of an aluminum complex containing no less than about 70 percent by weight oxygen on the aluminum. 2. The method according to claim 1, characterized in that the temperature in the immediate vicinity of the aluminum is kept at a value which is not higher than about 65.6 ⁰ C (150 ⁰ I ¹ ). 3. The method according to claim 1, characterized in that the aluminum contains no more than about 5 i « copper and 2 ia magnesium as impurities. 4. The method according to claim 1, characterized in that the aluminum has no more than about $ 0.01 impurities contains. 5. The method according to claim 4, characterized in that the temperature is maintained in the immediate vicinity of the aluminum at a level of not higher C (10O ⁰ P) than about 37.8 ^0th - 40 109820/2265 R-55772 6. The method according to claim 4, characterized in that the temperature in the immediate vicinity of the aluminum between approximately 26.7 to 65.6 ⁰ C. (80 to 150 ⁰ P) is maintained. 7. The method according to claim 4ι, characterized in that the temperature in the immediate vicinity of the aluminum between approximately 26.7 to 48.9 ⁰ G (80 to 120 ⁰ P) is maintained. 8. The method according to claim 4, characterized in that the metallic aluminum partially in a bath liquid mercury is immersed, whereby part of the aluminum is wetted with mercury and is absorbed into the surrounding, oxygen-containing atmosphere is enough and the hydrochloric acid floats on top of the mercury and is in contact with the aluminum. 9. The method according to claim 8, characterized in that the hydrochloric acid as a thin PiIm over at least a portion of the aluminum extends above the surface of the mercury bath. 10. The method according to claim 8, 'characterized in that the temperature in the immediate vicinity of the aluminum is kept at a value which is not higher than about 65.6 ⁰ C (150 ° P). 11. The method according to claim 8, characterized in that the temperature in the immediate vicinity of the aluminum at a level that is held, the non than about 48.9 ⁰ C (120 ⁰ P) is higher. 12. The method according to claim 8, characterized in that that the temperature in the immediate vicinity of the aluminum - 41 - 109820/2265 originally inspected R-55772 · W a value is held, not higher than about 37.8 ⁰ C (10O ⁰ P). 13 · The method of claim 8, characterized in that the temperature is between about 48.9 ⁰ C and 57.3 ⁰ C (120 and 135 ⁰ P) is maintained. 14. The method according to claim 8, characterized in that the temperature between approximately 26.7 ⁰ C and * 48.9 ⁰ C (80 to 120 ⁰ P). 15. The method according to claims 10, 11, 1.3 or 14, characterized in that the temperature is maintained at least in part by the fact that the immersion depth of aluminum in the mercury bath. 16. Procedure after. Claim 10, characterized in that that the hydrochloric acid is at least approximately 2 is normal. 17 · The method of claim 16, characterized gekennzeich- W net, that the temperature is maintained at a value which is not higher than about 57.3 ⁰ C (135 ⁰ P). 18. The method according to claim 16, characterized in that the temperature between approximately 26.7 and 48.9 ⁰ C (80 and 120 ⁰ P) is maintained. 19. The method according to claim 16, characterized in that the temperature is maintained at least in part is that one regulates the immersion depth of the aluminum in the Queoksilberbad. - 42 109820/2265 R-55772. ■ · ^ 20. The method according to claim 9 »characterized in that the hydrochloric acid is at least about 2 normal and! Temperature in the immediate vicinity of the aluminum at least in part by between about 26.7 and 57.3 ⁰ C. ⁰ C (80 and 135 ⁰ F) it is kept that one regulates the immersion depth of the aluminum in the mercury bath. 21. The method according to claim 4, characterized in that that the'metallic aluminum is partially immersed in a bath of liquid mercury, part of the Aluminum is wetted with mercury and reaches into the surrounding oxygen-containing atmosphere, the hydrochloric acid is not weaker than about 2 normal and in contact with the aluminum on the surface of the Mercury floats. 22. The method according to claim 21, characterized in that the temperature is maintained at least in part is that one regulates the immersion depth of the aluminum in the mercury bath. 23 · Device for the production of an oxygen-containing Aluminum complex, characterized by (a) a housing, (b) a plurality of reaction devices in the housing, (c) a relatively shallow vessel in each device, (d) Devices to allow gas flow over the top to conduct each vessel, (e) Containers under each vessel. - 43 109820/2265 2038625 R-55772 .M- «f 24. The device according to claim 23, characterized by devices for the continuous introduction of liquid reactants in each vessel, 25. The device according to claim 23 »characterized by support devices in each vessel, the support devices being vertical from outside the housing are adjustable. 26. The device according to claim 23, characterized by devices for continuous monitoring and Control of the relative humidity in the housing. 27. "· Device according to claim 23» characterized by devices for controlling the temperature, the
liquid reactants in each tube. 28. The device according to claim 23 »characterized by vertically adjustable support devices within of each vessel and devices · for temperature control of the liquid reactants in each Vessel. 29. The device according to claim 26, characterized by devices for heating and quenching liquid Reactants in each vessel. 30. · Device according to claim 26, characterized by a heat exchanger which is in a heat-exchanging Correlation to the respective vessel. 31. The device according to claim 23, characterized in that - 44 - 109820/2265 R-55772 I. by that each vessel is ring-shaped and has a central one Has passage, a multipurpose conduit generally vertically through the central passage in each vessel goes, a multipurpose gas line in this line to a Source of compressed gas is connected and a plurality of nozzles connected to a multipurpose gas line which rises radially outward, generally horizontally, across the top of each vessel. ■ 32., Apparatus according to claim 29 »characterized in that at least one multi-purpose feed line for liquid reactant in the multipurpose line is connected to reactant sources and a radially extending feed line for liquid reactants to the respective feed line for liquid reactant is connected for the respective vessel and opens into the vessel. 33. Process for the preparation of an oxygen-containing Aluminum complex, characterized in that aluminum purity in an oxygen-containing '' Atmosphere is irradiated with UV radiation of a wavelength that is short enough to cause the formation of a To cause aluminum complex on the aluminum containing not less than about 70% oxygen by weight. 34. The method according to claim 33, characterized in that the aluminum contains no more than about 5 1 » copper and 2 # magnesium as impurities. - 45 - 109820/2265 R-55772 35. The method according to claim 34, characterized in that the wavelength of the UV radiation is in the range of approximately 700 Angstroms to 3000 Angstroms. 36. The method according to claim 35, characterized in that the UV radiation is generated 'by the aluminum
contacted with liquid mercury in the presence of hydrochloric acid. 37. Procedure after. Claim 33, characterized in that that the aluminum contains no more than about $ 0.01 impurities. 38. The method according to claim 37, characterized in that the wavelength of the UV radiation is in the range of approximately 700 ar ^ ström to 3000 angstroms. 39. The method according to claim 38, characterized in that the UV radiation is generated by the
Aluminum with liquid mercury in the presence of
Hydrochloric acid contacted. 109820/2265 Blank page