Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F7/00—Compounds of aluminium
  • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
  • C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F7/00—Compounds of aluminium
  • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F7/00—Compounds of aluminium
  • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
  • C01F7/021—After-treatment of oxides or hydroxides
  • C01F7/025—Granulation or agglomeration
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F7/00—Compounds of aluminium
  • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
  • C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
  • C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination

Definitions

• the invention is directed to the production of alumina from aluminous raw materials by a wet chemical process.
• a suspension is produced from the ground aluminum-containing raw material, to which caustic soda is added.
• the suspension is processed at temperatures between 100 and 320 ° C and pressures up to 35 bar for several hours.
• the by-product is red mud.
• CARBONATES BY RECYCLING CONDENSATES ON DIGESTION UNDER PRESSURE OF MONOHYDRATE BAUXITES is used, for example, for the processing of
• Bauxites containing more than 1.5% calcium carbonate are proposed to process the ground bauxite with a solution containing aluminate and caustic soda.
• the processing requires a large number of series-connected autoclaves. After processing under pressure, a multistage separation of the suspension is carried out to remove water and water
• nepheline For the processing of nepheline, a modified Bayer process is used.
• the ground nepheline is mixed with ground limestone.
• the mixture is roasted at a temperature of 1100-1300 ° C.
• the roasted product is suspended in water and extracted from the suspension
• Silica from the solution is treated with carbon dioxide. In this way, aluminum hydroxide, sodium carbonate and potassium carbonate are recovered. Aluminum hydroxide is filtered from the solution and then washed. The solution is then included with recovery of the
• the processing of kaolin is essentially carried out with sulfuric, nitric or hydrochloric acid.
• the milled kaolin is processed at high temperatures of 150 to 350 ° C with the acids, in the case of nitric and hydrochloric acid under elevated pressure. In this way, the corresponding salts of the metals contained in kaolin form silica and silica.
• Water-soluble salts are separated from the settled substances.
• Disadvantages of the illustrated method are the high energy consumption in the acid processing of kaolin and the high corrosion activity of 95% sulfuric acid. Therefore, high-alloy steel or acid-resistant ceramics are required as the material of the equipments. A particular difficulty is the separation of the water-soluble heavy metal salts from the solution of the aluminum salts.
• Alumina is ground and mixed with dilute acids, thermally processed, filtered, impurities are removed from the solution. After concentration of the solution is the
• Aluminum salt hydrolyzed to aluminum hydroxide By thermal treatment, alumina and the acid used are recovered.
• Lignite has been proposed various acid and alkali processes.
• CO2 gas is processed to aluminum hydroxide and soda.
• the alumina is separated and calcined.
• Aluminum hydroxide is separated and calcined. Disadvantages of the illustrated method are the high energy consumption, the high corrosion activity under the reaction conditions of the acid extraction of aluminum hydroxide from the fly ash and the great difficulties of the separation of impurities from the aluminum salt solution. These problems result in the problems in the practical experiments
• Ultrasonic generators the actual consumption of electrical energy is 3-10 times.
• Alunite particles forms a silica film, which is the separation of the
• Aluminum hydroxide obstructed. It is an object of the present invention to provide a process for recovering a hydroxide from an aluminum-containing raw material
• Compounds are present, characterized by the following steps: a) optionally grinding and / or aluminum-containing raw material; b) preparing an aqueous suspension of the aluminum-containing
• Suspension with an electromagnet e) optionally admixing a chemical activator in the form of an amino compound, in particular in the form of a basic scleroprotein hydrolyzate, to the suspension; f) processing the suspension by a step of applying energy in the form of one or more of the following steps:
• Alumina / aluminum hydroxide by treatment with a membrane electrolyzer Alumina / aluminum hydroxide by treatment with a membrane electrolyzer.
• silicon oxide / silicon hydroxide and / or other inorganic compounds is to be understood as meaning an aluminum-containing raw material which comprises aluminum oxide / aluminum hydroxide which is chemically bound to other inorganic compounds in such a way that First, the crystal band must be resolved to the
• Alumina / aluminum hydroxide release is the kaolin (or its pure form kaolinite), whose structural units are two-dimensionally infinite networks of SiO-tetrahedron (tetrahedral layer) and Al (0, OH) octahedron (octahedral layer), which to a polar built unit to be stored together.
• alumina / aluminum hydroxide is in such a chemically bonded form or, so that the
• Crystal structure / mineral structure must first be dissolved to the
• a core step of the method according to the invention is the processing of the suspension of the aluminum-containing raw material with a step of
• Crystal structure / mineral structure of the aluminum-containing raw material so that the alumina / aluminum hydroxide can be separated in the later process.
• Rehbinder material refers to the change occurring in the hardness and ductility of a solid at the interface to a liquid, especially in the presence of
• the plastic is surface-active substances.
• the plastic is surface-active substances.
• the plastic is polystyrene foam
• Crystal structure / mineral structure succeeds by this combination of measures according to the inventive method is completely surprising for the expert.
• Ultrasonic generators with an output of 4000 - 5 000W / m 3 over 20-180min.
• an aluminous raw material selected from one or more of fly ash, kaolin, bauxite, nepheline, alunite, dawsonite, bentonite, andalusite, and kyanite is used.
• the grinding and / or screening takes place in step a) to a particle size of about 20 to 70 microns.
• a particle size has proved to be particularly favorable in order to achieve optimum results in the subsequent process steps.
• an unsaturated fatty acid preferably oleic acid
• the fatty acid especially in the form of oleic acid, acts as
• suspended aluminum-containing raw material and the added fatty acid have proven to be particularly favorable to a suspension with ideal
• the flotation in step c) is carried out by treatment in a conventional flotator, wherein subsequently aluminosilicates and / or metal oxides are separated in the form of the resulting foam.
• aluminosilicates and / or metal oxides are separated in the form of the resulting foam.
• aluminum silicates and / or metal oxides can already be separated off at an early stage of the process according to the invention.
• step d) by contacting the suspension with an electromagnet.
• This is preferably done by a treatment in the flotator, in which the suspension is passed to an electromagnet.
• a chemical activator in the form of an amino compound is added to the suspension prior to the step of processing by a step of the action of energy.
• This step of chemical activation enhances the effect of splitting the Crystal structure / mineral structure in the subsequent step of the action of energy (step f)).
• the admixing of a chemical activator in step e) is carried out so that 0.2 g to 5 g of an amino compound, preferably basic scleroprotein hydrolyzate, are admixed per liter of the suspension.
• the processing of the suspension by the action of energy in step f) takes place in the form of one or more of the following steps:
• Tube flotator for about 20 to 180 minutes
• Tube flotator for about 5 to 30 minutes.
• Substance is selected from a group consisting of nonionic
• surfactants e.g. Ethoxy polyoxylates of the 7th
• polymeric anionic surfactants e.g. Carboxymethylcellulose, basic polyacrylonitrile hydrolyzate.
• Alumina / aluminum hydroxide can be separated from the other components.
• step f) Silica, in step f) so that the suspension is allowed to stand for about 10 to 15 hours in a settling tank and then from
• Alumina / aluminum hydroxide is preferably subjected to a further agglomeration step so that it can be separated from the liquid phase.
• the agglomeration of the aluminum oxide / aluminum hydroxide present in the suspension preferably takes place in step h)
• Crystal structure / mineral structure of the aluminum-containing carbon is made possible when the aluminum-containing raw material prior to preparing an aqueous suspension of the aluminum-containing raw material in step b) an additional mechanical activation of the aluminum-containing raw material is subjected by grinding in a planetary mill or vibration mill.
• Alumina / aluminum hydroxide is preferably further processed after the agglomeration step by agglomerating
• Alumina / aluminum hydroxide in step h) is calcined at about 1,000 to 1,300 ° C.
• sulphates such as potassium sulphate in the case of the alunite
• the process of the invention generally does not require increased
• the process according to the invention is preferably carried out at room temperature, the optional calcination step being of course carried out at elevated temperature.
• the process according to the invention is carried out at a temperature of about 50.degree. C. to 60.degree.
• the 1500 g kaolin pattern was milled with 15 g of atrium carbonate and screened with a 60 micron sieve. Then 51 of an aqueous suspension having a concentration of 300 g / l were prepared.
• the sediment of 659 g contained 96.4% of silica and 1.8% of alumina. 8.
• the milky suspension was heated to 60 ° C after addition of 10 g of monoethanolamine. After a period of 1 hour at 60 ° C, 30 g of calcium chloride were added. After a further life of 12 hours at room temperature, the sediment (20g calcium silicate) of the
• Electrolyzer The processing took place for 5 minutes with 4 volts and 3 amps. In this process, the cleaning and agglomeration of the
• Aluminiumhydroxides and the deposition of the initially added oleic acid are aluminium and the deposition of the initially added oleic acid.
• Washed tap water dried at 130 ° C for two hours and calcined at 1100 ° C for one hour.
• the yield of alumina was 397.4g, i. 92% of the total aluminum oxide contained was extracted.
• Raw materials were made with commercially available mills and sieves. To prepare the suspension, vessels with mixers and equipment for dissolving chemicals are required. The molecular disintegration of the aluminum-containing raw materials was similar to a pilot plant Tube flotation performed. Excentric vibrators were used for the mechanical vibration and diaphragm compressors for the pneumatic vibration. The steam vibration was carried out with the help of steam generators. For ultrasonic treatment piezo elements and generators were used. The separation of the products after the molecular disintegration was carried out by settling tanks and separators. The final removal of silica was carried out at temperatures of 50-60 ° C by gravitational separation.
• the agglomeration of the aluminum hydroxide was carried out in membrane electrolyzers in the anode compartment and subsequent separation and washing of the settled aluminum hydroxide.
• Aluminum hydroxide was dried at 130 ° C in a drying oven.
• Calcination was carried out in a muffle furnace at a temperature of 1100 ° C
• Example 1 A sample of 1500 g of bauxite was ground with 15 g of sodium carbonate and sieved with a 60 micron sieve. Subsequently, an aqueous suspension with a concentration of 300 g / l was prepared. To the suspension was added oleic acid in a ratio of 300 g / t. After treatment in the flotator, the suspension was attached to an electromagnet with a field strength of 90 KA / M
• Aluminum hydroxide (alumina) from bauxite are shown in Table 1.
• Example 5 Analogous to Example 1, but using lignite fly ash instead of bauxite. The results of the experiments on the separation of alumina
• Lignite fly ash are shown in Table 5.
• Example 6 Analogously to Example 1, but instead of air, the suspension was processed with steam from a steam generator. The results of the experiments are shown in Table 6.
• Example 7 Analogously to Example 2, but instead of air, the suspension was processed with steam from a steam generator. The results of the experiments are shown in Table 7.
• Example 8 Analogously to Example 3, but instead of air, the suspension was processed with steam from a steam generator. The results of the experiments are shown in Table 8.
• Example 9 Analogously to Example 4, but instead of air, the suspension was processed with steam of a steam generator. The results of the experiments are shown in Table 9.
• Example 10 Analogously to Example 5, but instead of air, the suspension was processed with steam from a steam generator. The results of the experiments are shown in Table 10.
• Example 11 Analogously to Example 1, but instead of air, the uspension was processed for 5-30min with vibrations of a vibrator. The results of the experiments are shown in Table 11.
• Example 12 Analogously to Example 2, but instead of air, the suspen- sion was processed for 5-30 minutes with the vibrations of a vibrator. The results of the experiments are shown in Table 12.
• Example 14 Analogously to Example 4, but instead of air, the suspension was processed for 5-30min with vibrations of a vibrator. The results of the experiments are shown in Table 14.
• Example 15 Analogously to Example 5, but instead of air, the suspension was processed for 5-30min with vibrations of a vibrator. The results of the experiments are shown in Table 15.
• Example 16 Analogously to Example 1, but instead of air, the suspension was sonicated for 5-30min. The results of the experiments are shown in Table 16.
• Example 21 A sample of 1500g of bauxite was ground with 15g of sodium carbonate and screened with a 60 micron sieve. Subsequently, an aqueous suspension having a concentration of 300 g / l was prepared. To the suspension was added oleic acid in a ratio of 300 g / t. After treatment in the flotator, the suspension was attached to an electromagnet with a field strength of 90 KA / M
• the suspension was passed to an electromagnet with a field strength of 90 KA / M. After separation of
• Example 24 Analogously to Example 23, however, a sample of nepheline was processed and in the tube flotation CC> 2 gas was used. The results of the experiments are shown in Table 24.
• Suspension was added to oleic acid in a ratio of 300 g / t.
• the suspension was passed to an electromagnet with a field strength of 90 KA / M. After separation of the dimagnetic and ferromagnetic admixtures, the suspension and a
• Suspensions of bauxites, nephelins, kaolins, alunites and flyashes and other aluminum-bearing raw materials are subjected to various actions: air, gas, steam, mechanical vibration, ultrasonic, chemical activation over a period of 30-120 minutes (Examples 1-25, Tables 1) - 24).
• Non-ionic surfactants allow 3-9% alumina to be extracted by various actions of bauxite, nepheline, kaolin, alunite, and fly ash (Examples 1-20, Tables 1-20).
• Sodium citrate and sulfur compounds (sodium sulfamate, sodium lauryl sulfate) make it possible to extract 1-9% alumina using various bauxite, nepheline, kaolin, alunite and fly ash agents (Examples 1-20, Tables 1-20).
• Amphoteric surfactants make it possible to extract 1-7% alumina by means of various actions from bauxite, nepheline, kaolin, alunite and fly ash (Examples 1-20, Tables 1-20).
• Amphoteric surfactants in basic form allow to extract 1-7% alumina and from alunite 38-54% alumina by means of various actions from bauxite, nepheline, kaolin and fly ash (Examples 3) , 8,13,18, Tables 3,8,13,18)
• Anionic surfactants based on unsaturated fatty acids and soaps based on oils containing unsaturated fatty acids make it possible, by means of various bauxite effects, Nepheline, kaolin, alunite and fly ash extract 45-58% alumina (Examples 1-20, Tables 1-20).

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• Geology (AREA)
• Inorganic Chemistry (AREA)
• Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

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• 2012
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