DE4124171A1 - Complex alkaline earth salt prepn. of poly:aluminium:chloride(s) - comprises reacting suspension of basic alkaline earth metal salts with soln. of poly:aluminium chloride of specified average empirical formula - Google Patents

Complex alkaline earth salt prepn. of poly:aluminium:chloride(s) - comprises reacting suspension of basic alkaline earth metal salts with soln. of poly:aluminium chloride of specified average empirical formula

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Publication number
DE4124171A1
DE4124171A1 DE4124171A DE4124171A DE4124171A1 DE 4124171 A1 DE4124171 A1 DE 4124171A1 DE 4124171 A DE4124171 A DE 4124171A DE 4124171 A DE4124171 A DE 4124171A DE 4124171 A1 DE4124171 A1 DE 4124171A1
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Prior art keywords
alkaline earth
poly
chloride
aluminium
earth metal
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DE4124171A
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German (de)
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Bettina Affonso
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • 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
    • C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Geology (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Prodn. comprises reacting a suspension of a basic alkaline earth salt with a soln. of polyaluminium chloride of the average empirical compsn. Al2(OH)2Cl2-3H2O. The basic salt is pref. an alkaline earth metal oxide, hydroxide, or carbonate and is esp. pref. calcium hydroxide. The average empirical compsn. of the polyaluminium chloride is pref. Al2(OH)4.95Cl1.05 to Al2(OH)5.05Cl0.95 with a water content of 2-3 mols and a basicity of 50-80, pref. 60%. USE -Used as a flocculating agent for swimming pool water and waste water. The powder is almost insol. in water and binds to heavy metal ions and turbidity-causing particles at neutral pH values.

Description

Polyaluminiumchloride sind basische Aluminiumchloridsalze der mittleren Brutto- Zusammensetzung Al₂(OH)₅Cl 2-3 H₂O. Die Zusammensetzung kann variieren von Al₂(OH)4,95Cl1,05 bis zu Al₂(OH)5,05Cl0,95 mit einem Gehalt von 2 bis 3 Mol H₂O. Polyaluminiumchloride (PAC's) finden zunehmende Anwendung als Flockungsmittel für Schwimmbadwasser und Abwasser (Handelsnamen "Locron" und "Provimal" der Firma Hoechst AG).Polyaluminium chlorides are basic aluminum chloride salts with an average gross composition of Al₂ (OH) ₅Cl 2-3 H₂O. The composition can vary from Al₂ (OH) 4.95 Cl 1.05 to Al₂ (OH) 5.05 Cl 0.95 with a content of 2 to 3 mol H₂O. Polyaluminium chlorides (PAC's) are increasingly used as flocculants for swimming pool water and waste water (trade names "Locron" and "Provimal" from Hoechst AG).

Über die chemische Struktur ist wenig Verläßliches bekannt. Waters and Henty (Journal of the Chemical Society Dalton Transactions 3 [1977], S. 243-245) nehmen aufgrund ramanspektroskopischer Untersuchungen im Aluminiumhydroxychlorid eine Struktur eines vielkernigen AluminiumkomplexesLittle is known about the chemical structure. Waters and Henty (Journal of the Chemical Society Dalton Transactions 3 [1977], pp. 243-245) based on Raman spectroscopic investigations in aluminum hydroxychloride a structure of a multi-core aluminum complex

[Al₁₃O₄(OH)₂₄(OH₂)₁₂]7+ [Al₁₃O₄ (OH) ₂₄ (OH₂) ₁₂] 7+

an. Zlatev, Trendafelov und Nikolov (Bulgarische Akademie der Wissenschaften, Communications of the Department of Chemistry, Volume VIII, Nr. 3, 1975, Page 433-442) kommen zu der Ansicht, daß ein tetramerer Komplex vorliegt:at. Zlatev, Trendafelov and Nikolov (Bulgarian Academy of Sciences, Communications of the Department of Chemistry, Volume VIII, No. 3, 1975, Page 433-442) conclude that there is a tetrameric complex:

[Al₈(OH)₂₀(H₂O)₁₀]4+.[Al₈ (OH) ₂₀ (H₂O) ₁₀] 4+ .

Die Basizität (m/3n×100) soll 50 bis 60% betragen. Nach Datenblättern einiger Hersteller ist PAC im sauren wäßrigen Millieu beständig, jedoch fällt bei einem pH über 5 Aluminiumchlorid aus. Es ist bekannt, daß Aluminium Natriumaluminat bildet durch die Einwirkung von Natronlauge auf Aluminiumhydroxid. Natriumaluminat läßt sich leicht in Calciumaluminat umwandeln. Aus Patentschrift EP 02 18 487 ist ein basisches Aluminiumchlorosulfat bekannt, welches als Flockungsmittel verwendet wird. Die Eigenschaft von reinem Calciumaluminat, das Sulfation zu binden, ist nach Patentschrift EP 02 50 626 abhängig von einer Dosierung von Kalkmilch bis zu einem konstant gehaltenen pH-Wert von 11,2 bis 11,8. Es ist daher leicht zu erkennen, daß reines Calciumaluminat zusätzliche Chemikalien benötigt, damit eine Reaktivität zu Sulfationen stattfindet. Ein ideales Wasseraufbereitungsmittel wäre ein solches, welches die Sulfationen bei neutralem pH bindet und gleichzeitig flockungs- und adsorptive Eigenschaften zeigt.The basicity (m / 3n × 100) should be 50 to 60%. According to data sheets of some The manufacturer is resistant to PAC in the acidic aqueous environment, but falls at a pH over 5 aluminum chloride. Aluminum is known to form sodium aluminate by the action of caustic soda on aluminum hydroxide. Sodium aluminate can be easily converted into calcium aluminate. From patent EP 02 18 487 is a basic aluminum chlorosulfate known, which is used as a flocculant becomes. The property of pure calcium aluminate to bind the sulfate ion is after Patent EP 02 50 626 depending on a dosage of milk of lime up to one pH kept constant from 11.2 to 11.8. It is therefore easy to see that Pure calcium aluminate requires additional chemicals to be reactive Sulfate ion takes place. An ideal water purifier would be one that which binds the sulfate ions at neutral pH and at the same time flocculates and shows adsorptive properties.

In vorliegender Erfindung wird eine bisher unbekannte Herstellungsmethode von Alkalierdesalzen der Polyaluminiumchloride beschrieben. Vorzugsweise wurde das Calciumsalz nach sorgfältigem Trocknen und Mahlen als Feinpulver erhalten. Das Pulver ist fast unlöslich in Wasser und bindet bei neutralem pH sehr schnell Sulfationen sowie Trübungen und Schwermetalle. Das Problem eines fast idealen Austauschmaterials zur Wasseraufbereitung ist der vorliegenden Erfindung zu­ grunde gelegt. Folgendes Herstellungsbeispiel für einen Laboransatz wird näher beschrieben:In the present invention, a previously unknown production method of Alkalierdesalzen the polyaluminiumchloride described. Preferably that was Calcium salt obtained after fine drying and grinding as fine powder. The Powder is almost insoluble in water and binds very quickly at neutral pH Sulphate ions as well as turbidity and heavy metals. The problem of an almost ideal Exchange material for water treatment is the present invention based. The following manufacturing example for a laboratory approach is closer described:

Beispiel 1Example 1 Suspension ASuspension A

54,5 g Calciumhydroxyd (Merck) wurden in 4000 ml Wasser suspendiert.54.5 g calcium hydroxide (Merck) were suspended in 4000 ml water.

Lösung BSolution B

259,8 g Polyaluminiumhydroxychlorid in feine Schuppen (LOCRON S, Hoechst AG) wurden in 2500 ml Wasser gelöst.259.8 g polyaluminium hydroxychloride in fine flakes (LOCRON S, Hoechst AG) were dissolved in 2500 ml of water.

Suspension A wurde langsam und mit kräftigem Rühren zur Lösung B hinzugefügt. Nach einigen Minuten hat sich eine dicke, geleeartige Verbindung gebildet. Der pH-Wert der Mischung ist 7,3. Durch Filtration und Pressen der Filterkuchen werden alle löslichen Bestandteile ausgewaschen. Das geleeartige Produkt wird bei 40°C und 10 mm Vakuum getrocknet. Das Trockenprodukt läßt sich leicht zu Pulver zermahlen mit einem Partikeldurchmesser von 20 Mikron. Es ist fast unlöslich in Wasser, und die Partikel quellen geleeartig auf. Suspension A was slowly added to solution B with vigorous stirring. After a few minutes, a thick, jelly-like connection has formed. The pH of the mixture is 7.3. By filtering and pressing the filter cake washed out all soluble components. The jelly-like product is at 40 ° C and 10 mm vacuum dried. The dry product can be easily powdered grind with a particle diameter of 20 microns. It is almost insoluble in Water, and the particles swell like a jelly.  

Eigenschaftenproperties

1 g des beschriebenen Produktes besitzt die Kapazität, 20 mg Sulfationen sowie 5 mg Kupferionen zu binden. Gleichzeitig werden auch Trübungen koaguliert. Durch Variieren des Masseanteils von Calciumhydroxyd und Polyaluminiumchlorid erhält man Salze mit unterschiedlichen Adsorptions- und Bindungskapazitäten.1 g of the product described has the capacity, 20 mg of sulfate ions and 5 to bind mg copper ions. At the same time, cloudiness is also coagulated. By varying the mass fraction of calcium hydroxide and polyaluminium chloride salts with different adsorption and binding capacities are obtained.

Claims (4)

1. Herstellung von Komplex-Erdalkalisalzen von Polyaluminiumchloriden, dadurch gekennzeichnet, daß eine Suspension eines basischen Salzes der Erdalkalimetalle mit einer Lösung von Polyaluminiumchloride der mittleren Brutto-Zusammensetzung Al₂(OH)₅Cl 2-3 H₂O in wäßrigem Milieu reagiert.1. Production of complex alkaline earth metal salts of polyaluminium chlorides, characterized in that a suspension of a basic salt of the alkaline earth metals reacts with a solution of polyaluminium chlorides of average gross composition Al₂ (OH) ₅Cl 2-3 H₂O in an aqueous medium. 2. Herstellung von Komplex-Erdalkalisalzen von Polyaluminiumchloriden nach Anspruch 1, dadurch gekennzeichnet, daß das basische Salz der Erdalkalimetalle ein Oxid, Hydroxid oder Carbonat, vorzugsweise Calciumhydroxyd, ist.2. Production of complex alkaline earth metal salts of polyaluminium chlorides after Claim 1, characterized in that the basic salt of Alkaline earth metals an oxide, hydroxide or carbonate, preferably Calcium hydroxide. 3. Herstellung von Komplex-Erdalkalisalzen von Polyaluminiumchloriden nach Anspruch 1 und 2, dadurch gekennzeichnet, daß das Polyaluminiumchlorid der mittleren Brutto-Zusammensetzung variiert von Al₂(OH)4,95Cl1,05 bis zu Al₂(OH)5,05Cl0,95 mit einem Gehalt von 2 bis 3 Mol Wasser und einer Basizität von 50 bis 80%, vorzugsweise 60%.3. Preparation of complex alkaline earth metal salts of polyaluminium chlorides according to claim 1 and 2, characterized in that the polyaluminium chloride of the average gross composition varies from Al₂ (OH) 4.95 Cl 1.05 to Al₂ (OH) 5.05 Cl 0 , 95 with a content of 2 to 3 moles of water and a basicity of 50 to 80%, preferably 60%. 4. Herstellung von Komplex-Erdalkalisalzen von Polyaluminiumchloriden nach Ansprüchen 1, 2, 3, 4, dadurch gekennzeichnet, daß der Masseanteil von Erdalkalihydroxid/Polyaluminiumchlorid = 1/3 bis 6, vorzugsweise 1/4,8 beträgt.4. Preparation of complex alkaline earth metal salts of polyaluminium chlorides Claims 1, 2, 3, 4, characterized in that the mass fraction of Alkaline earth metal hydroxide / polyaluminium chloride = 1/3 to 6, preferably 1 / 4.8 is.
DE4124171A 1991-07-20 1991-07-20 Complex alkaline earth salt prepn. of poly:aluminium:chloride(s) - comprises reacting suspension of basic alkaline earth metal salts with soln. of poly:aluminium chloride of specified average empirical formula Withdrawn DE4124171A1 (en)

Priority Applications (1)

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DE4124171A DE4124171A1 (en) 1991-07-20 1991-07-20 Complex alkaline earth salt prepn. of poly:aluminium:chloride(s) - comprises reacting suspension of basic alkaline earth metal salts with soln. of poly:aluminium chloride of specified average empirical formula

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DE4124171A DE4124171A1 (en) 1991-07-20 1991-07-20 Complex alkaline earth salt prepn. of poly:aluminium:chloride(s) - comprises reacting suspension of basic alkaline earth metal salts with soln. of poly:aluminium chloride of specified average empirical formula

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DE4124171A1 true DE4124171A1 (en) 1993-01-21

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0744378A1 (en) * 1995-05-24 1996-11-27 Rhone-Poulenc Chimie New polychloride or polychlorosulfate of aluminium, process for its preparation and its use for the treatment of water
WO2008070218A1 (en) * 2006-12-05 2008-06-12 General Chemical Llc Polyaluminum calcium hydroxychlorides and methods of making the same
DE102009049200A1 (en) * 2009-10-13 2011-04-28 Tetra Gmbh Means for clarifying water supply

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0744378A1 (en) * 1995-05-24 1996-11-27 Rhone-Poulenc Chimie New polychloride or polychlorosulfate of aluminium, process for its preparation and its use for the treatment of water
FR2734559A1 (en) * 1995-05-24 1996-11-29 Rhone Poulenc Chimie NOVEL ALUMINUM POLYCHLORIDES OR POLYCHLOROSULFATES, PROCESS FOR PREPARING THEM AND APPLICATION THEREOF TO THE TREATMENT OF AQUEOUS MEDIA
WO2008070218A1 (en) * 2006-12-05 2008-06-12 General Chemical Llc Polyaluminum calcium hydroxychlorides and methods of making the same
DE102009049200A1 (en) * 2009-10-13 2011-04-28 Tetra Gmbh Means for clarifying water supply

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