DE10318746A1 - Purification of liquids, especially water containing heavy metal ions, involves bonding the impurities on or in magnesium hydroxide - Google Patents
Purification of liquids, especially water containing heavy metal ions, involves bonding the impurities on or in magnesium hydroxide Download PDFInfo
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- DE10318746A1 DE10318746A1 DE2003118746 DE10318746A DE10318746A1 DE 10318746 A1 DE10318746 A1 DE 10318746A1 DE 2003118746 DE2003118746 DE 2003118746 DE 10318746 A DE10318746 A DE 10318746A DE 10318746 A1 DE10318746 A1 DE 10318746A1
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- magnesium hydroxide
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- metal ions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3007—Moulding, shaping or extruding
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
- C02F1/64—Heavy metal compounds of iron or manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
Description
In vielen Bereichen müssen Verunreinigungen aus Flüssigkeiten entfernt werden. Beispiele hierfür sind die Grundwasseraufbereitung im Rahmen von Altlastensanierungen, die industrielle Abwasserreinigung oder die Aufbereitung von Trinkwasser.In many areas need Contamination from liquids be removed. Examples of this are groundwater treatment in the context of contaminated site remediation, industrial wastewater treatment or the treatment of drinking water.
Hierfür stehen zahlreiche Methoden zur Verfügung. Zur Entfernung von organischen, unpolaren Stoffen wird mit Erfolg Aktivkohle verwendet. Aktivkohle eignet sich jedoch nur sehr begrenzt zur Entfernung von anorganischen Verunreinigungen oder zur Entfernung von polaren Verbindungen.Stand for it numerous methods available. The removal of organic, non-polar substances is successful Activated carbon used. Activated carbon is only of limited use for removal of inorganic contaminants or for removal of polar connections.
An Partikel gebundene Schadstoffe können durch Copräzipitation mit Eisen- oder Aluminiumhydroxid entfernt werden. Dieses Verfahren ist jedoch sehr aufwendig. Viele Schwermetalle bilden schwerlösliche Hydroxide. Sie können durch Einstellen eines neutralen bis schwach alkalischen pH-Wertes gefällt werden. Das Verfahren ist ebenfalls aufwendig und nicht in allen Fällen lässt sich damit der geforderte Grenzwert einhalten. Gründe hierfür können sein, dass die Löslichkeit der Hydroxide zu hoch ist oder, dass die Schwermetalle durch andere Stoffe, wie zum Beispiel Komplexbildnern, in Lösung gehalten werden.On Particle-bound pollutants can pass through coprecipitation can be removed with iron or aluminum hydroxide. This method however, is very complex. Many heavy metals form poorly soluble hydroxides. You can can be precipitated by setting a neutral to weakly alkaline pH. The process is also complex and cannot be carried out in all cases to comply with the required limit. Reasons for this can be that the solubility the hydroxides are too high or that the heavy metals are caused by others Substances such as complexing agents are kept in solution.
Viele als Ionen gelöste Schadstoffe können mit Ionenaustauscherharzen entfernt werden. Diese Harze sind jedoch meistens teuer. Eine eventuell mögliche Regenerierung ist sehr aufwendig. Der Einsatz von Ionenaustauscherharzen zur Aufbereitung von Trinkwasser ist aufgrund der Gefahr der Verunreinigung mit Mikroorganismen im allgemeinen nicht praktikabel.Lots dissolved as ions Pollutants can with Ion exchange resins are removed. However, these resins are mostly expensive. A possible one Regeneration is very expensive. The use of ion exchange resins for the treatment of drinking water is due to the risk of contamination generally not practicable with microorganisms.
Nach
Die
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Verfügung zu stellen, mit dem Verunreinigungen bis auf sehr geringe Restgehalte mit einfachen technischen Mitteln umweltgerecht und zuverlässig aus Flüssigkeiten entfernt werden können.The The invention has for its object to provide a method with the impurities except for very low residual contents environmentally friendly and reliable with simple technical means liquids can be removed.
Es ist ein gebräuchliches Verfahren Magnesiumhydroxid zur Anhebung des pH-Wertes und zur Verringerung der Aggressivität gegenüber Blei bei der Trinkwasser aufbereitung einzusetzen. Es ist ebenfalls bekannt Magnesiumhydroxid zur Anhebung des pH-Wertes bei der Aufbereitung von Industrieabwasser zu verwenden. Daneben ist bekannt, dass Schwermetalle mit Magnesiumhydroxid gefällt werden können. Vorteilhaft ist hierbei der gegenüber Alkali- und Calciumhydroxid langsamere Anstieg des pH-Wertes verbunden mit der langsameren Ausfällung der Schwermetallhydroxide und der Bildung größerer Kristalle.It is a common one Magnesium hydroxide process for raising the pH and reducing aggressiveness towards lead used in drinking water treatment. It is also known Magnesium hydroxide to raise the pH value during processing of industrial wastewater to use. In addition, it is known that heavy metals be precipitated with magnesium hydroxide can. The advantage here is over alkali and calcium hydroxide slower increase in pH associated with slower precipitation of the Heavy metal hydroxides and the formation of larger crystals.
Erfindungsgemäß hat sich gezeigt, dass Magnesiumhydroxid nicht nur zum Anstieg des pH-Wertes führt, sondern Verunreinigungen durch Bindung an oder in Magnesiumhydroxid aus Flüssigkeiten entfernt werden. Magnesiumhydroxid tritt in der Natur als blättchenförmiger hexagonaler Brucit auf. Es kristallisiert in der Cdl2-Struktur. Die (OH)–-Ionen bilden eine hexagonal dichteste Kugelpackung in der jede zweite Oktaederlücken-Schicht mit Mg2+-Ionen besetzt ist. Synthetisch kann es einfach durch Hydratation von Magnesiumoxid erzeugt werden.According to the invention, it has been shown that magnesium hydroxide not only leads to an increase in the pH value, but that impurities are removed from liquids by binding to or in magnesium hydroxide. Magnesium hydroxide occurs in nature as a flaky hexagonal brucite. It crystallizes in the Cdl 2 structure. The (OH) - ions form a hexagonally closest spherical packing in which every second octahedral gap layer is occupied by Mg 2+ ions. Synthetically, it can be created simply by hydrating magnesium oxide.
Magnesiumhydroxid besitzt aufgrund seines blättchenförmigen Habitus eine sehr hohe Oberfläche. Es ist in Wasser sehr wenig löslich und erhöht damit den pH-Wert nicht wesentlich.magnesium hydroxide possesses due to its leaf-like habit a very high surface. It is very slightly soluble in water and increases with it the pH is not essential.
Bei der Fixierung von Verunreinigungen an oder in Magnesiumhydroxid sind unterschiedliche Mechanismen möglich. So können Verunreinigungen zum Beispiel durch Adsorption an die hohe Oberfläche gebunden werden. Denkbar ist auch die Einbindung von Verunreinigungen in die Kristallsturktur des Brucit. Jenes gilt besonders für Ionen die die gleiche Ladung und einen ähnlichen Ionenradius aufweisen wie Mg2+. Beispiele hiefür sind die Ionen der Nebengruppenmetalle Mn2+, Fe2+, Co2+, Ni2+, Cu2+, Zn2+. Die Fixierung dreiwertiger Ionen wie Cr3+ oder Al3+, Fe3+, ist zum Beispiel durch Reaktion zu Metall-Metall-Hydroxisalzen vom AFM-Typ möglich.Different mechanisms are possible for fixing impurities on or in magnesium hydroxide. For example, impurities can be bound to the high surface by adsorption. It is also conceivable to incorporate impurities in the crystal structure of the brucite. This is especially true for ions that have the same charge and a similar ion radius as Mg 2+ . Examples of these are the ions of the subgroup metals Mn 2+ , Fe 2+ , Co 2+ , Ni 2+ , Cu 2+ , Zn 2+ . Trivalent ions such as Cr 3+ or Al 3+ , Fe 3+ can be fixed, for example, by reaction to metal-metal hydroxyl salts of the AFM type.
Vorteilhaft ist die Verwendung von granuliertem Magnesiumhydroxid in Filtern. Die bevorzugten Korngrößen sind 1 bis 8 mm. Das Granulat kann als Filterschüttung in einen handelsüblichen Kiesfilter, einen Aktivkohlefilter oder eine Ionenaustauschersäule eingebracht werden.Advantageous is the use of granulated magnesium hydroxide in filters. The preferred grain sizes are 1 to 8 mm. The granulate can be used as a filter bed in a commercially available Gravel filter, an activated carbon filter or an ion exchange column introduced become.
Möglich ist die Herstellung eines hierfür geeigneten Granulates durch Extrusion eines Gemisches aus Magnesiumhydroxid, Magnesiumoxid und Wasser. Durch anschließendes Trocknen bei 80 bis 100°C wird durch Verdampfen des Wassers eine hohe Porosität und damit eine hohe Oberfläche erzeugt. Zudem wird das Granulat bei diesen Temperaturen hygienisiert.Is possible making one for this suitable granules by extrusion of a mixture of magnesium hydroxide, Magnesium oxide and water. Subsequent drying at 80 to 100 ° C is followed by Evaporation of the water creates a high porosity and thus a high surface. In addition, the granules are hygienized at these temperatures.
Zum Extrudieren ist es vorteilhaft dem Gemisch aus Magnesiumhydroxid, Magnesiumoxid und Wasser gemahlene Zeolithe zuzugeben. Der Anteil liegt dabei bei 5 bis 50 Masse-%, bevorzugt bei 10 bis 20 Masse-% bezogen auf die Summe aus Magnesiumhydroxid und Magnesiumoxid. Damit erhält das Granulat eine höhere Anfangsfestigkeit.To the It is advantageous to extrude the mixture of magnesium hydroxide, Add magnesium oxide and water ground zeolites. The share is 5 to 50% by mass, preferably 10 to 20% by mass on the sum of magnesium hydroxide and magnesium oxide. This gives the granules a higher one Initial strength.
Zur Erhöhung der wirksamen Oberfläche und der Reaktivität des Granulats ist es vorteilhaft dem Gemisch Eisen(III)-haltige Verbindungen zuzugeben. Röntgenbeugungsuntersuchungen zeigten, dass dadurch die Kristallinität des Magnesiumhydroxids deutlich verschlechtert wurde. Der Anteil des dabei zugeführten Eisens liegt bevorzugt bei 1 bis 4 Masse-% bezogen auf die Summe aus Magnesiumhydroxid und Magnesiumoxid.to increase the effective surface and of reactivity of the granulate, it is advantageous to the mixture containing iron (III) Add connections. X-ray diffraction studies showed that this made the crystallinity of the magnesium hydroxide clear has deteriorated. The proportion of iron fed in is preferred at 1 to 4 mass% based on the sum of magnesium hydroxide and magnesium oxide.
Beispiele 1:Examples 1:
Zu 250 ml einer wässerigen Lösung die 1000 mg/l Nickel enthält, werden 3 g Magnesiumhydroxid gegeben. Nach 10 h Reaktionszeit stellt sich in der Lösung eine Nickelkonzentration von 0,5 mg/l ein. Der pH-Wert beträgt 8,7. Bei diesem pH-Wert ist zu erwarten, dass ohne die Bindung des Nickels an das Magnesiumhydroxid und nur aufgrund der Ausfällung als Nickelhydroxid 23 mg/l Nickel in Lösung sind.To 250 ml of an aqueous solution which contains 1000 mg / l nickel, 3 g of magnesium hydroxide are added. After 10 h reaction time yourself in the solution a nickel concentration of 0.5 mg / l. The pH is 8.7. At this pH it is expected that without the binding of the nickel to the magnesium hydroxide and only because of the precipitation as Nickel hydroxide 23 mg / l nickel are in solution.
Beispiel 2:Example 2:
Zu 250 ml einer wässerigen Lösung die 1000 mg/l Kupfer enthält werden 3 g Magnesiumhydroxid gegeben. Nach 10 h Reaktionszeit beträgt die Kupferkonzentration in der Lösung < 0,01 mg/l.To 250 ml of an aqueous solution which contains 1000 mg / l copper 3 g of magnesium hydroxide are added. After a reaction time of 10 h, the copper concentration is in the solution <0.01 mg / l.
Beispiel 3:Example 3:
Zu 250 ml einer wässerigen Lösung die 1000 mg/l Zink enthält werden 3 g Magnesiumhydroxid gegeben. Nach 10 h Reaktionszeit stellt sich eine Konzentration von < 0,01 mg/l Zink ein.To 250 ml of an aqueous solution which contains 1000 mg / l zinc 3 g of magnesium hydroxide are added. After 10 h reaction time a concentration of <0.01 mg / l zinc.
Beispiel 4:Example 4:
1000 g Magnesiumhydroxid, 1000 g Magnesiumoxid und 1000 ml Wasser werden in einem Mischer vorgemischt, anschließend in einem Extruder zu einem Granulat mit 2 mm Korngröße geformt und schließlich 3 h bei 80°C getrocknet. 750 g des getrockneten Granulates werden in eine Filtersäule mit einem Durchmesser von 50 mm gefüllt. Über diese Filterschüttung wird mit einem Durchsatz von 1 l/h Wasser mit einer Nickelkonzentration von 100 mg/l gegeben. Am Ablauf der Filtersäule stellt sich eine Nickelkonzentration von < 0,005 mg/l ein.1000 g of magnesium hydroxide, 1000 g of magnesium oxide and 1000 ml of water premixed in a mixer, then in an extruder into one Granules with 2 mm grain size shaped and finally 3 h at 80 ° C dried. 750 g of the dried granules are placed in a filter column filled with a diameter of 50 mm. About these filter bed is with a throughput of 1 l / h of water with a nickel concentration of 100 mg / l. There is a nickel concentration at the outlet of the filter column of <0.005 mg / l on.
Beispiel 5:Example 5:
Über eine Filtersäule mit 750 g Magnesiumhydroxidgranulat, wie in Beispiel 4 erläutert, wird Wasser gegeben, das 5 mg/l Zink enthält, welches in einem Amminokomplex gebunden ist. Am Ablauf der Säule stellt sich eine Zinkkonzentration von 0,1 mg/l ein.Over a filter column with 750 g of magnesium hydroxide granules, as explained in Example 4, water given that contains 5 mg / l zinc, which is bound in an amino complex. At the end of the column there is a zinc concentration of 0.1 mg / l.
Claims (9)
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140326673A1 (en) * | 2008-04-29 | 2014-11-06 | Baker Hughes Incorporated | Wastewater purification with nanoparticle-treated bed |
WO2021232391A1 (en) * | 2020-05-22 | 2021-11-25 | 兰州兰石中科纳米科技有限公司 | Product recovery method and device used in preparation and use processes of wastewater treatment agent |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3534472A1 (en) * | 1985-09-27 | 1987-04-02 | Henkel Kgaa | METHOD AND MEANS FOR WATER TREATMENT |
DE3927678C2 (en) * | 1987-11-09 | 1998-07-02 | Aluminum Co Of America | Process for reducing the amount of anionic metal-ligand complexes in a solution |
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2003
- 2003-04-25 DE DE2003118746 patent/DE10318746A1/en not_active Ceased
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3534472A1 (en) * | 1985-09-27 | 1987-04-02 | Henkel Kgaa | METHOD AND MEANS FOR WATER TREATMENT |
DE3927678C2 (en) * | 1987-11-09 | 1998-07-02 | Aluminum Co Of America | Process for reducing the amount of anionic metal-ligand complexes in a solution |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140326673A1 (en) * | 2008-04-29 | 2014-11-06 | Baker Hughes Incorporated | Wastewater purification with nanoparticle-treated bed |
US9540251B2 (en) * | 2008-04-29 | 2017-01-10 | Baker Hughes Incorporated | Wastewater purification with nanoparticle-treated bed |
US10449513B2 (en) | 2008-04-29 | 2019-10-22 | Baker Hughes, A Ge Company, Llc | Wastewater purification with nanoparticle-treated bed |
WO2021232391A1 (en) * | 2020-05-22 | 2021-11-25 | 兰州兰石中科纳米科技有限公司 | Product recovery method and device used in preparation and use processes of wastewater treatment agent |
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