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DE4103165A1 - Purifying contaminated effluent waters - by liq. liq. extraction followed by treatment in adsorption reactor - Google Patents

Purifying contaminated effluent waters - by liq. liq. extraction followed by treatment in adsorption reactor

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Publication number
DE4103165A1
DE4103165A1 DE4103165A DE4103165A DE4103165A1 DE 4103165 A1 DE4103165 A1 DE 4103165A1 DE 4103165 A DE4103165 A DE 4103165A DE 4103165 A DE4103165 A DE 4103165A DE 4103165 A1 DE4103165 A1 DE 4103165A1
Authority
DE
Germany
Prior art keywords
adsorption
liq
filling
flooded
polyurethane foam
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
DE4103165A
Other languages
German (de)
Inventor
Des Erfinders Auf Nennung Verzicht
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
IFG INGENIEUR und FORSCHUNGSGE
Original Assignee
IFG INGENIEUR und FORSCHUNGSGE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by IFG INGENIEUR und FORSCHUNGSGE filed Critical IFG INGENIEUR und FORSCHUNGSGE
Priority to DE4103165A priority Critical patent/DE4103165A1/en
Publication of DE4103165A1 publication Critical patent/DE4103165A1/en
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
    • 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
    • C02F1/26—Treatment of water, waste water, or sewage by extraction
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/301—Detergents, surfactants
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

Process for purifying effluent waters contaminated with very small concns. of heavy metals and halogenated hydrocarbons by liq.-liq. extn., whereby after the extn. stage the remaining heavy metal residues are removed in an adsorption reactor. Pref. the adsorbent is used in such an amt. and has a surface such that it need not be replaced or regenerated throughout the whole life of the unit. Suitable adsorption agents are e.g. active carbon coated onto a reticulated polyurethane foam or an adsorption resin in the form of granules, chips or an open pored solid bed. USE/ADVANTAGE - The process allows treatment of condensate waste waters obtd. in the distn. of recirculating solvents from the chemical cleaning of leather and textiles after extn. with modified paraffin oils, and effluent waters obtd. in the regeneration of air extn. filters from metal degreasing. The process is cost effective and requires little supervision. No special waste is produced during operation of the unit and the filling is disposed of only at the end of the useful life of the uni

Description

Die bei der Chemisch-Reinigung von Leder und Textilien anfallenden, mit Lösemittelresten verunreinigten Kondensatabwässer (unter anderem aus der Destillation des im Kreislauf geführten Lösemittels) können nach der Extraktionsbehandlung mit modifiziertem Paraffinöl bei der die haloge­ nierten Kohlenwasserstoffe entfernt wurden, noch Schwermetalle ent­ halten. Auch bei der Regenerierung der Abluftfilter in der Metallent­ fettung fallen Abwässer an, die neben den Kohlenwasserstoffen (Lösemittel) auch noch Schwermetalle enthalten können. Es stand bisher kein wirksames Verfahren zur Abtrennung dieser Verschmutzungen zur Verfügung.The resulting from the chemical cleaning of leather and textiles, with Residual solvent contaminated condensate waste water (among other things from the distillation of the circulated solvent) can after Extraction treatment with modified paraffin oil in which the halogen hydrogenated hydrocarbons have been removed, heavy metals still ent hold. Also when regenerating the exhaust air filter in the metal ent greasing, waste water is produced which, in addition to the hydrocarbons (solvents) can also contain heavy metals. So far there has been no effective one Processes for removing these contaminants are available.

Die Aufgabe, ein kostengünstiges und wenig wartungsintensives Verfahren für die sichere Eliminierung dieser Schwermetalle zur Verfügung zu stellen wird gemäß der vorliegenden Erfindung dadurch gelöst, daß die nach der Extraktionsstufe verbleibende Verschmutzung an Schwermetallen in einem Adsorptions-Reaktor entfernt wird, wobei das Adsorptionsmittel, z. B. Aktiv­ kohle, insbesondere Adsorberharze, in einer solchen Menge und mit einer solchen aktiven Oberfläche zur Verfügung gestellt wird, daß es während der ganzen Lebensdauer der Anlage nicht ersetzt oder regeneriert zu werden braucht. Hierbei werden also beide bekannten Eliminationsverfahren in der Form miteinander kombiniert, daß das eine, wirkungsvollere für die Haupt­ fracht an Kohlenwasserstoffen und das andere für die dort nicht abgetrennten Schwermetalle eingesetzt wird. Während des ganzen Betriebs der Anlage fällt somit kein Sondermüll an. Das Adsorptionsmittel, z. B. Adsorberharz, wird erst am Ende der Lebensdauer der Reinigungsanlage entsorgt.The task of an inexpensive and low-maintenance process for to provide the safe elimination of these heavy metals is solved according to the present invention in that the after Extraction level residual contamination of heavy metals in one Adsorption reactor is removed, the adsorbent, for. B. Active coal, in particular adsorber resins, in such an amount and with a such active surface is made available that it during the to be replaced or regenerated throughout the life of the system needs. This means that both known elimination processes in the Form combined that one, more effective for the main cargo of hydrocarbons and the other for those not separated there Heavy metals is used. During the whole operation of the plant falls therefore no hazardous waste. The adsorbent, e.g. B. adsorber resin, is only disposed of at the end of the life of the cleaning system.

Vorzugsweise wird bei Verwendung von Adsorberharz als Adsorptionsmittel dieses als Granulat, Schnitzel oder offenporiges Festbett zur Verfügung ge­ stellt. Dies ergibt eine definierte große aktive Oberfläche und eine hervor­ ragende Eliminationsrate durch Mikroturbulenzen.Is preferred when using adsorber resin as an adsorbent this is available as granules, schnitzel or open-pore fixed bed poses. This results in a defined large active surface and one excellent elimination rate due to microturbulence.

Es ist bekannt, in der Extraktionsstufe einen offenporigen Polyurethanschaum zu verwenden, der mit dem Extraktionsmittel belegt oder geflutet ist. Im Betrieb einer solchen Extraktionsstufe kommt es vor, daß die in Zeiten hoher Frachten von dem Extraktionsmittel aufgenommenen halogenierten Kohlenwasser­ stoffe in Zeiten geringerer Frachten wieder rückgelöst werden. Auch diese rückgelösten halogenierten Kohlenwasserstoffe werden erfindungsgemäß in der Adsorptionsstufe weitestgehend adsorbiert und die Gesamtfracht wird hier­ durch erheblich verringert. Für diese Elimination der rückgelösten haloge­ nierten Kohlenwasserstoffe ist es von Vorteil, wenn die Extraktionsstufe von der Adsorptionsstufe durch einen wassergefluteten, einbaufreien Abschnitt 11 getrennt ist. Dieser Abschnitt verhindert auch, daß Extraktionsmittel in die Adsorptionsstufe geschwemmt wird. Beispielhafte Einrichtungen zur Ausführung des erfindungsgemäßen Verfahrens sind in den beigefügten Zeichnungen darge­ stellt und werden nachfolgend näher beschrieben.It is known to use an open-pore polyurethane foam in the extraction stage, which is coated or flooded with the extractant. In the operation of such an extraction stage it happens that the halogenated hydrocarbons absorbed by the extractant in times of high loads are redissolved in times of lower loads. According to the invention, these redissolved halogenated hydrocarbons are also adsorbed as far as possible in the adsorption stage and the total load is considerably reduced here. For this elimination of the redissolved halogenated hydrocarbons, it is advantageous if the extraction stage is separated from the adsorption stage by a water-flooded, installation-free section 11 . This section also prevents extractant from being swept into the adsorption stage. Exemplary devices for performing the method according to the invention are shown in the accompanying drawings and are described in more detail below.

Fig. 1. zeigt einen Reaktor 1, der beinahe über die ganze Höhe mit Polyurethan- Schaum 2 gefüllt ist. Der oberste Abschnitt ist bis über die Oberseite mit Extraktionsmittel 5 geflutet. Ein unterer Abschnitt 3 vor der einbaufreien Auslaufzone 4 ist mit Aktivkohle beschichtet. Der Reaktor wird von dem Ab­ wasser von oben nach unten durchströmt. Bei der Variante nach Fig. 2 liegt auf der von einem Gitterrost 6 getragenen Adsorptionsmittelschicht 7 z. B: Adsorberharzgranulat, eine Kiesschicht 8, 9, deren oberster Abschnitt 9 wiederum mit Extraktionsmittel 10 geflutet ist. Die extraktionsmittelfreie Zone 8 sorgt dafür, daß die aus der Extraktionsmittelschicht eventuell mitgerissenen Partikel nicht bis in die Adsorptionsmittelschicht gelangen, sondern in Zeiten verminderten Zulaufs wieder in die Extraktionsmittelschicht 10 auf­ steigen können. Fig. 1. shows a reactor 1, which is filled almost over the entire height with polyurethane foam. 2 The top section is flooded with extractant 5 up to the top. A lower section 3 in front of the installation-free outlet zone 4 is coated with activated carbon. The reactor is flowed through from the top down water. In the variant according to FIG. 2 lies on the adsorbent layer 7 supported by a grating 6 z. B: adsorber resin granulate, a gravel layer 8 , 9 , the top section 9 of which is in turn flooded with extractant 10 . The extractant-free zone 8 ensures that the particles which may be entrained from the extractant layer do not reach the adsorbent layer, but can rise back into the extractant layer 10 in times of reduced inflow.

Dieses Prinzip ist auch bei der Ausführungsform nach Fig. 3 zu finden. Hier ist die Schichtdicke des Extraktionsmittels 10 größer als die des Poly­ urethan-Schaums 2. Bei langen Zeiten ohne Zufluß kann es vorkommen, daß aus dem Polyurethan-Schaum Rücklösung in das Wasser auftritt. Diese Rücklösungen werden vermieden, da der Polyurethan-Schaum von Extraktionsmittel geflutet ist.This principle can also be found in the embodiment according to FIG. 3. Here the layer thickness of the extractant 10 is greater than that of the polyurethane foam 2 . During long periods without an inflow, it can happen that redissolution into the water occurs from the polyurethane foam. These redissolutions are avoided because the polyurethane foam is flooded with extractant.

Anstelle eines Reaktors, der beide Stufen enthält, kann einem normalen Ex­ traktionsreaktor auch eine Adsorptionsstufe nachgeschaltet sein (Fig. 4). Diese enthält einen Einsatz 16 aus z. B. Aktivkohle beschichtetem Poly­ urethan-Schaum oder einer Granulat-, Füllkörper- oder Pulverfüllung eines Adsorptionsmittels, z. Adsorberharze, Aktivkohle. Dort werden die Schwer­ metalle abgetrennt.Instead of a reactor containing both stages, a normal Ex traction reactor can also be followed by an adsorption stage ( Fig. 4). This contains an insert 16 from z. B. activated carbon coated poly urethane foam or a granulate, packing or powder filling of an adsorbent, for. Adsorber resins, activated carbon. The heavy metals are separated there.

Claims (13)

1. Verfahren zur Reinigung von mit Schwermetallen und halogenierten Kohlen­ wasserstoffen in geringster Konzentration verunreinigten Abwässern durch Flüssig-Flüssig-Extraktion an einem Extraktionsmittel, dadurch gekenn­ zeichnet, daß die nach der Extraktionsmittelstufe verbleibende Restver­ schmutzung an Schwermetallen in einem Adsorptions-Reaktor entfernt wird.1. Process for the purification of heavy metals and halogenated hydrocarbons in the lowest concentration contaminated wastewater by liquid-liquid extraction on an extracting agent, characterized in that the residual dirt remaining after the extraction agent stage of heavy metals is removed in an adsorption reactor. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Adsorptions­ mittel in einer solchen Menge und Oberfläche zur Verfügung gestellt wird, daß es während der ganzen Lebensdauer der Anlage nicht ersetzt oder rege­ neriert zu werden braucht.2. The method according to claim 1, characterized in that the adsorption medium is provided in such a quantity and surface, that it will not replace or brisk throughout the life of the system needs to be nerded. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß das Adsorptions­ mittel als Aktivkohlebeschichtung auf einem retikulierten Polyurethan-Schaum dargeboten wird.3. The method according to claim 2, characterized in that the adsorption medium as an activated carbon coating on a reticulated polyurethane foam is presented. 4. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß das Adsorptions­ mittel als Adsorberharz in Form von Granulat oder Schnitzel oder offenporiges Festbett zur Verfügung gestellt wird.4. The method according to claim 2, characterized in that the adsorption medium as an adsorber resin in the form of granules or chips or open-pore Fixed bed is provided. 5. Verfahren nach Anspruch 1, 2, 3 oder 4, dadurch gekennzeichnet, daß Ex­ traktionsstufe und Adsorptionsstufe in einem Reaktor unmittelbar hinterein­ ander angeordnet und durch eine wassergeflutete Zone voneinander getrennt sind.5. The method according to claim 1, 2, 3 or 4, characterized in that Ex traction stage and adsorption stage in a reactor immediately behind arranged and separated from each other by a water-flooded zone are. 6. Verfahren nach Anspruch 1, 2, 3 oder 4, dadurch gekennzeichnet, daß zu­ mindest der erste Abschnitt der Adsorptionsstufenelimination zeitgleich mit der Extraktion stattfindet.6. The method according to claim 1, 2, 3 or 4, characterized in that to at least the first section of the adsorption stage elimination at the same time with the extraction takes place. 7. Einrichtung zur Durchführung des Verfahrens nach Anspruch 1 bis 6, mit mindestens einem das Extraktionsmittel enthaltenden, vertikal durchströmten Gefäß, dadurch gekennzeichnet, daß im zuletzt durchströmten Abschnitt (3) des Gefäßes (1) oder in einem nachgeschalteten Gefäß eine Adsorptionsmittel­ füllung (3, 7, 16) vorgesehen ist.7. Device for carrying out the method according to claim 1 to 6, with at least one vertically flow-through vessel containing the extractant, characterized in that in the last flow-through section ( 3 ) of the vessel ( 1 ) or in a downstream vessel, an adsorbent filling ( 3 , 7 , 16 ) is provided. 8. Einrichtung nach Anspruch 7, dadurch gekennzeichnet, daß über der Ad­ sorptionsmittelfüllung (7) eine vom Extraktionsmittel (10) mindestens im oberen Abschnitt (9) geflutete Kiesfüllung (8) angeordnet ist.8. Device according to claim 7, characterized in that above the ad sorbent filling ( 7 ) from the extractant ( 10 ) at least in the upper section ( 9 ) flooded gravel filling ( 8 ) is arranged. 9. Einrichtung nach Anspruch 7, dadurch gekennzeichnet, daß über der Ad­ sorptionsmittelfüllung (3) eine von Extraktionsmittel (10) mindestens im oberen Abschnitt (5) geflutete Füllung (2) aus retikuliertem Polyurethan- Schaum angeordnet ist.9. Device according to claim 7, characterized in that above the ad sorbent filling ( 3 ) one of extracting agent ( 10 ) at least in the upper section ( 5 ) flooded filling ( 2 ) of reticulated polyurethane foam is arranged. 10. Einrichtung nach Anspruch 7, dadurch gekennzeichnet, daß die Adsorp­ tionsmittelfüllung als granulat-, füllkörper- oder pulvergefüllte, austausch­ bare Packung oder offenporiges Festbett von z. B. Aktivkohle oder Adsorber­ harz ausgeführt wird.10. Device according to claim 7, characterized in that the adsorp Filling agent as granules, packing or powder-filled exchange bare pack or open-pore fixed bed of z. B. activated carbon or adsorber resin is running. 11. Einrichtung nach Anspruch 7, dadurch gekennzeichnet, daß das Adsorp­ tionsmittel als Adsorberharz oder Aktivkohle in Pulverform als Beschichtung eines retikulierten Polyurethan-Schaums angeboten wird.11. The device according to claim 7, characterized in that the adsorb tion agent as adsorber resin or activated carbon in powder form as a coating a reticulated polyurethane foam is offered. 12. Einrichtung nach Anspruch 11, dadurch gekennzeichnet, daß der unbeschichtete obere Abschnitt (5) des Polyurethan-Schaums (2) von dem Extraktionsmittel (10) geflutet ist.12. The device according to claim 11, characterized in that the uncoated upper portion ( 5 ) of the polyurethane foam ( 2 ) is flooded by the extractant ( 10 ). 13. Einrichtung nach Anspruch 12, dadurch gekennzeichnet, daß zwischen geflutetem und beschichtetem Abschnitt eine freie Zone (8, 11) angeordnet ist.13. The device according to claim 12, characterized in that a free zone ( 8 , 11 ) is arranged between the flooded and coated portion.
DE4103165A 1991-02-02 1991-02-02 Purifying contaminated effluent waters - by liq. liq. extraction followed by treatment in adsorption reactor Withdrawn DE4103165A1 (en)

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DE4103165A DE4103165A1 (en) 1991-02-02 1991-02-02 Purifying contaminated effluent waters - by liq. liq. extraction followed by treatment in adsorption reactor

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5413717A (en) * 1993-08-30 1995-05-09 Texaco Inc. Method of recovering MTBE from wastewater
US7267776B2 (en) * 2004-05-05 2007-09-11 Lanxess Deutschland Gmbh Foams for removing pollutants and/or heavy metals from flowable media
EP1832554A1 (en) * 2006-03-06 2007-09-12 Akzo Nobel N.V. Use of an adsorbent for the removal of liquid, gaseous and/ or dissolved constituents from a process stream
GB2516885A (en) * 2013-08-02 2015-02-11 Adler And Allan Ltd Coalescent hydrocarbon filter

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