DE102012000699A1 - Agent, useful to remove volatile heavy metals e.g. mercury, from gases, preferably from flue gases, comprises porous inorganic and/or organic materials, sulfur and binder for fixing sulfur on the inorganic and/or organic substances - Google Patents

Agent, useful to remove volatile heavy metals e.g. mercury, from gases, preferably from flue gases, comprises porous inorganic and/or organic materials, sulfur and binder for fixing sulfur on the inorganic and/or organic substances Download PDF

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DE102012000699A1
DE102012000699A1 DE201210000699 DE102012000699A DE102012000699A1 DE 102012000699 A1 DE102012000699 A1 DE 102012000699A1 DE 201210000699 DE201210000699 DE 201210000699 DE 102012000699 A DE102012000699 A DE 102012000699A DE 102012000699 A1 DE102012000699 A1 DE 102012000699A1
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sulfur
agent
mercury
inorganic
mixed
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wird später genannt werden Erfinder
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Ftu Forschung und Tech Entwicklung Im Umweltschutz GmbH
Ftu Forschung und Technische Entwicklung Im Umweltschutz GmbH
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Ftu Forschung und Tech Entwicklung Im Umweltschutz GmbH
Ftu Forschung und Technische Entwicklung Im Umweltschutz GmbH
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    • 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
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B01J20/106—Perlite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/64—Heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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    • 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
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    • 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
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    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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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    • 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
    • B01J20/28014—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 form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
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    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/30—Alkali metal compounds
    • B01D2251/304—Alkali metal compounds of sodium
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2251/608—Sulfates
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

Agent comprises porous inorganic and/or organic materials, sulfur and binder for fixing sulfur on the inorganic and/or organic substances. An independent claim is included for use of the agent for the removal of volatile heavy metals, preferably mercury, where the removal of volatile heavy metals comprises introducing the agent into the gas stream to be purified and mixing, reacting the obtained mixture with the pollutants and depositing the pollutants on fabric filters and/or electrostatic precipitators.

Description

Bei thermischen Prozessen, z. B. Hüttenprozessen, Kohlefeuerungen, Abfallverbrennungen und zahlreichen industriellen Verfahren werden Abgase erzeugt, die mit flüchtigen Schwermetallen, z. B. Cadmium, Quecksilber, Thallium, Arsen, Antimon und Blei belastet sind. Es handelt sich dabei um elementare, d. h. nullwertige Schwermetalle, oder Salze, vorzugsweise Chloride und Oxide. Weiterhin enthalten sie noch in vielen Fällen organische Schadstoffe, z. B. Dioxine, Furane, Aromaten und dergleichen.For thermal processes, eg. As metallurgical processes, coal firing, waste incineration and numerous industrial processes exhaust gases are generated with volatile heavy metals, eg. As cadmium, mercury, thallium, arsenic, antimony and lead are charged. These are elementary, d. H. zerovalent heavy metals, or salts, preferably chlorides and oxides. Furthermore, they still contain organic pollutants in many cases, eg. As dioxins, furans, aromatics and the like.

Üblicherweise werden die Gase abgekühlt und die Schadstoffe naß ausgewaschen. Häufig ist dies nicht ausreichend, wenn die Schwermetalle in elementarer Form vorliegen. Quecksilber z. B. wird als Element emittiert. Es läßt sich dann auch über eine Naßwäsche nicht aus dem Gas abtrennen. Hinzu kommt noch das Problem, daß flüchtige Schwermetallsalze auch nach der Naßwäsche als Aerosole und/oder schwerabscheidbarer Feinstaub emittiert werden. Auch die Dioxine, Aromaten und Halogenkohlenwasserstoffe werden nur unzureichend abgeschieden.Usually, the gases are cooled and the pollutants washed out wet. Often this is not sufficient if the heavy metals are present in elemental form. Mercury z. B. is emitted as an element. It can then be separated via a wet wash not from the gas. In addition, there is the problem that volatile heavy metal salts are emitted even after the wet scrubbing as aerosols and / or difficult-to-release fine dust. The dioxins, aromatics and halogenated hydrocarbons are also insufficiently deposited.

Eine andere Methode besteht darin, Abgasströme über Aktivkohle-Filter zu leiten. Dies führt zu einer Verminderung des Gehaltes an flüchtigen Schadstoffen, z. B. von Quecksilber, doch ist dieses Verfahren mit erheblichen Kosten belastet, da große Mengen hochaktiver Kohle eingesetzt werden müssen und immer die Gefahr der Schwelbrände im Kohlebett besteht. Über den stets vorhandenen Abrieb wird außerdem schadstoffhaltiger Feinstaub emittiert, der schwierig abzuscheiden ist. Im Falle von elementarem Quecksilber ist grundsätzlich Nullemission anzustreben.Another method is to pass exhaust streams through activated carbon filters. This leads to a reduction of the content of volatile pollutants, z. As mercury, but this process is burdened with significant costs, since large amounts of highly active coal must be used and there is always the risk of smoldering in the coal bed. In addition, pollutant-containing particulate matter, which is difficult to remove, is emitted via the abrasion that is always present. In the case of elemental mercury, zero emission should always be the aim.

Ein weiteres Verfahren besteht darin, Schwefel auf Aktivkohle aufzubringen und den Gasstrom darüber zu leiten. Die Quecksilberabscheidung und die Abtrennung organischer Schadstoffe ist zwar recht wirksam, doch bleiben die Probleme der Selbstentzündung und der Emission von Abrieb bestehen. Hinzu kommt noch, daß der allgemeine Einsatz von sulfidierter Kohle am exorbitanten Preis derselben scheitert. Weiterhin wird durch die Beladung der Aktivkohle das Porensystem verstopft und die aktive Oberfläche vermindert.Another method is to apply sulfur to activated carbon and pass the gas stream over it. Although mercury removal and separation of organic pollutants are quite effective, the problems of auto-ignition and emission of abrasion remain. In addition, the general use of sulphided coal at the exorbitant price of the same fails. Furthermore, the loading of the activated carbon blocks the pore system and reduces the active surface area.

Es hat deshalb nicht an weiteren Versuchen gefehlt, die Abscheidung von elementarem Quecksilber durch Oxidation zu ein- oder zweiwertigem Quecksilber zu verbessern.There has therefore been no lack of further attempts to improve the deposition of elemental mercury by oxidation to monovalent or divalent mercury.

Die dabei eingesetzten Oxidationsmittel, vorzugsweise Wasserstoffperoxid, reagieren jedoch mit allen oxidierbaren Stoffen, z. B. Schwefeldioxid. Dies bedeutet einen erheblichen Mehrverbrauch an Oxidationsmittel. Außerdem zersetzt sich Wasserstoffperoxid an den Stäuben des Abgases, z. B. Flugstaub, Calciumhydroxid, Aktivkohle und Herdofenkoks. Auch dies bedeutet einen erheblichen Mehrverbrauch an Oxidationsmittel.However, the oxidizing agent used, preferably hydrogen peroxide, but react with all oxidizable substances, eg. B. sulfur dioxide. This means a considerable excess consumption of oxidizing agent. In addition, hydrogen peroxide decomposes on the dusts of the exhaust gas, z. As flue dust, calcium hydroxide, activated carbon and Herdofenkoks. This also means a considerable additional consumption of oxidizing agent.

Es liegt demnach das Bedürfnis vor, aus den Gasströmen, vornehmlich von Abgasen thermischer Anlagen, flüchtige Schwermetalle, insbesondere Quecksilber, in ihren verschiedenen Verbindungsformen und auch als Elemente, gezielt, einfach und preiswert abzuscheiden, aber auch organische Schadstoffe, wie Dioxine und Furane zu erfassen und ebenfalls abzuscheiden. Mit der Erfindung können die gestellten Aufgaben gelöst werden.Accordingly, there is a need to selectively, simply and inexpensively separate from the gas streams, primarily exhaust gases of thermal plants, volatile heavy metals, in particular mercury, in their various forms of connection and also as elements, but also to detect organic pollutants, such as dioxins and furans and also to be separated. With the invention, the tasks can be solved.

Im Wesen besteht die Erfindung darin, elementaren Schwefel mit Hilfe von Bindemitteln auf poröse anorganische Stoffe und/oder organische Stoffe zu fixieren. Damit steht Schwefel im Reaktionsraum für die Oxidation von elementarem Quecksilber zur Verfügung und kann nicht als Einzelsubstanz ausgetragen werden. Neben elementarem Schwefel kann auch gebundener Schwefel in Form von Schwefel abgebenden Verbindungen eingesetzt werden.In essence, the invention consists in fixing elemental sulfur with the aid of binders to porous inorganic substances and / or organic substances. Thus, sulfur is available in the reaction space for the oxidation of elemental mercury and can not be discharged as a single substance. In addition to elemental sulfur, it is also possible to use bound sulfur in the form of sulfur-donating compounds.

Im Einzelnen ist das Mittel dadurch gekennzeichnet, daß die porösen anorganischen Stoffe als Traß, Bimsstein, Perlite, Kieselgur, Ziegelmehl, Tone, Blähton, Gasbeton, Aluminiumoxid und/oder Kieselgel vorliegen. Geeignet sind Stoffe, die ein Porenvolumen von 0,15 cm3/g und höher haben. Rheinischer Traß hat ein Porenvolumen von 0,15 cm3/g, Süddeutscher Traß (Suevit) von 0,2 cm3/g, Kieselgur 0,8 cm3/g.Specifically, the agent is characterized in that the porous inorganic substances are as a trass, pumice, perlite, kieselguhr, brick dust, clays, expanded clay, aerated concrete, alumina and / or silica gel. Suitable substances are those with a pore volume of 0.15 cm 3 / g and higher. Rheinischer Traß has a pore volume of 0.15 cm 3 / g, Süddeutscher Traß (Suevit) of 0.2 cm 3 / g, diatomaceous earth 0.8 cm 3 / g.

Die porösen organischen Stoffe Aktivkohle oder Herdofenkoks (HOK) haben ein Porenvolumen von 0.4 cm3/g.The porous organic substances activated charcoal or hearth furnace coke (HOK) have a pore volume of 0.4 cm 3 / g.

Schwefel liegt elementar in feinpulvriger Form vor oder er wird aus Schwefel abgebenden Verbindungen durch höhere Temperaturen oder Säuren im Reaktionsraum in sehr feiner Form abgeschieden. Geeignete Schwefel abgebende Verbindungen sind die gut wasserlöslichen Salze der Thiosulfate und der Polysulfide. Beispiele sind Natriumthiosulfat, Na2S2O3, und Natriumtetrasulfid, Na2S4.Sulfur is elemental in feinpulvriger form or it is deposited from sulfur donating compounds by higher temperatures or acids in the reaction space in very fine form. Suitable sulfur donating compounds are the readily water-soluble salts of thiosulfates and polysulfides. Examples are sodium thiosulfate, Na 2 S 2 O 3 , and sodium tetrasulfide, Na 2 S 4 .

Da aus Natronwasserglas bei Einwirkung von Säuren des Abgases Kieselgel in feinster Form abgeschieden wird und gleichzeitig feinst verteilter Schwefel aus den aufgeführten Verbindungen entsteht, liegt hier ein hochreaktives Gemisch zur Adsorption für Quecksilber und Oxidation des nullwertigen Quecksilbers zu höhenwertigen Stufen vor, das sich leicht abscheiden läßt.Since silica gel is deposited in the finest form from soda water glass on exposure to acids of the exhaust gas and at the same time very finely divided sulfur is formed from the listed compounds, here is a highly reactive mixture for adsorption of mercury and oxidation of zerovalent mercury to höhenwertigen stages, which can be easily separated ,

Die anorganischen Bindemittel liegen als Natronwasserglas, Sumpfkalk, Zement und/oder Bindemittel aus dem Bauwesen, die wie Zement nach Wasserzugabe erhärten, vor. Von den organischen Klebstoffen werden lösungsmittelfreie Kleber/Bindemittel oder wäßrige Dispersionen bevorzugt.The inorganic binders are available as sodium silicate, lime, cement and / or Binders from the construction industry, which harden like cement after the addition of water. Of the organic adhesives, solventless adhesives / binders or aqueous dispersions are preferred.

Auf die porösen Stoffe werden elementarer Schwefel und/oder gebundener Schwefel in Form von Schwefel abgebender Verbindungen dadurch aufgetragen, daß Schwefel oder die Schwefel abgebenden Verbindungen mit den Bindemitteln in einer eigenen Stufe vermischt und dann zu diesem Gemisch der poröse Stoff zugegeben wird. Es wird mindestens soviel der porösen Stoffe zugegeben bis ein Pulver entsteht, das in den Abgas- oder Gasstrom eingesetzt werden kann.Elemental sulfur and / or bound sulfur in the form of sulfur donating compounds are applied to the porous materials by mixing sulfur or the sulfur donating compounds with the binders in a separate step and then adding the porous material to this mixture. At least as much of the porous material is added until a powder is formed which can be used in the exhaust or gas stream.

Besonders bewährt hat sich als Bindemittel Natronwasserglas. Dieses ist flüssiges Natriumsilikat, das alkalisch reagiert. Zu dem Schwefel-Wasserglas-Gemisch wird soviel von den porösen Stoffen gegeben, daß ein pulverförmiger Stoff entsteht, der z. B. beim Flugstromverfahren eingesetzt werden kann. Z. B. ergeben 2 g feinpulvriger Schwefel und 5 g Wasserglas mit einem Silikatgehalt von 42 Gew.-% und 50 g Süddeutscher Traß ein trockenes Pulver.Sodium waterglass has proven particularly useful as a binding agent. This is liquid sodium silicate that reacts alkaline. To the sulfur-water glass mixture is added so much of the porous materials that a powdery substance is formed, the z. B. can be used in the air flow method. For example, 2 g of finely powdered sulfur and 5 g of water glass having a silicate content of 42% by weight and 50 g of South German Traß give a dry powder.

Bei Verwendung von Calciumhydroxid, z. B. in Form von Sumpfkalk oder als festes Calciumhydroxid, ist es notwendig soviel Wasser zuzusetzen, daß eine Suspension entsteht, die leicht mit Schwefel zu mischen ist und sich auch einfach auf die porösen Stoffe auftragen läßt.When using calcium hydroxide, z. B. in the form of limestone or solid calcium hydroxide, it is necessary to add so much water that a suspension is formed, which is easy to mix with sulfur and can also be easily applied to the porous materials.

Je nach Verwendungszweck werden die porösen anorganischen oder organischen Stoffe als Pulver oder als Granulat eingesetzt. Für das Flugstromverfahren ist eine Korngröße von < 100 μm, besser < 50 μm, erforderlich. Als Granulate werden die geschwefelten porösen anorganischen Stoffe mit einer Korngröße im Bereich von 1–10 mm, vorzugsweise 2–5 mm, verwendet. Es ist möglich, die porösen anorganischen und/oder organischen Stoffe als vorgegebenes Granulat zu schwefeln oder pulverförmige poröse anorganische und/oder organische Stoffe mit Schwefel oder Schwefel abgebenden Verbindungen und Bindemittel zu granulieren.Depending on the intended use, the porous inorganic or organic substances are used as powder or as granules. For the airflow method, a particle size of <100 microns, better <50 microns, required. The granules used are the sulfurized porous inorganic substances having a particle size in the range of 1-10 mm, preferably 2-5 mm. It is possible to sulfurize the porous inorganic and / or organic substances as specified granules or to granulate powdery porous inorganic and / or organic substances with sulfur or sulfur donating compounds and binders.

Für die Gasreinigung bei sauren Abgasen werden die Mittel nach Anspruch 1 je nach Bedarf noch mit Calciumhydroxid, Calciumcarbonat, Branntkalk, Dolomit, Natriumcarbonat und/oder Natriumbicarbonat gemischt. Dabei ist Calciumhydroxid bei säurehaltigen Abgasen, z. B. bei Abfallverbrennungsanlagen, das bevorzugte Mittel. Die Menge der basischen Stoffe richtet sich nach der Säurebelastung des Abgases.For gas purification in acidic waste gases, the compositions according to claim 1 are mixed with calcium hydroxide, calcium carbonate, quicklime, dolomite, sodium carbonate and / or sodium bicarbonate as required. This calcium hydroxide is acidic exhaust gases, z. As in waste incineration plants, the preferred means. The amount of basic substances depends on the acid load of the exhaust gas.

Weiterhin ist es möglich, die mit Schwefel beladenen porösen anorganischen Stoffe noch mit Aktivkohle und/oder HOK zu vermischen.Furthermore, it is possible to mix the sulfur-loaded porous inorganic substances with activated carbon and / or HOK.

Die Aktivkohlen und der Herdofenkoks unterstützen die Abscheidung des Quecksilbers und der organischen Schadstoffe, wie Dioxine, chlorierte Kohlenwasserstoffe und aromatische Kohlenwasserstoffe.The activated carbons and the hearth furnace coke assist in the separation of mercury and organic pollutants such as dioxins, chlorinated hydrocarbons and aromatic hydrocarbons.

Im Sinne der Erfindung werden die Mittel und ihre Verwendung bevorzugt, bei denen Schwefel oder die Schwefel abgebenden Verbindungen auf den anorganischen Stoffen fixiert sind und damit Aktivkohle und/oder Herdofenkoks frei von Poren verstopfenden Zusätzen sind. Damit wird die Adsorptionsfähigkeit der Aktivkohle und des Herdofenkoks nicht beeinträchtigt.For the purposes of the invention, the agents and their use are preferred in which sulfur or the sulfur donating compounds are fixed on the inorganic materials and thus activated carbon and / or Herdofenkoks are pore-clogging additives. Thus, the adsorption capacity of the activated carbon and the Herdofenkoks is not affected.

Die Mengenverhältnisse lassen sich nach Zusammensetzung des zu behandelnden Abgases beliebig wählen.The proportions can be chosen arbitrarily according to the composition of the exhaust gas to be treated.

Die Verwendung der Mittel besteht darin, daß das pulverförmige Material auf bekannte Weise in den Abgasstrom eingedüst, in diesem verwirbelt und anschließend die Feststoffe an einem Gewebefilter oder in einem Elektrofilter abgeschieden werden.The use of the means is that the powdery material is injected in a known manner in the exhaust gas stream, swirled in this and then the solids are deposited on a fabric filter or in an electrostatic precipitator.

Eine andere Verwendung besteht darin, daß die nach den vorliegenden Ansprüchen als Granulat verwendet werden. Die Gasströme werden dann durch diese Feststoffschicht geleitet.Another use is that of the present claims are used as granules. The gas streams are then passed through this solid layer.

Die Temperatur muß hierbei so hoch sein, daß es nicht zu Kondensationen von Wasser auf den erfindungsgemäßen Mitteln kommt. Im allgemeinen wird hierzu eine Temperatur von 30°C oberhalb des Taupunktes des Gases gewählt.The temperature must be so high that it does not come to condensation of water on the inventive compositions. In general, a temperature of 30 ° C above the dew point of the gas is chosen for this purpose.

Die erfinderischen Mittel können für sich allein eingesetzt werden oder beliebig in Mischung mit Calciumhydroxid, Calciumcarbonat, Branntkalk, Natriumcarbonat und/oder Natriumbicarbonat und/oder Aktivkohle und/oder Herdofenkoks. In dieser Form werden sie eingesetzt, wenn nicht nur Quecksilber aus Gasströmen abgeschieden werden sollen, sondern auch saure Bestandteile des Abgases, z. B. Chlorwasserstoff. Die Aktivkohlen unterstützen die Abscheidung organischer Schadstoffe.The inventive compositions may be used alone or in any admixture with calcium hydroxide, calcium carbonate, quicklime, sodium carbonate and / or sodium bicarbonate and / or activated carbon and / or hearth furnace coke. In this form, they are used when not only mercury to be separated from gas streams, but also acidic constituents of the exhaust gas, for. For example, hydrogen chloride. The activated carbons support the separation of organic pollutants.

Verfahren zur Herstellung der Mittel:Process for preparing the compositions:

5 g Süddeutscher Traß (Suevit), Korngröße < 45 μm, 0,2 g feinpulvriger Schwefel und 0,5 g Natronwasserglas mit einem Feststoffgehalt von 42% wurden in einem Schlagkreuz-Mischer 5 Minuten gemischt. Es entstand ein trockenes, pulvriges Gemisch. Die prozentualen Mischungsverhältnisse lauten: Traß 87,7%, Schwefel 3,5%, Wasserglas 8,8%. Diese Mischung wird als Traßmischung-1 bezeichnet.5 g of Süddeutscher Traß (Suevit), grain size <45 .mu.m, 0.2 g of finely powdered sulfur and 0.5 g of sodium silicate with a solids content of 42% were mixed in a beater mixer for 5 minutes. The result was a dry, powdery mixture. The percentage mixing ratios are: Traß 87.7%, sulfur 3.5%, water glass 8.8%. This mixture is called Traßmischung-1.

BeispieleExamples

Beispiel 1example 1

Über 12,5 g der Traßmischung-1 wurden bei 140°C 27 l des folgenden Gases geleitet: Stickstoff 90 Vol.-%, Sauerstoff 10 Vol.-%, HCl 18,1 mg/l, Feuchte 0,15 g/l, Hg (als HgCl2) 0,3 μg/l.About 12.5 g of Traßmischung-1 were passed at 140 ° C 27 l of the following gas: nitrogen 90 vol .-%, oxygen 10 vol .-%, HCl 18.1 mg / l, humidity 0.15 g / l , Hg (as HgCl 2 ) 0.3 μg / l.

Die Hg-Abscheidung betrug 62%.The Hg deposition was 62%.

Beispiel 2Example 2

Für den Einsatz der Traßmischung zur Reinigung eines salzsäurehaltigen und quecksilberhaltigen Abgases wurde die Traßmischung-1 mit soviel Calciumhydroxid vermischt, daß ein Absorbens mit einem Calciumhydroxidgehalt von 95% entstand. Der Rest war 5% Traßmischung 1. Die prozentuale Zusammensetzung des Gemisches war: Calciumhydroxid 95%, Traß 4,4%, Schwefel 0,18% und Natronwasserglas 0,44%.For the use of the Traßmischung for cleaning a hydrochloric acid and mercury-containing exhaust gas Traßmischung-1 was mixed with sufficient calcium hydroxide that an absorbent with a calcium hydroxide content of 95% was formed. The remainder was 5% trace mixture 1. The percent composition of the mixture was: calcium hydroxide 95%, turf 4.4%, sulfur 0.18% and soda water glass 0.44%.

Über 250 mg dieses Gemisches wurden bei 140°C 27 l des folgenden Gases geleitet: Stickstoff 90 Vol.-%, Sauerstoff 10 Vol.-%, HCl 18,1 mg/l, Feuchte 0,15 g/l, Hg (als HgCl2) 0,3 μg/l.Over 250 mg of this mixture were passed at 140 ° C 27 l of the following gas: nitrogen 90 vol .-%, oxygen 10 vol .-%, HCl 18.1 mg / l, moisture 0.15 g / l, Hg (as HgCl2) 0.3 μg / l.

Die Quecksilberabscheidung betrug 70%.The mercury removal was 70%.

Beispiel 3Example 3

Unter den Versuchsbedingungen von Beispiel 2 wurde ein Gemisch aus 90% Calciumhydroxid und 10% Traßmischung eingesetzt. Die prozentuale Zusammensetzung des Gemisches war: Calciumhydroxid 90 Gew.-%, Traß 8,8 Gew.-%, Schwefel 0,36 Gew.-%, Wasserglas 0,88 Gew.-%.Under the experimental conditions of Example 2, a mixture of 90% calcium hydroxide and 10% Traßmischung was used. The percent composition of the mixture was: calcium hydroxide 90% by weight, Tray 8.8% by weight, sulfur 0.36% by weight, water glass 0.88% by weight.

Die Quecksilberabscheidung betrug 85%.The mercury deposition was 85%.

Die Verdoppelung des Schwefelgehaltes brachte eine deutliche Erhöhung der Quecksilberabscheidung.The doubling of the sulfur content brought a significant increase in mercury removal.

Beispiel 4Example 4

Es wurden Traß-Schwefel-Gemische ohne Natronwasserglas hergestellt und diese dann mit Calciumhydroxid vermischt.
Mischung 1: Calciumhydroxid 95 Gew.-&, Traß 4,8 Gew.-%, Schwefel 0,2 Gew.-%
Mischung 2: Calciumhydroxid 90 Gew.-%, Traß 9,65 Gew.-%, Schwefel 0,35 Gew.-% Unter den Versuchbedingungen der vorhergehenden Beispiele betrug die Quecksilberabscheidung bei Mischung 1 39%, bei Mischung 2 44%.Traß-sulfur mixtures were prepared without soda waterglass and then mixed with calcium hydroxide.
Mixture 1: calcium hydroxide 95% by weight, Traß 4.8% by weight, sulfur 0.2% by weight
Mixture 2: calcium hydroxide 90% by weight, Trap 9.65% by weight, sulfur 0.35% by weight Under the experimental conditions of the preceding examples, the mercury deposition in mixture 1 was 39%, in mixture 2 44%.

Beispiel 5Example 5

5 g Kieselgur mit einem Porenvolumen von 0,8 cm3/g, einer Teilchengröße von 8,5 μm und einem Naßvolumen von 430 g/l und 1 ml Natriumtetrasulfid-Lösung mit einem Gehalt von 40% Natriumtetrasulfid sowie 0,5 g Natronwasserglas wurden in einem Schlagkreuz-Mischer 5 Minuten gemischt. Es entstand ein lockeres Pulver.5 g of kieselguhr with a pore volume of 0.8 cm 3 / g, a particle size of 8.5 microns and a wet volume of 430 g / l and 1 ml of sodium tetrasulfide solution containing 40% sodium tetrasulfide and 0.5 g of sodium silicate were mixed in a beater mixer for 5 minutes. It created a loose powder.

Über 250 mg dieses Gemisches wurde unter den Bedingungen von Beispiel 1 das Prüfgas geleitet.Over 250 mg of this mixture was passed under the conditions of Example 1, the test gas.

Die Quecksilberabscheidung betrug 92%.The mercury separation was 92%.

Die Bindung von Schwefel an poröse Stoffe mit Natronwasserglas führt, wie am Beispiel von Traß und Kieselgur gezeigt werden konnte, zu einer deutlichen Steigerung der Quecksilberabscheidung! Erfindungsgemäß schwefelfixierte poröse anorganische Stoffe erreichen und übertreffen damit die Quecksilber-Abscheideleistung von Aktivkohlen! Sie sind damit in Kombination mit Aktivkohlen ein hervorragendes Adsorbens zur Abgasreinigung.The binding of sulfur to porous materials with soda water glass leads, as the example of Traß and diatomaceous earth could be shown, to a significant increase in mercury removal! According to the invention, sulfur-fixed porous inorganic substances reach and exceed the mercury separation efficiency of activated carbons! In combination with activated carbons, they are an excellent adsorbent for exhaust gas purification.

Claims (14)

Mittel bestehend aus porösen anorganischen und/oder organischen Stoffen, Schwefel und Bindemittel zur Fixierung von Schwefel auf den anorganischen und/oder organischen Stoffen.Agent consisting of porous inorganic and / or organic substances, sulfur and binder for fixing sulfur on the inorganic and / or organic substances. Mittel nach Anspruch 1, dadurch gekennzeichnet, daß die porösen anorganischen Stoffe als Traß, Bimsstein, Perlite, Kieselgur, Ziegelmehl, Tone, Blähton, Gasbeton, Aluminiumoxid und/oder Kieselgel vorliegen, die organischen Stoffe als Aktivkohle und/oder Herdofenkoks vorliegen, die Bindemittel als Natronwasserglas, Sumpfkalk und/oder Bindemittel aus dem Bauwesen, die wie Zement nach Wasserzugabe erhärten, oder als organische Klebstoffe vorliegen, und daß Schwefel feinpulvrig in elementarer Form oder gebunden in Form Schwefel abgebender Verbindungen vorliegt.Means according to claim 1, characterized in that the porous inorganic substances are present as trass, pumice, perlite, kieselguhr, brick dust, clays, expanded clay, aerated concrete, alumina and / or silica gel, the organic substances being activated carbon and / or hearth furnace coke, the binding agents as soda waterglass, lime lime and / or building binders which harden like cement after addition of water, or as organic adhesives, and that sulfur is finely powdery in elemental form or bound in the form of sulfur-donating compounds. Mittel nach den Ansprüchen 1–2, dadurch gekennzeichnet, daß die festen Stoffe in feinpulvriger Form mit einer Korngröße von < 100 μm, vorzugsweise < 50 μm vorliegen oder als Granulat mit einer Korngröße im Bereich von 1–10 mm, vorzugsweise 2–5 mm.Agent according to claims 1-2, characterized in that the solids are present in finely powdered form with a particle size of <100 microns, preferably <50 microns, or as granules having a particle size in the range of 1-10 mm, preferably 2-5 mm , Mittel nach den vorhergehenden Ansprüchen dadurch gekennzeichnet, daß Schwefel in Form von Schwefel abgebenden Verbindungen vorliegt, die Schwefel bei Temperaturen über 100°C oder durch Säuren des Gases abscheiden.Agent according to the preceding claims, characterized in that sulfur is present in the form of sulfur-donating compounds which precipitate sulfur at temperatures above 100 ° C or by acids of the gas. Mittel nach Anspruch 4, dadurch gekennzeichnet, daß als Schwefel abscheidende Verbindungen wasserlösliche Thiosulfate, z. B. Natriumthiosulfat, und/oder als Polysulfide, z. B. Natriumtetrasulfid, vorliegen. Agent according to claim 4, characterized in that as sulfur-depositing compounds water-soluble thiosulfates, e.g. As sodium thiosulfate, and / or as polysulfides, eg. For example, sodium tetrasulfide present. Mittel nach Ansprüchen 1–5, dadurch gekennzeichnet, daß sie mit den basischen Stoffen Calciumhydroxid, Calciumcarbonat, Branntkalk, Natriumcarbonat und/oder Natriumbicarbonat gemischt sind.Composition according to Claims 1-5, characterized in that they are mixed with the basic substances calcium hydroxide, calcium carbonate, quicklime, sodium carbonate and / or sodium bicarbonate. Mittel nach Ansprüchen 1–5, dadurch gekennzeichnet, daß sie Aktivkohle und/oder Herdofenkoks gemischt sind.Composition according to claims 1-5, characterized in that they are mixed activated carbon and / or Herdofenkoks. Mittel nach Ansprüchen 1–5, dadurch gekennzeichnet, daß sie mit den basischen Stoffen Calciumhydroxid, Calciumcarbonat, Branntkalk, Natriumcarbonat und/oder Natriumbicarbonat und/oder mit Aktivkohle und/oder Herdofenkoks gemischt sind.Compositions according to Claims 1-5, characterized in that they are mixed with the basic substances calcium hydroxide, calcium carbonate, quicklime, sodium carbonate and / or sodium bicarbonate and / or with activated carbon and / or hearth furnace coke. Mittel aus feinpulvrigem Traß, auf dem mit Natronwasserglas feinpulvriger Schwefel direkt oder als gebundener Schwefel in Form von Schwefel abgebenden Verbindungen aufgetragen ist.Agent of feinpulvrigem Traß, on which with soda water glass finely powdered sulfur directly or as bound sulfur in the form of sulfur donating compounds is applied. Mittel aus feinpulvrigem Traß nach Anspruch 9, dadurch gekennzeichnet, daß sie mit basischen Stoffen nach Anspruch 6 und/oder mit Aktivkohle und/oder Herdofenkoks nach Anspruch 7 vermischt sind.Finely powdery pulp means according to claim 9, characterized in that they are mixed with basic substances according to claim 6 and / or with activated carbon and / or hearth furnace coke according to claim 7. Mittel aus 80–95 Gew.-% feinpulvrigem Traß, 1–6 Gew.-% feinpulvrigem Schwefel und 4–14 Gew.-% Natronwasserglas.Agent of 80-95 wt .-% feinpulvrigem Traß, 1-6 wt .-% feinpulvrigem sulfur and 4-14 wt .-% sodium silicate. Verwendung der Mittel nach den vorhergehenden Ansprüchen zur Entfernung von flüchtigen Schwermetallen, insbesondere von Quecksilber, dadurch gekennzeichnet, daß die Mittel in den zu reinigenden Gasstrom eingebracht, mit diesem durchmischt, mit den Schadstoffen zur Reaktion gebracht und an Gewebefiltern und/oder Elektrofiltern abgeschieden werden.Use of the agents according to the preceding claims for the removal of volatile heavy metals, in particular of mercury, characterized in that the means are introduced into the gas stream to be cleaned, mixed with this, reacted with the pollutants and deposited on fabric filters and / or electrostatic precipitators. Verwendung der Mittel nach den vorhergehenden Ansprüchen zur Entfernung von flüchtigen Schwermetallen, insbesondere Quecksilber, chlorierten Dioxinen und Furanen, chlorierten aromatischen und aliphatischen Kohlenwasserstoffen, chlorierten Biphenylen, aromatischen Kohlenwasserstoffen, toxischen organischen Verbindungen, Chlorwasserstoff und/oder Schwefeldioxid und Stickstoffoxiden aus Gasen, insbesondere aus Abgasen, dadurch gekennzeichnet, daß ein Mittel nach einem der vorhergehenden Ansprüche 1–9 in den Gasstrom eingebracht wird, die schädlichen Inhaltsstoffe des Gases mit dem Mittel bei einer Temperatur von 20–400°C, insbesondere 60–250°C, vorzugsweise 120–210°C, behandelt werden und die Reaktionsprodukte sowie nicht umgesetztes Mittel an Gewebefiltern und/oder Elektrofiltern abgeschieden werden.Use of the agents according to the preceding claims for the removal of volatile heavy metals, in particular mercury, chlorinated dioxins and furans, chlorinated aromatic and aliphatic hydrocarbons, chlorinated biphenyls, aromatic hydrocarbons, toxic organic compounds, hydrogen chloride and / or sulfur dioxide and nitrogen oxides from gases, in particular from exhaust gases , characterized in that an agent according to any one of the preceding claims 1-9 is introduced into the gas stream, the harmful ingredients of the gas with the agent at a temperature of 20-400 ° C, in particular 60-250 ° C, preferably 120-210 ° C, and the reaction products and unreacted agent are deposited on fabric filters and / or electrostatic precipitators. Verwendung der Mittel nach Anspruch 1–10, dadurch gekennzeichnet, daß die Mittel nach den Ansprüchen 1–3 sowie 6–8 und die basischen Stoffe nach Anspruch 4 und/oder Aktivkohle oder Herdofenkoks nach Anspruch 5 getrennt in den Gasstrom eingegeben und dort vermischt werden.Use of the agents according to Claims 1-10, characterized in that the agents according to Claims 1-3 and 6-8 and the basic substances according to Claim 4 and / or activated carbon or hearth furnace coke according to Claim 5 are introduced separately into the gas stream and mixed there ,
DE201210000699 2012-01-16 2012-01-16 Agent, useful to remove volatile heavy metals e.g. mercury, from gases, preferably from flue gases, comprises porous inorganic and/or organic materials, sulfur and binder for fixing sulfur on the inorganic and/or organic substances Withdrawn DE102012000699A1 (en)

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DE102007020421A1 (en) * 2007-04-27 2008-10-30 Rwe Power Ag Process for the preparation of elemental sulfur doped carbonaceous adsorbents and methods for exhaust gas purification using such adsorbents
US20100004119A1 (en) * 2008-07-03 2010-01-07 Kishor Purushottam Gadkaree Sorbent Comprising Activated Carbon Particles, Sulfur And Metal Catalyst

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CN110386795A (en) * 2019-08-31 2019-10-29 郑州恒博环境科技股份有限公司 A kind of light flame-retardant diatomite brick and preparation method thereof
CN110357557B (en) * 2019-08-31 2022-02-08 郑州恒博环境科技股份有限公司 Flame-retardant diatomite wall brick and preparation method thereof
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