DE19718131A1 - Regeneration of black liquor from wood digester - Google Patents

Regeneration of black liquor from wood digester

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Publication number
DE19718131A1
DE19718131A1 DE1997118131 DE19718131A DE19718131A1 DE 19718131 A1 DE19718131 A1 DE 19718131A1 DE 1997118131 DE1997118131 DE 1997118131 DE 19718131 A DE19718131 A DE 19718131A DE 19718131 A1 DE19718131 A1 DE 19718131A1
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Germany
Prior art keywords
gas
molten salt
gasification
gasification gas
bath
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Granted
Application number
DE1997118131
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German (de)
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DE19718131C2 (en
Inventor
Manfred Dr Schingnitz
Juergen Dr Goerz
Wolfgang Seidel
Dietmar Degenkolb
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Future Energy GmbH
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KRC Umwelttechnik GmbH
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Priority to DE1997118131 priority Critical patent/DE19718131C2/en
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/06—Treatment of pulp gases; Recovery of the heat content of the gases; Treatment of gases arising from various sources in pulp and paper mills; Regeneration of gaseous SO2, e.g. arising from liquors containing sulfur compounds
    • D21C11/063—Treatment of gas streams comprising solid matter, e.g. the ashes resulting from the combustion of black liquor
    • D21C11/066—Separation of solid compounds from these gases; further treatment of recovered products
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/46—Gasification of granular or pulverulent flues in suspension
    • C10J3/48—Apparatus; Plants
    • C10J3/485—Entrained flow gasifiers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/74—Construction of shells or jackets
    • C10J3/76—Water jackets; Steam boiler-jackets
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/82—Gas withdrawal means
    • C10J3/84—Gas withdrawal means with means for removing dust or tar from the gas
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/82—Gas withdrawal means
    • C10J3/84—Gas withdrawal means with means for removing dust or tar from the gas
    • C10J3/845—Quench rings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/101—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids with water only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/103—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkali- or earth-alkali- or NH4 salts or inorganic acids derived from sulfur
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/12—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkaline-reacting including the revival of the used wash liquors
    • C10K1/122—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkaline-reacting including the revival of the used wash liquors containing only carbonates, bicarbonates, hydroxides or oxides of alkali-metals (including Mg)
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/12—Combustion of pulp liquors
    • D21C11/122—Treatment, e.g. dissolution, of the smelt
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/12—Combustion of pulp liquors
    • D21C11/125—Decomposition of the pulp liquors in reducing atmosphere or in the absence of oxidants, i.e. gasification or pyrolysis

Abstract

To regenerate the recovered liquids from a wood digester, they are gassed in a free flow reactor at temps. over the melting point of the sodium compounds followed by jet cooling over or below the dew point for molten salts to drop in a water bath. In the gassing zone, the gas and the molten salts are taken off separately. The gas take-off has a jet cooling system using water or a watery sodium salt solution, before the gas flows to a further processing station. The molten salts flow into a water bath, containing a watery sodium hydroxide solution, where they dissolve. The concentration in the bath is controlled by a fresh water feed or the delivery of a low concentration sodium salt solution. Also claimed is an assembly with units (4,8) in the gassing zone (3) to separate the gas and the molten salts. Jets (7) to cool the gas are at the unit (4) to take off the gas, and jets (9) to cool and release the molten salts are at the cooling zone (5) of the gassing system. A bath (6) to dissolve the salts is below the gassing zone (3). The gas is passed out through an exhaust (12).

Description

Die Erfindung betrifft ein Verfahren zur Regeneration einer beim Kraftprozeß zum Aufschluß von Holz anfallenden Flüssigkeit durch Vergasung entsprechend dem Oberbegriff des Patentanspruches 1 und eine Vorrichtung zur Durchführung des Verfahrens.The invention relates to a method for the regeneration of a power process Digestion of liquid wood by gasification according to the Preamble of claim 1 and a device for performing the Procedure.

Der allgemein bekannte Kraftprozeß beruht darauf, daß mit einer aus Natronlauge sowie Natriumkarbonat und -sulfid bestehenden wäßrigen Lösung zerkleinertes Holz zur Zellulosegewinnung aufgeschlossen wird. Die eingesetzte Flüssigkeit reichert sich während dieses Prozesses mit organischen Bestandteilen aus der Holzsubstanz an. Es entsteht eine als Black Liquor bezeichnete Flüssigkeit, deren Trockensubstanz zu 30-40 Masse-% aus Natronlauge und Natriumsalzen sowie zu 60-70 Masse-% aus organischer Substanz besteht.The well-known power process is based on the fact that with a sodium hydroxide solution as well as sodium carbonate and sulfide existing aqueous solution Wood for cellulose production is broken down. The liquid used enriches itself with organic components from the Wood substance. This creates a liquid called black liquor, whose Dry matter to 30-40 mass% from sodium hydroxide and sodium salts as well 60-70% by mass consists of organic matter.

Zur Regeneration und Wiederverwendung durch eine Kreislaufführung wird Black Liquor nach dem stand der Technik nach einer Eindampfung auf einen Trockensubstanzgehalt von 70-80 Masse-% in einer Kesselanlage drucklos verbrannt, um die organischen Bestandteile zu entfernen. Gleichzeitig wird die dabei frei werdende Energie im Kessel genutzt. Um das während des Aufschlußprozesses zu Na-Sulfat oxidierte Na-Sulfid wieder zu gewinnen, wird der Verbrennungsvorgang zweistufig betrieben. Im unteren Teil der Kesselanlage wird zunächst nur eine partielle Verbrennung im reduzierenden Bereich vorgenommen so daß die gewünschte Zusammensetzung der Salzschmelze erreicht wird; die vollständige Verbrennung vollzieht sich danach durch Sekundärluftzuführung im oberen Teil. Die aus dem unteren Kesselteil ablaufende regenerierte Salzschmelze wird gelöst und als Green Liquor einer Kaustifizierung zur CO2- Abtrennung unterzogen, um danach als White Liquor dem Prozeß des Holzaufschlusses wieder zugeführt zu werden, Gewünschte Hauptbestandteile des White Liquor sind Natriumlauge und Natriumsulfid in hohen Konzentrationen.For regeneration and reuse by means of a circuit, state-of-the-art black liquor is burned without pressure after evaporation to a dry matter content of 70-80% by mass in a boiler system in order to remove the organic constituents. At the same time, the energy released in the boiler is used. In order to recover the Na sulfide oxidized to Na sulfate during the digestion process, the combustion process is carried out in two stages. In the lower part of the boiler system, only a partial combustion is carried out in the reducing area so that the desired composition of the molten salt is achieved; The complete combustion then takes place through secondary air supply in the upper part. The regenerated molten salt flowing out of the lower part of the boiler is dissolved and subjected to causticization for CO 2 separation as green liquor, in order to be reused as a white liquor in the process of wood digestion.The main components of white liquor are sodium hydroxide and sodium sulfide in high concentrations.

Ein Nachteil des Kraft-Prozesses besteht darin, daß im überstöchiometrisch betriebenen oberen Teil der Kesselanlage bei der Black-Liquor-Verbrennung Maßnahmen zur Rauchgasreinigung (Rauchgasentschwefelung und Elektrofilter) entfernt werden, bevor das Rauchgas an die Atmosphäre abgegeben werden darf. Außerdem enthält auch die Salzschmelze einen Anteil von Natriumsulfat und -thiosulfat, die in den weiteren Aufbereitungsstufen nicht entfernt werden und, da sie beim Holzaufschluß nicht benötigt werden, als Ballast im Kraftprozeß umlaufen.A disadvantage of the Kraft process is that it's superstoichiometric operated upper part of the boiler plant in the black liquor combustion  Measures for flue gas cleaning (flue gas desulfurization and electrostatic precipitators) removed before the flue gas is released into the atmosphere may. In addition, the molten salt also contains a proportion of sodium sulfate and -thiosulfate, which are not removed in the further treatment stages and, because they are not needed for wood digestion, as ballast in the power process circulate.

Außerdem entsteht während der Black-Liquor-Verbrennung bei üblichen Temperaturen von 900 bis 1000°C nur ein vernachlässigbarer Anteil von Natronlauge in der Salzschmelze, der jedoch wesentlich für den Prozeß des Holzaufschlusses ist. Der Großteil der benötigten Natronlauge wird in dem der Verbrennung nachgeschalteten Kaustifizierungsprozeß gewonnen, der Rest muß als make up NaOH zudosiert werden.In addition, during normal black liquor combustion occurs Temperatures from 900 to 1000 ° C only a negligible proportion of Sodium hydroxide solution in the molten salt, which is however essential for the process of Wood outcrop is. The majority of the sodium hydroxide solution required is in the Combustion downstream caustification process won, the rest must can be added as makeup NaOH.

Ein weiterer Nachteil des dem Stand der Technik entsprechenden Kraftprozesses besteht darin, daß die chemisch gebundene Wärme der Black Liquor mit einem geringen Kesselwirkungsgrad in Dampf umgewandelt wird. Die Erzeugung eines Brenngases ist ausgeschlossen.Another disadvantage of the prior art power process consists of the chemically bound heat of the black liquor is converted to steam with a low boiler efficiency. The Generation of a fuel gas is excluded.

Nun sind in der Literatur auch Verfahren zur Pyrolyse und Partialverbrennung von Natriumverbindungen enthaltenden Flüssigkeiten bekannt, beispielsweise WO 93/02249.Processes for pyrolysis and partial combustion of Liquids containing sodium compounds are known, for example WO 93/02249.

Dabei erfolgt die Pyrolyse und Partialverbrennung in einem ungekühlten, ausgemauerten Reaktionsraum und ist mit dem Nachteil verbunden, daß das Ausmauerungsmaterial von der im Prozeß entstehenden flüssigen Schmelze und dem schwefelhaltigen Rohgas angegriffen wird, was die Standzeit der Reaktorausmauerung verringert.The pyrolysis and partial combustion take place in an uncooled, bricked reaction chamber and is associated with the disadvantage that the Masonry material from the liquid melt and the raw gas containing sulfur is attacked, which increases the service life of the Reactor lining reduced.

Außerdem führt der nachgeschaltete trockene Schlackeabzug zu einem apparativen Mehraufwand für die Trennung von erzeugtem Gas und Salzpartikeln und ist mit der Gefahr von Anbackungen und Verkrustungen im Gasweg und Salzaustrag verbunden.In addition, the downstream dry slag discharge leads to a additional equipment expenditure for the separation of generated gas and salt particles and is with the risk of caking and incrustation in the gas path and Salt discharge connected.

Aus EP 0459962 A1 ist ein Verfahren bekannt, das ein Quenchsystem zur Rohgaskühlung nutzt, um die mit dem Rohgas aus dem Reaktor ausgetragenen Salze in gelöster Form naß auszutragen. Mit diesem Verfahrensvorschlag ist der Nachteil verbunden, daß auf Grund der längeren Verweilzeit der Salze unter Anwesenheit von H2O, CO2 und H2S im Rohgas bis zu ihrer Lösung im Wasser chemische Reaktionen zur unerwünschten Karbonatbildung führen. Die Gewinnung von Natronlauge durch den Vergasungsprozeß ist, wenn überhaupt, nur in geringem Umfang möglich.From EP 0459962 A1 a method is known which uses a quench system for raw gas cooling in order to wetly remove the salts discharged from the reactor with the raw gas in dissolved form. This process proposal has the disadvantage that, due to the longer residence time of the salts in the presence of H 2 O, CO 2 and H 2 S in the raw gas until they are dissolved in water, chemical reactions lead to undesirable carbonate formation. The extraction of caustic soda by the gasification process is only possible to a limited extent, if at all.

Alle bekannten Verfahren zur thermischen Regeneration von Black Liquor zu Green Liquor sind mit dem Nachteil behaftet, daß bei der thermischen Behandlung zu wenig Na2CO3 gespalten und zu wenig NaOH gebildet wird oder aber die gebildete Natronlauge bei der direkten Gaskühlung mit CO2 reagiert und wiederum Karbonatbildung erfolgt. Dadurch muß die benötigte NaOH über die Kaustifizierung von Na2CO3 gewonnen werden bzw. als make up NaOH zum Kraftprozeß zudosiert werden.All known methods for the thermal regeneration of black liquor to green liquor have the disadvantage that too little Na 2 CO 3 is split and too little NaOH is formed in the thermal treatment or the sodium hydroxide solution formed reacts with CO 2 in the direct gas cooling and again carbonate formation occurs. As a result, the required NaOH must be obtained by causticizing Na 2 CO 3 or added as makeup NaOH to the power process.

Der Erfindung liegt daher die Aufgabe zugrunde, die beim Kraftprozeß erforderliche Regenerierung der beim Holzaufschluß anfallenden alkalischen Flüssigkeit, als Black Liquor bezeichnet, verfahrenstechnisch und vorrichtungsgemäß so zu gestalten, daß weitgehend unabhängig von der Black- Liquor-Zusammensetzung ein Zielprodukt entsteht, das es erlaubt, die Produktionskapazität des Kraftprozesses zu erhöhen, die Emissionen zu senken und die Energie durch Erzeugung eines heizwertreichen Brenngases in Synthesegasqualität in höherer Qualität zu erhalten.The invention is therefore based on the object in the power process Required regeneration of the alkaline resulting from the wood digestion Liquid, known as black liquor, process engineering and to design according to the device so that largely independent of the black Liquor composition creates a target product that allows that Increase the production capacity of the power process, reduce emissions and the energy by generating a high-calorific fuel gas in Obtain syngas quality in higher quality.

Die Aufgabe wird durch die Merkmaie des ersten und des sechsten Patentanspruches gelöst. Weitere Ausgestaltung der Erfindung sind in den Unteransprüchen genannt.The task is characterized by the characteristics of the first and sixth Claim resolved. Further embodiments of the invention are in the Subclaims called.

Entsprechend Patentanspruch 1 geht das erfindungsgemäße Verfahren davon aus, daß zur Regeneration einer beim Kraftprozeß zum Aufschluß von Holz anfallenden Flüssigkeit, die neben hohen Konzentrationen an Natriumverbindungen beim Holzaufschluß extrahierte organische Verbindungen enthält, durch Vergasen in einem Flugstromreaktor bei Temperaturen oberhalb der Schmelztemperaturen der Natriumverbindungen und Abkühlung des Vergasungsgases durch Eindüsen einer kühlenden Flüssigkeit auf Temperaturen oberhalb oder unterhalb des Taupunktes und die Salzschmelze in ein Wasserbad tropft, das durch Zuführung von Kondensat oder Natriumverbindungen enthaltende Prozeßwässer gelöst und als regenerierte, von organischen Komponenten befreite Lösung als regeneriert dem Holzaufschluß wieder zugeführt wird. Das Verfahren ist dadurch gekennzeichnet, daß das im Vergasungsraum entstehende Vergasungsgas und die Salzschmelze getrennt abgeführt werden, wobei das Vergasungsgas in der Vorrichtung zur Abführung des Vergasungsgases durch Einspritzen von Wasser oder wäßriger Natriumsalzlösung über die Düsen abgekühlt wird und über die Abführleitung des Vergasungsgases zur weiteren Behandlung abströmt und die Salzschmelze über die Vorrichtung zur Abführung der Salzschmelze in ein Bad abläuft und gelöst wird und das Bad aus einer wäßrigen Lösung von Natriumhydroxid und Natriumsalzen besteht, wobei über Düsen Frischwasser oder geringer konzentrierte Natriumsalzlösungen zur Einstellung der gewünschten Konzentrationsverhältnisse zugeführt wird.According to claim 1, the method according to the invention is based on this from that for regeneration one in the process of strength to digest wood resulting liquid, which in addition to high concentrations Sodium compounds extracted from wood during organic extraction contains, by gasification in an entrained flow reactor at temperatures above the melting temperatures of the sodium compounds and cooling of the Gasification gas by injecting a cooling liquid at temperatures above or below the dew point and melt the salt in a water bath that drips by adding condensate or sodium compounds Process water containing dissolved and as regenerated, from organic Component-free solution as regenerated wood digestion again is fed. The method is characterized in that the The gasification gas produced and the salt melt separated  are discharged, the gasification gas in the device for discharge the gasification gas by injecting water or aqueous Sodium salt solution is cooled via the nozzles and via the discharge line of the Gasification gas flows out for further treatment and the salt melt over the device for removing the molten salt runs into a bath and is released and the bath from an aqueous solution of sodium hydroxide and sodium salts consists of fresh water or less concentrated via nozzles Sodium salt solutions for setting the desired concentration ratios is fed.

Vorteilhaft ist, daß durch die Wahl der Verbindung zwischen Reaktionsraumkontur und der Vorrichtung zur Abführung der Salzschmelze ein ringförmiges Salzschmelzbad entsteht, aus dem die Salzschmelze über die Abführvorrichtung in den Kühlraum und die Salzlösung abfließt.It is advantageous that the choice of the connection between the reaction chamber contour and the device for removing the molten salt an annular Salt melt bath arises from which the salt melt passes through the discharge device into the refrigerator and the saline solution drains away.

Weiterhin ist vorteilhaft, daß das Vergasungsgas über eine Vorrichtung zur Abführung des Vergasungsgases getrennt von der Salzschmelze seitlich aus dem Vergasungsraum abgeführt wird und die Salzschmelze aus einem Salzschmelzbad über die Vorrichtung in den Kühlraum und die Salzlösung abfließt.It is also advantageous that the gasification gas via a device for Removal of the gasification gas separately from the molten salt from the side Gasification chamber is discharged and the salt melt from one Salt melt bath via the device into the cold room and the salt solution drains away.

Weiterhin ist vorteilhaft, daß die Vorrichtung zur Abführung des Vergasungsgases mit einem äußeren Wasserfilm gekühlt und benetzt wird.It is also advantageous that the device for removing the gasification gas is cooled and wetted with an outer film of water.

Es ist von Vorteil, daß dem Bad der Salzlösung schwefelwasserstoffhaltige Gase aus fremdem Aufkommen oder aus der Entschwefelungsstufe des Vergasungsgases zugeführt werden. Schließlich ergeben sich bei unterschiedlichen Betriebsfällen und bei unterschiedlichen Schlackebildungsbedingungen dadurch besondere Vorteile, daß die Reaktionskontur zur äußeren Begrenzung des Vergasungsraumes aus einem feuerfesten Mauerwerk, aus einem gasdichten, gekühlten Rohrschirm im Sinne einer im Kesselbau üblichen Membranwand oder teils aus feuerfestem Mauerwerk und teils aus einem gekühlten Rohrschirm besteht.It is advantageous that the bath of saline gases containing hydrogen sulfide from foreign sources or from the desulphurization stage of the Gasification gas are supplied. Eventually arise at different operating cases and in different Slag formation conditions in particular advantages that the Reaction contour for the outer boundary of the gasification space from one fireproof masonry, from a gas-tight, cooled pipe umbrella in the sense a membrane wall common in boiler construction or partly made of fireproof masonry and partly consists of a cooled tubular umbrella.

Die Erfindung sei an nachfolgendem Ausführungsbeispiel unter Heranziehung schematischer Darstellungen näher erläutert. The invention is based on the following exemplary embodiment schematic representations explained in more detail.  

Die Figuren zeigen:The figures show:

Fig. 1: Flugstromvergaser mit getrennter Abführung des Vergasungsgases und der Schmelzschlacke, Fig. 1: entrained flow gasifier with separate removal of the gasification gas and the molten slag,

Fig. 2: Flugstromvergaser mit einer Vorrichtung zur Abführung der Salzschmelze, Fig. 2: entrained flow gasifier with a device for discharging the molten salt,

Fig. 3: Flugstromvergaser mit Vorrichtung zur seitlichen Abführung des Vergasungsgases, Fig. 3: entrained flow gasifier with a device for lateral removal of the gasification gas,

Fig. 4: Flugstromvergaser mit Reaktionsraumkontur, die als Membranwand ausgeführt ist. Fig. 4: entrained-flow gasifier with reaction chamber contour, which is designed as a membrane wall.

Die Fig. 1 zeigt einen Flugstromvergaser mit getrennter Abführung des Vergasungsgases und der Salzschmelze. Black Liquor und Sauerstoff als Vergasungsmittel werden am Kopf des Vergasungsreaktors 1 über spezielle Vergasungsbrenner zugeführt und in einer Flammenreaktion im Vergasungsraum 3 umgesetzt. Der Druck kann der späteren Verwertung des Vergasungsgases angepaßt werden und zwischen Umgebungsdruck und ca. 50 bar liegen. Ein gasdichter Druckmantel 2 ermöglicht dies. Während der Vergasungsreaktion in der Flamme werden die organischen Anteile des Black Liquor durch die partielle Oxidation mit Sauerstoff in typische Synthesegaskomponenten wie H2, CO, CO2 und H2O umgewandelt. Die Vergasungstemperaturen werden zwischen 850°C und 1400°C so ausgewählt, daß der Kohlenstoffumsatz des Black Liquor praktisch vollständig ist und die anorganischen Bestandteile als Salzschmelze an der inneren Reaktionsraumkontur 16 des Vergasungsraumes 3 nach unten ablaufen. Die Salzschmelze gelangt über die Vorrichtung 8 in den Kühlraum 5, wo sie durch Eindüsen von Wasser 9 oder aus dem Prozeß resultierenden Salzlösungen wie Green Liquor gekühlt und gelöst werden und sich im Bad 6 sammeln. Über den Stutzen 11 wird die Salzlösung zur weiteren Verwertung abgeführt. Durch den Stutzen 10 kann zusätzlich schwefelwasserstoffhaltiges Gas aus der Gasentschwefelungsstufe des Vergasungsgases oder aus fremdem aufkommen zugeführt werden, um den Sulfidgehalt der Salzlösung 6 in gewünschter Form zu erhöhen. Das Vergasungsgas wird über die Vorrichtung 4 aus dem Vergasungsraum 3 abgeleitet, durch Einspritzen von Kühlflüssigkeit, beispielsweise Wasser über die Düsen 7 gekühlt und über die Rohrleitung 12 zur weiteren Behandlung abgeführt. Die Vorrichtungen 4 und 12 zur Abführung des Vergasungsgases sind als Doppelmantel ausgeführt und mit Kühlwasser 13 gekühlt. Die frühzeitige Trennung von Vergasungsgas und Salzschmelze verhindert die Aufnahme von unerwünschtem Kohlendioxid durch die Salzlösung und die Desorption des gewünschten Schwefelwasserstoffs. Fig. 1 shows an entrained-flow gasifier with separate removal of the gasification gas and the molten salt. Black liquor and oxygen as the gasification agent are fed to the head of the gasification reactor 1 via special gasification burners and implemented in a flame reaction in the gasification chamber 3 . The pressure can be adapted to the later utilization of the gasification gas and can be between ambient pressure and approx. 50 bar. A gas-tight pressure jacket 2 makes this possible. During the gasification reaction in the flame, the organic components of the black liquor are converted into typical synthesis gas components such as H 2 , CO, CO 2 and H 2 O by partial oxidation with oxygen. The gasification temperatures are selected between 850 ° C and 1400 ° C so that the carbon conversion of the black liquor is practically complete and the inorganic constituents run down as a salt melt on the inner reaction chamber contour 16 of the gasification chamber 3 . The molten salt passes through the device 8 into the cooling space 5 , where it is cooled and dissolved by injecting water 9 or salt solutions such as green liquor resulting from the process and collecting in the bath 6 . The saline solution is discharged via the nozzle 11 for further use. Through the nozzle 10 , hydrogen sulfide-containing gas can also be supplied from the gas desulfurization stage of the gasification gas or from foreign sources in order to increase the sulfide content of the salt solution 6 in the desired form. The gasification gas is discharged from the gasification chamber 3 via the device 4 , cooled by injecting cooling liquid, for example water via the nozzles 7, and discharged via the pipeline 12 for further treatment. The devices 4 and 12 for removing the gasification gas are designed as double jackets and cooled with cooling water 13 . The early separation of gasification gas and molten salt prevents the absorption of unwanted carbon dioxide by the salt solution and the desorption of the desired hydrogen sulfide.

Fig. 2 zeigt eine besonders vorteilhafte Ausgestaltung der Vorrichtung zur Abführung der Salzschmelze 8 durch Schaffung eines Salzschmelzbades 14 aus dem die Salzschmelze in den Kühlraum 5 überläuft. Fig. 2 shows a particularly advantageous embodiment of the device for discharging the molten salt 8 by providing a molten salt bath 14 from spilling the salt melt into the cooling chamber 5.

Fig. 3 zeigt die vorteilhafte Möglichkeit, das Vergasungsgas über die Vorrichtung 4 seitlich aus dem Vergasungsraum 3 abzuführen. Die Salzschmelze wird aus dem Schmelzbad 14 über eine zentrale Abführvorrichtung 8 in den Kühlraum 5 geführt Fig. 3 shows the advantageous possibility of the gasification gas via the discharge device 4 out of the gasification chamber 3 side. The molten salt is fed out of the molten bath 14 into the cooling space 5 via a central discharge device 8

Fig. 4 zeigt die Reaktionsraumkontur 16 als eine im Kesselbau übliche Membranwand gestaltet. Die Membranwand besteht aus einem gasdicht verschweißten Rohrschirm, dessen Kühlrohre wasserdurchflossen sind und damit auf Temperaturen zwischen 200-250°C gekühlt werden. Fig. 4 shows the reaction space contour 16 designed as a membrane wall customary in boiler construction. The membrane wall consists of a gas-tight welded tubular screen, the cooling tubes of which are flooded with water and thus cooled to temperatures between 200-250 ° C.

BezugszeichenlisteReference list

11

Vergasungsreaktor
Gasification reactor

22nd

Druckmantel
Pressure jacket

33rd

Vergasungsraum
Gasification room

44th

Vorrichtung zur Abführung des Vergasungsgases
Device for removing the gasification gas

55

Kühlraum
Cold room

66

Bad zur Salzlösung
Bath to the saline solution

77

Einspritzdüsen zur Kühlung des Vergasungsgases
Injection nozzles for cooling the gasification gas

88th

Vorrichtung zur Abführung der Salzschmelze
Device for removing the molten salt

99

Einspritzdüsen zur Kühlung und Lösung der Salzschmelze
Injection nozzles for cooling and dissolving the salt melt

1010th

Zuführung schwefelwasserstoffhaltiger Gase
Supply of gases containing hydrogen sulfide

1111

Abführung der wäßrigen Lösung von Natriumhydroxid und Natriumsalzen
Removal of the aqueous solution of sodium hydroxide and sodium salts

1212th

Abführleitung des Vergasungsgases
The gasification gas discharge line

1313

Kühlwasserzuführung
Cooling water supply

1414

Salzschmelzbad
Melting salt bath

1515

Zuführung von Wasser oder Natriumsalzlösung
Add water or sodium salt solution

1616

Reaktionsraumkontur
Reaction space contour

1717th

Wasserfilm
Water film

Claims (10)

1. Verfahren zur Regeneration einer beim Kraftprozeß zum Aufschluß von Holz anfallenden Flüssigkeit, die neben hohen Konzentrationen an Natriumverbindungen beim Holzaufschluß extrahierte organische Verbindungen enthält, durch Vergasen in einem Flugstromreaktor bei Temperaturen oberhalb der Schmelztemperaturen der Natriumverbindungen und Abkühlung des Vergasungsgases durch Eindüsen einer kühlenden Flüssigkeit auf Temperaturen oberhalb oder unterhalb des Taupunktes und die Salzschmelze in ein Wasserbad tropft, das durch Zuführung von Kondensat oder Natriumverbindungen enthaltende Prozeßwässer gelöst und als regenerierte, von organischen Komponenten befreite Lösung als regeneriert dem Holzaufschluß wieder zugeführt wird, dadurch gekennzeichnet, daß im Vergasungsraum entstehendes Vergasungsgas und die Salzschmelze getrennt abgeführt werden, wobei das Vergasungsgas in einer Vorrichtung zur Abführung von Vergasungsgas durch Einspritzen von Wasser oder wäßriger Natriumsalzlösung über Düsen abgekühlt wird und über eine Abführleitung des Vergasungsgases zur weiteren Behandlung abströmt und die Salzschmelze über eine Vorrichtung zur Abführung der Salzschmelze in ein Bad abläuft und gelöst wird und das Bad aus einer wäßrigen Lösung von Natriumhydroxid und Natriumsalzen besteht, wobei über Düsen Frischwasser oder geringer konzentrierte Natriumsalzlösungen zur Einstellung der gewünschten Konzentrationsverhältnisse zugeführt wird.1. A process for the regeneration of a liquid obtained in the power process for the digestion of wood, which contains, in addition to high concentrations of sodium compounds, organic compounds extracted during the wood digestion, by gasification in an entrained flow reactor at temperatures above the melting temperature of the sodium compounds and cooling of the gasification gas by injecting a cooling liquid Temperatures above or below the dew point and the molten salt drips into a water bath, which is dissolved by supplying process water containing condensate or sodium compounds and fed back to the wood digestion as a regenerated solution freed from organic components, characterized in that gasification gas and the molten salt are removed separately, the gasification gas in a device for removing gasification gas by injecting water or aqueous sodium lz solution is cooled via nozzles and flows out through a discharge line of the gasification gas for further treatment and the molten salt runs through a device for discharging the molten salt into a bath and is dissolved and the bath consists of an aqueous solution of sodium hydroxide and sodium salts, fresh water or less concentrated sodium salt solutions to adjust the desired concentration ratios is supplied. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß durch die Wahl der Verbindung zwischen Reaktionsraumkontur und der Vorrichtung zur Abführung der Salzschmelze ein ringförmiges Salzschmelzbad entsteht, aus dem die Salzschmelze über die Abführvorrichtung in den Kühlraum und die Salzlösung abfließt,2. The method according to claim 1, characterized in that by the choice the connection between the reaction chamber contour and the device for Removing the molten salt creates an annular molten salt bath, from which the molten salt via the discharge device into the cold room and the saline solution drains away 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Vergasungsgas über eine Vorrichtung zur Abführung des Vergasungsgases getrennt von der Salzschmelze seitlich aus dem Vergasungsraum abgeführt wird und die Salzschmelze aus einem Salzschmelzbad über die Vorrichtung in den Kühlraum und die Salzlösung abfließt.3. The method according to claim 1, characterized in that the Gasification gas via a device for discharging the gasification gas separated from the molten salt from the side of the gasification chamber  is discharged and the molten salt from a molten salt bath over the Device into the refrigerator and the saline solution drains away. 4. Verfahren nach den Ansprüchen 1 bis 3, dadurch gekennzeichnet, daß die Vorrichtung zur Abführung des Vergasungsgases mit einem äußeren Wasserfilm gekühlt und benetzt wird.4. The method according to claims 1 to 3, characterized in that the Device for discharging the gasification gas with an external Water film is cooled and wetted. 5. Verfahren nach den Ansprüchen 1 bis 4, dadurch gekennzeichnet, daß dem Bad der Salzlösung schwefelwasserstoffhaltige Gase aus fremdem Aufkommen oder aus der Entschwefelungsstufe des Vergasungsgases zugeführt werden.5. The method according to claims 1 to 4, characterized in that the bath of the salt solution gases containing hydrogen sulfide from foreign Emergence or from the desulfurization stage of the gasification gas be fed. 6. Vorrichtung zur Durchführung eines Verfahrens nach Anspruch 1, dadurch gekennzeichnet, daß
  • - im Vergasungsraum (3) Aggregate (4, 8) zur Trennung von Vergasungsgas und Salzschmelze angeordnet sind,
  • - wobei Einspritzdüsen (7) zur Abkühlung des Vergasungsgases in der Vorrichtung (4) zur Abführung des Vergasungsgases,
  • - Düsen (9) zur Kühlung und Lösung der Salzschmelze im Kühlraum (5) des Vergasers,
  • - ein Bad (6) zur Lösung des Salzes unterhalb des Vergasungsraumes (3)
  • - und eine Abführleitung (12) für das Vergasungsgas angeordnet sind.
6. Apparatus for performing a method according to claim 1, characterized in that
  • - Units ( 4 , 8 ) for separating gasification gas and molten salt are arranged in the gasification chamber ( 3 ),
  • - Injection nozzles ( 7 ) for cooling the gasification gas in the device ( 4 ) for discharging the gasification gas,
  • - nozzles ( 9 ) for cooling and dissolving the salt melt in the cooling chamber ( 5 ) of the carburetor,
  • - a bath ( 6 ) for dissolving the salt below the gasification chamber ( 3 )
  • - And a discharge line ( 12 ) for the gasification gas are arranged.
7. Vorrichtung nach Anspruch 6, dadurch gekennzeichnet, daß die Verbindung zwischen Reaktionsraumkontur (16) und der Vorrichtung zur Abführung der Salzschmelze (8) so angeordnet wird, daß ein ringförmiges Salzschmelzbad (14) entsteht, aus dem die Salzschmelze über die Abführvorrichtung (8) in den Kühlraum (5) und die Salzlösung (6) abfließt.7. The device according to claim 6, characterized in that the connection between the reaction chamber contour ( 16 ) and the device for removing the molten salt ( 8 ) is arranged so that an annular molten salt bath ( 14 ) is formed, from which the molten salt via the discharge device ( 8 ) flows into the refrigerator ( 5 ) and the salt solution ( 6 ). 8. Vorrichtung nach Anspruch 6, dadurch gekennzeichnet, daß die Vorrichtung (4) zur Abführung des Vergasungsgases seitlich aus dem Vergasungsraum (3) herausführt,8. The device according to claim 6, characterized in that the device ( 4 ) for removing the gasification gas leads laterally out of the gasification chamber ( 3 ), 9. Vorrichtung nach den Ansprüchen 6 bis 8, dadurch gekennzeichnet, daß die Vorrichtung zur Abführung des Vergasungsgases (4) mit einem äußeren Wasserfilm (17) versehen ist. 9. Device according to claims 6 to 8, characterized in that the device for removing the gasification gas ( 4 ) is provided with an outer water film ( 17 ). 10. Vorrichtung nach den Ansprüchen 6 bis 8, dadurch gekennzeichnet, daß die Reaktionsraumkontur (16) zur äußeren Begrenzung des Vergasungsraumes (3) aus einem feuerfesten Mauerwerk, aus einem gasdichten, gekühlten Rohrschirm im Sinne einer im Kesselbau üblichen Membranwand oder teils aus feuerfestem Mauerwerk und teils aus einem gekühlten Rohrschirm besteht.10. Device according to claims 6 to 8, characterized in that the reaction chamber contour ( 16 ) for the outer boundary of the gasification chamber ( 3 ) made of fireproof masonry, from a gas-tight, cooled tubular screen in the sense of a membrane wall common in boiler construction or partially made of fireproof masonry and partly consists of a cooled tubular umbrella.
DE1997118131 1997-04-29 1997-04-29 Method and device for the regeneration of a liquid obtained in the power process for the digestion of wood by gasification Expired - Lifetime DE19718131C2 (en)

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