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DE4129566A1 - Absorption of hydrogen sulphide from waste contg. carbon di:sulphide from viscose prodn. - in sodium hydroxide soln. contg. silicone oil or paraffin or alcohol - Google Patents

Absorption of hydrogen sulphide from waste contg. carbon di:sulphide from viscose prodn. - in sodium hydroxide soln. contg. silicone oil or paraffin or alcohol

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Publication number
DE4129566A1
DE4129566A1 DE19914129566 DE4129566A DE4129566A1 DE 4129566 A1 DE4129566 A1 DE 4129566A1 DE 19914129566 DE19914129566 DE 19914129566 DE 4129566 A DE4129566 A DE 4129566A DE 4129566 A1 DE4129566 A1 DE 4129566A1
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DE
Germany
Prior art keywords
contg
absorption
soln
sulphide
sodium hydroxide
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Withdrawn
Application number
DE19914129566
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German (de)
Inventor
Klaus Burkhardt
Wolfgang Schmidt
Walter Hartwich
Birgit Mooz
Roland Dr Sperhacke
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THUERINGISCHE FASER AG SCHWARZ
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THUERINGISCHE FASER AG SCHWARZ
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Priority to DE19914129566 priority Critical patent/DE4129566A1/en
Publication of DE4129566A1 publication Critical patent/DE4129566A1/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • B01D53/48—Sulfur compounds
    • B01D53/52—Hydrogen sulfide
    • 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
    • B01D53/48—Sulfur compounds
    • B01D53/485—Sulfur compounds containing only one sulfur compound other than sulfur oxides or hydrogen sulfide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C01B17/32—Hydrosulfides of sodium or potassium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)

Abstract

Spray columns are used as absorber and NaOH soln. as absorbent, with recovery of Na2S and/or NaHs soln., 0.0001-0.004 wt.%, w.r.t. the NaOH soln., of silicone oils and/or paraffins and/or alcohols are added to the absorption system. ADVANTAGE - Absorption effect is high, and there is negligible residual content (0.3%) of H2S, even with a high initial concn. (2000-3000 mg/cubic m). High quality solns. of Na2S and/or NaHS, with only small amts. of Na2S2O3, are obtd. In an example, 150 kg/h of H2S was led with a waste air stream of 50,000 cubic m/h into an absorber fed with 1500 1/h or NaOH (200 g/l of NaOH and 40 g/l of hemicellulose), giving conversion to a soln. contg. 120 g/l of Na2S and 40 g/l of NaHS. The amt. of Na2S2O3 formed was 28.5 g/l. During 24 h, 2 x 100 ml of polyalkylene glycol was added discontinuously, when the formation of Na2S2O3 fell to 7.5 g/l. The content of residual H2S was 0.3-0.1 wt.%, compared with an initial value of 1 wt.

Description

Die Erfindung betrifft die Absorption von Schwefel­ wasserstoff aus Natronlauge bei der Reinigung von schwefelwasserstoff- und schwefelkohlenstoffhaltigen Abgasen der Produktion von Viskoseerzeugnissen.The invention relates to the absorption of sulfur hydrogen from caustic soda when cleaning containing hydrogen sulfide and carbon disulphide Exhausting the production of viscose products.

Es ist bekannt, daß Schwefelwasserstoff aus Abgasen mittels Natronlauge als Absorptionsmittel in unter­ schiedlichen technischen Anlagen gebunden wird. Durch solche Absorptionsanlagen werden Restgehalte an Schwefelwasserstoff von ca. 20 mg/m3, das heißt ca. 1%, im Abgas erreicht.It is known that hydrogen sulfide is bound from exhaust gases using sodium hydroxide solution as an absorbent in various technical systems. Such absorption systems achieve residual levels of hydrogen sulfide of approximately 20 mg / m 3 , that is to say approximately 1%, in the exhaust gas.

Bei der üblichen Lauge-Naßwäsche wird durch Sprüh­ kolonnen und Natronlauge als Absorptionsmittel bei Schwefelwasserstoff-Eingangskonzentrationen von ca. 1000 mg/m3 eine Absorptionsleistung von ca. 97% erzielt.In the usual alkali wet scrubbing, an absorption rate of about 97% is achieved by spraying columns and sodium hydroxide solution as an absorbent at hydrogen sulfide input concentrations of about 1000 mg / m 3 .

In Abluftreinigungsanlagen für Gase aus der Viskose­ faserproduktion bedeutet eine unvollkommene Absorp­ tionswirkung gegenüber Schwefelwasserstoff eine Be­ lastung der nachgeschalteten Adsorptionsanlagen, wo der noch im Gas enthaltene Schwefelkohlenstoff an Aktivkohle adsorbiert wird. Zusätzlich anwesender Schwefelwasserstoff führt unerwünscht zu verstärkter Bildung von Schwefel und Schwefelsäure auf der Aktiv­ kohle, welche in kürzeren Intervallen entfernt werden müssen und das Abwassersystem belasten. In exhaust air purification systems for gases from viscose fiber production means an imperfect absorption action against hydrogen sulfide a Be load of the downstream adsorption systems, where the carbon disulphide still contained in the gas Activated carbon is adsorbed. Additionally present Hydrogen sulfide undesirably leads to increased Formation of sulfur and sulfuric acid on the active coal, which are removed at shorter intervals need and pollute the sewage system.  

Außer Schwefelwasserstoff enthält das Abgas von Vis­ koseanlagen noch Schwefelkohlenstoff, Luftsauerstoff und Kohlendioxid, wodurch es zur Bildung von uner­ wünschten Nebenprodukten wie Natriumthiosulfat und Natriumcarbonat kommt.In addition to hydrogen sulfide, the Vis exhaust gas contains koseanlagen still carbon disulphide, atmospheric oxygen and carbon dioxide, which leads to the formation of imm wanted by-products such as sodium thiosulfate and Sodium carbonate is coming.

(VDI-Richtlinie Nr. 3452, März 1977, Düsseldorf; "Ver­ fahren zur Viskoseabgasreinigung" Lenzinger Berichte, Heft 59, S. 80; "Abluftreinigung" LURGI-Schnellinfor­ mation, Werbematerial).(VDI Guideline No. 3452, March 1977, Düsseldorf; "Ver drive to viscous exhaust gas purification "Lenzinger reports, Issue 59, p. 80; "Exhaust air purification" LURGI quick information mation, advertising material).

Natriumthiosulfat bildet sich in Größenordnungen von 20-30 g/l in der Sulfidlauge.Sodium thiosulfate forms in the order of magnitude 20-30 g / l in the sulfide solution.

Die bei der Absorption von Schwefelwasserstoff zu Natronlauge anfallende Natriumsulfidlauge mit den Haupt­ bestandteilen Natriumsulfid und möglicherweise Natrium­ hydrogensulfid wird vorzugsweise in der Papierindustrie beim Kochen des Zellstoffes nach dem Sulfatverfahren zur Einstellung der Sulfidität eingesetzt. Dabei führen hohe Bestandteile an Natriumthiosulfat größer als 10 g/l zu einer verstärkten Korrosion der Anlage, wo­ durch der Einsatz einer solchen Natriumsulfidlauge nur bedingt, unter Zumischung geringer Anteile, möglich ist. ("Zu Einfluß Thiosulfat auf Korrosion", Müller, W. A., Internationales Seminar Pulp Paper Ind., Corrosion Problemes, Chicago 1974; "Mechanismus und Verhütung der Korrosion von Stählen, die Kraftzellstofflaugen aus­ gesetzt sind")Which increases in the absorption of hydrogen sulfide Sodium hydroxide solution with the main ingredients sodium sulfide and possibly sodium Hydrogen sulfide is preferred in the paper industry when the pulp is boiled using the sulfate process used to adjust the sulfidity. Do this high levels of sodium thiosulfate greater than 10 g / l to an increased corrosion of the system, where by using such a sodium sulfide solution only conditionally, with the addition of small portions, is possible. ("Influence of thiosulfate on corrosion", Müller, W. A., International Pulp Paper Ind. Seminar, Corrosion Problemes, Chicago 1974; "Mechanism and prevention the corrosion of steels made from kraft pulp are set ")

Es sind Verfahren zur Entfernung von Schwefelwasser­ stoff aus Gasgemischen durch alkalische Wäschen bekannt, bei denen jedoch durch Zusatz von Oxidationsmitteln der Schwefelwasserstoff zu elementarem Schwefel umgesetzt wird (DE-OS 32 16 161, DE-OS 32 19 782). Bei der an­ schließenden Regenerierung der hierbei verwendeten Waschmittel wird Sauerstoffhaltiges Gas zur Rückoxydation des Oxydationsmittels eingesetzt. They are procedures for removing sulfur water known from gas mixtures by alkaline washes, in which, however, by the addition of oxidizing agents Hydrogen sulfide converted to elemental sulfur is (DE-OS 32 16 161, DE-OS 32 19 782). At the at closing regeneration of the used here Detergent becomes oxygen-containing gas for re-oxidation of the oxidizing agent used.  

Diese Lösung ist nicht anwendbar, wenn die zur Gas­ wäsche verwendete Lauge in anderen Produktionsanlagen verwertet werden soll.This solution is not applicable when going to gas laundry used lye in other production facilities should be recycled.

Es ist auch bekannt, daß in einem Absorptionsverfahren zur Entfernung von Schwefelwasserstoff aus Gasgemischen, insbesondere höhere Alkohole und modifizierte Silikone eingesetzt werden. Bei diesem Verfahren werden als Waschlösung Amine eingesetzt, die beim Kontakt mit sau­ ren Gasen schwere, sauerstoffhaltige Verbindungen bil­ den (DE-OS 30 21 921). Eine Weiterverarbeitung der Waschlösung in anderen Produktionsanlagen ist auch hier nicht gegeben.It is also known that in an absorption process to remove hydrogen sulfide from gas mixtures, especially higher alcohols and modified silicones be used. In this procedure, as Washing solution used amines, which when in contact with sau heavy gases, oxygen-containing compounds bil the (DE-OS 30 21 921). A further processing of the Washing solution in other production facilities is too not given here.

Der im Patentanspruch angegebenen Erfindung liegt das Problem zugrunde, unter Anwendung der Lauge-Naßwäsche, bei der Absorption von Schwefelwasserstoff aus Abgasen der Viskoseproduktion mittels Natronlauge ein Verfahren zu finden, welches eine sehr hohe Absorptionswirkung mit nur unwesentlichem Restgehalt an Schwefelwasser­ stoff aufweist, bei gleichzeitiger Gewinnung von Natrium­ sulfidlauge und/oder Natriumhydrogensulfidlauge gleich­ mäßig hoher Qualität mit nur geringem Anteil an Natrium­ thiosulfat.The invention specified in the claim is Underlying problem, using the alkali wet wash, in the absorption of hydrogen sulfide from exhaust gases a process for the production of viscose using sodium hydroxide solution to find which has a very high absorption effect with only an insignificant residual sulfur water content Has substance with simultaneous extraction of sodium sulfide liquor and / or sodium hydrogen sulfide liquor the same moderately high quality with only a small amount of sodium thiosulfate.

Erfindungsgemäß werden bei der Anwendung von Sprüh­ kolonnen als Absorber und Natronlauge als Absorptions­ mittel dem Absorptionssystem Silikonöle und/oder Paraffine und/oder Alkohole in Mengen von 0,0001 bis 0,004 Masse­ anteile in %, bezogen auf das Absorptionsmittel Natron­ lauge, zugegeben.According to the invention when using spray columns as absorbers and caustic soda as absorption by means of the silicone oils and / or paraffins absorption system and / or alcohols in amounts of 0.0001 to 0.004 mass proportions in%, based on the absorbent sodium lye, admitted.

Dabei kann die Natronlauge Anteile an Hemicellulose ent­ halten. The sodium hydroxide solution may contain some hemicellulose hold.  

Mit der erfindungsgemäßen Zugabe eines oder mehrerer der aufgeführten Stoffe als Kombination wird die Leistungsfähigkeit der Absorberanlage derartig erhöht, daß aus den schwefelwasserstoff- und schwefelkohlen­ stoffhaltigen Abgasen der Viskoseproduktion der Schwefelwasserstoff durch das Absorptionsmittel Natron­ lauge annähernd vollständig ausgewaschen wird.With the addition of one or more according to the invention of the substances listed as a combination Performance of the absorber system increased in such a way that from the hydrogen sulfide and carbon disulphide exhaust gases from the production of viscose Hydrogen sulfide through the absorbent sodium lye is almost completely washed out.

Gleichzeitig wird eine Senkung des unerwünschten Na­ triumthiosulfatgehaltes in der entstehenden Natrium­ sulfidlauge und damit eine günstige Weiterverarbeit­ barkeit in gleichmäßig guter Qualität erreicht. Die entscheidende Erhöhung der Absorptionsleistung bezüglich Schwefelwasserstoff wird durch dieses Absorp­ tionsverfahren selbst bei sehr hohen Eingangskonzentra­ tionen von 2000-3000 mg/m3 mit dem Gewährleisten gleich­ bleibend geringem Restanteile von ca. 0,3% deutlich.At the same time, a reduction in the undesirable sodium thiosulfate content in the sodium sulfide liquor formed and thus a favorable further processing ability in uniformly good quality is achieved. The decisive increase in the absorption capacity with regard to hydrogen sulfide becomes clear through this absorption process even at very high input concentrations of 2000-3000 mg / m 3 with the guarantee of a consistently low residual content of approx. 0.3%.

Die Erfindung soll an einem Ausführungsbeispiel er­ läutert werden.The invention is based on an exemplary embodiment to be refined.

AusführungsbeispielEmbodiment

In einem Absorber, der als Düsenwäscher ausgebildet ist, werden mit einem Abluftstrom von 50 000 m3/h i.N. stünd­ lich 150 kg Schwefelwasserstoff eingeleitet, der mit 1500 l/h Natronlauge einer Konzentration von 200 g/l NaOH und 40 g/l Hemicellulosegehalt absorbiert und zu einer Sulfidlauge der Konzentration von 120 g/l Natriumsulfid und 40 g/l Natriumhydrogensulfid umgesetzt wird. Der gebildete Anteil Natriumcarbonat beträgt 28,5 g/l.In an absorber, which is designed as a nozzle scrubber, 150 kg of hydrogen sulfide are introduced per hour with an exhaust air flow of 50,000 m 3 / h iN, containing 1500 l / h sodium hydroxide solution at a concentration of 200 g / l NaOH and 40 g / l hemicellulose content is absorbed and converted to a sulfide solution with a concentration of 120 g / l sodium sulfide and 40 g / l sodium hydrogen sulfide. The proportion of sodium carbonate formed is 28.5 g / l.

Der Absorber ist als zweistufiger Apparat mit Sprüh­ kreisläufen ausgebildet. The absorber is a two-stage device with spray circuits trained.  

Der Absorptionslauge wird in 24 Stunden 2 · 100 ml Polyalkylenglykol diskontinuierlich zugegeben. Durch diese Zugabe reduziert sich der Restgehalt des Schwefelwasserstoffes von anfangs ca. 1,0 Masse-%, bezogen auf die Eingangsmenge, auf 0,3 bis 0,1 Masse-%; die Bildung von Natriumthiosulfat geht von 28,0 g/l auf 7,5 g/l in der Sulfidlauge zurück.The absorption liquor becomes 2 x 100 ml in 24 hours Polyalkylene glycol added discontinuously. This addition reduces the residual content of the hydrogen sulfide initially approx. 1.0% by mass, based on the input quantity, 0.3 to 0.1 mass%; the formation of sodium thiosulfate goes from 28.0 g / l to 7.5 g / l in the sulfide liquor.

Dabei sinkt die Belastung der nachgeschalteten Ad­ sorptionsstufe für CS2 mittels Aktivkohle durch Schwefel- bzw. Schwefelsäure, indem sich der Anfall Schwefelwasserstoff durch verbesserte Absorption von ca. 1,5 kg/h auf 0,5 kg/h bis ca. 0,15 kg/h reduziert. Dies führt zu einer im gleichen Verhältnis verlänger­ ten Standzeit der Aktivkohle in den Adsorbern bis zur notwendigen Entfernung von Schwefelsäure und Schwefel sowie einer Verlängerung der absoluten Standzeit der Kohle durch geringeren Verschleiß.The load on the downstream adsorption stage for CS 2 by means of activated carbon is reduced by sulfuric or sulfuric acid, since the hydrogen sulfide accumulates through improved absorption from approx. 1.5 kg / h to 0.5 kg / h to approx. 0.15 kg / h reduced. This leads to a prolonged service life of the activated carbon in the adsorbers in the same ratio until the necessary removal of sulfuric acid and sulfur as well as an increase in the absolute service life of the coal due to less wear.

Im zurückgewonnenen Schwefelkohlenstoff der Adsorp­ tionsanlage reduziert sich der Restgehalt an Schwefel­ wasserstoff von 7,5 mg/kg auf 2 mg/kg. Die entstehende Natriumsulfidlauge weist eine gleichmäßig gute Qualität auf und wird in der Zellstoffindustrie zum Holzauf­ schluß im Kochprozeß eingesetzt ohne Überschreitung des zulässigen Wertes für Natriumthiosulfat.In the recovered carbon disulfide the adsorp the residual sulfur content is reduced hydrogen from 7.5 mg / kg to 2 mg / kg. The emerging Sodium sulfide lye has an equally good quality and turns into wood in the pulp industry finally used in the cooking process without exceeding the permissible value for sodium thiosulfate.

Claims (1)

Absorption von Schwefelwasserstoff aus schwefelkohlen­ stoff- und schwefelwasserstoffhaltigen Abgasen der Produktion von Viskoseerzeugnissen nach dem Lauge­ Naßwäsche-Verfahren bei Anwendung von Sprühkolonnen als Absorber und Natronlauge als Absorptionsmittel und Gewinnung von Natriumsulfidlauge und/oder Natrium­ hydrogensulfidlauge, gekennzeichnet dadurch, daß dem Absorptionssystem Silikonöle und/oder Paraffine und/oder Alkohole in Mengen von 0,0001-0,004 Masseanteile in %, bezogen auf Natronlauge, zugegeben werden.Absorption of hydrogen sulfide from carbon disulphide exhaust gases containing hydrogen sulfide and Production of viscose products after the lye Wet washing process using spray columns as absorber and sodium hydroxide solution as absorbent and Obtaining sodium sulfide liquor and / or sodium Hydrogen sulfide lye, characterized in that the Absorption system silicone oils and / or paraffins and / or Alcohols in amounts of 0.0001-0.004 parts by mass in%, based on sodium hydroxide solution, are added.
DE19914129566 1991-09-06 1991-09-06 Absorption of hydrogen sulphide from waste contg. carbon di:sulphide from viscose prodn. - in sodium hydroxide soln. contg. silicone oil or paraffin or alcohol Withdrawn DE4129566A1 (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT400530B (en) * 1994-04-06 1996-01-25 Austria Metall METHOD FOR PURIFYING OVEN EXHAUST GASES
WO1998052680A1 (en) * 1997-05-21 1998-11-26 Turbotak Technologies Inc. Removal of contaminants from gas streams in rayon production
DE19603837C2 (en) * 1996-02-05 2002-06-13 Rag Ag Process for H2S deposition from a gas containing H2S, e.g. B. coke oven gas, and device for performing the method
DE102004025224A1 (en) * 2004-05-21 2005-12-15 Gesellschaft zur Förderung von Medizin-, Bio- und Umwelttechnologie e.V. Quantitative dermination of hydrogen sulfide in gases, e.g. for monitoring waste gases, using flow system with biosensor comprising sulfur-oxidizing bacteria immobilized on oxygen sensor and/or pH sensor
CN114082277A (en) * 2021-12-03 2022-02-25 湖北润驰环保科技有限公司 Process for fine desulfurization and purification of waste lubricating oil hydrogenation tail gas

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JPH03159905A (en) * 1989-11-17 1991-07-09 Jgc Corp Production of sodium hydrosulfide and production equipment

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT400530B (en) * 1994-04-06 1996-01-25 Austria Metall METHOD FOR PURIFYING OVEN EXHAUST GASES
DE19603837C2 (en) * 1996-02-05 2002-06-13 Rag Ag Process for H2S deposition from a gas containing H2S, e.g. B. coke oven gas, and device for performing the method
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US6416725B1 (en) 1997-05-21 2002-07-09 Turbotak Technologies Inc. Removal of contaminants from gas streams in rayon production
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