DE2205796A1 - Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate - Google Patents

Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate

Info

Publication number
DE2205796A1
DE2205796A1 DE19722205796 DE2205796A DE2205796A1 DE 2205796 A1 DE2205796 A1 DE 2205796A1 DE 19722205796 DE19722205796 DE 19722205796 DE 2205796 A DE2205796 A DE 2205796A DE 2205796 A1 DE2205796 A1 DE 2205796A1
Authority
DE
Germany
Prior art keywords
sulfur
solvent
arsenic
processing method
hydrogen sulphide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
DE19722205796
Other languages
German (de)
Inventor
Guenter Dr Rer Nat Bracht
Fritz Goetza
Gustav Kloss
Horst Kurapkat
Guenter Dipl Chem Voigt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
RAG AG
Original Assignee
Ruhrkohle AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ruhrkohle AG filed Critical Ruhrkohle AG
Priority to DE19722205796 priority Critical patent/DE2205796A1/en
Priority to GB504374A priority patent/GB1387257A/en
Priority to GB990772A priority patent/GB1379624A/en
Priority to AU39801/72A priority patent/AU3980172A/en
Priority to AR24086872A priority patent/AR195165A1/en
Priority to FR7208447A priority patent/FR2128831B1/fr
Priority to BE780509A priority patent/BE780509A/en
Priority to SE310072A priority patent/SE366558B/xx
Priority to IT6778472A priority patent/IT960890B/en
Priority to US00259225A priority patent/US3777640A/en
Publication of DE2205796A1 publication Critical patent/DE2205796A1/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C10K1/105—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids containing metal compounds other than alkali- or earth-alkali carbonates, -hydroxides, oxides, or salts of inorganic acids derived from sulfur
    • C10K1/107—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids containing metal compounds other than alkali- or earth-alkali carbonates, -hydroxides, oxides, or salts of inorganic acids derived from sulfur containing As-, Sb-, Sn compounds
    • 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
    • C10K1/128—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 organic oxygen transferring compounds, e.g. sulfoxides

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Industrial Gases (AREA)

Abstract

Removal of H2S (and also NH3, HCN, org. cpds. such as benzene) from coking plant gases by washing the precooled, compressed gases with a solvent contg. As which catalyses reaction between NH3 and H2S to form ammonium polythionate, and then oxidising this to S, using another catalyst (e.g. cpds. of as, Sb, or Sn).

Description

"Aufbereitungsverfahren zur Entfernung von Schwefelwasserstoff und Ammoniak aus damit verunreinigten Gasen" 1. Zusatz zu Patent . ... ... (Patentanmeldung P 21 11 839.8) Die Erfindung betrifft ein Aufbereitungsverfahren, z.B. für Kokereigas, bei dem aus dem von dem Vorkühler kommenden, komprimiertem Rohgas, das Ammoniak, Schwefelwasserstoff, Oyan-Wasserstoff und organische Verbindungen aufweist, mit einen Lösungsmittel, da Arsen enthält, ausgewaschen wird und mit den dabei absorbierten Schwefel aus H2S und JE Ammoniumpolythionate gebildet werden, die unter Anwesenheit von wasserlöslichen Chinonderivaten oxydiert werden, worauf der elementare Schwefel aus dem Lösungsmittel entfernt wird, nach Patent . ... ..."Treatment process for the removal of hydrogen sulfide and Ammonia from gases contaminated with it "1. Addendum to patent. ... ... (patent application P 21 11 839.8) The invention relates to a processing method, e.g. for coke oven gas, in the case of the compressed raw gas coming from the pre-cooler, the ammonia, Has hydrogen sulfide, oyan hydrogen and organic compounds with a solvent, as it contains arsenic, is washed out and absorbed with the Sulfur from H2S and JE ammonium polythionate are formed in the presence are oxidized by water-soluble quinone derivatives, whereupon the elemental sulfur is removed from the solvent, according to patent. ... ...

(Patentanmeldung P 21 11 839.8).(Patent application P 21 11 839.8).

Dieses Verfahren ist Gegenstand des Hauptpatentes. Das Verfahren ist gegenüber den vorbekannten Verfahren wesentlich vereinfacht, weil eine Einstellung des Lösungsmittels auf einen bestimmten pH-Wert nicht erforderlich und der Temperaturbereich des Systems weitgehend unkritisch ist. Das Rohgas braucht weder aufgeheizt noch abgekühlt zu werden. Die Rohgastemperaturen können bei 10 bis 45° C liegen.This process is the subject of the main patent. The procedure is significantly simplified compared to the previously known method, because one setting of the solvent to a certain pH value is not required and the temperature range of the system is largely uncritical. The raw gas does not need to be heated up still to be cooled down. The raw gas temperatures can be between 10 and 45 ° C.

Es wurde nun gefunden, daß sich dieses Verfahren auf die Entfernung von Cyan und organisch gebundenem Schwefel aus dem Rohgas anwenden läßt, wobei der im Lösungsmittel physikalisch gelöste Cyan-Wasserstoff zu @@odanid umgesetzt und aus den organisch gebundenen Schwefeln wasserlösliche Sauerstoffverbindungen gebildet werden.It has now been found that this procedure affects the removal of cyan and organically bound sulfur can be applied from the raw gas, the Cyanohydrogen physically dissolved in the solvent is converted to @@ odanide and water-soluble oxygen compounds are formed from the organically bound sulfur will.

@isher wurden zur Entfernung von Cyan-Wasserstoff aus Gasen Verfahren verwendet, die mit Alkali, z.B. Ammonium-Polysulfid-Lösung als Waschlösung arbeiteten. Diese Verfahren sind jedoch verhältnismäßig kompliziert und dementsprechend kostspielig. Die @ntfexnung des organisch gebundenen Schwefels war bisher nur in ungenügendem Maße möglich.Previously, processes were used to remove cyanogen hydrogen from gases that worked with alkali, e.g. ammonium polysulphide solution, as a washing solution. However, these methods are relatively complex and accordingly costly. The discovery of the organically bound sulfur has so far only been inadequate Dimensions possible.

Es empfiehlt sich bei der Durchführung des erfindungsgemäßen Verfahrens im Oxydeur und in der Waschlösung eine Redoxpotentialdifferenz von 10 - 300 mV aufrechtzuerhalten.It is recommended when carrying out the method according to the invention to maintain a redox potential difference of 10-300 mV in the oxidizer and in the washing solution.

@ispielsweise wurde ein Kokereigas nach dem beschriebenen Verfahren behandelt, das 0,8 g Cyanwasser/Nm3 sowie 0,36 g organischen Schwefel/Nm3 enthielt. Der organisch gebundene Schwefel setzt sich etwa wie folgt zusammen: 60 Gew.-% CS2 20 Gew.-% COS 15 Gew.-% Th@kphen 5 Gew.-% Merkaptane Dieses Gas wurde bei etwa 30° C mit einer Waschlösung gewaschen, welche außer Arsen wasserlösliche Chinonderivate, nämlich z.B.For example, a coke oven gas was produced using the method described treated, which contained 0.8 g cyanide / Nm3 and 0.36 g organic sulfur / Nm3. The organically bound sulfur is made up roughly as follows: 60% by weight CS2 20% by weight COS 15% by weight Th @ kphen 5% by weight mercaptans This gas was at about 30 ° C washed with a washing solution which, in addition to arsenic, contains water-soluble quinone derivatives, namely e.g.

Hydrochinon oder Naphthochinon enthielt.Contained hydroquinone or naphthoquinone.

Dabei wurde ein Auswaschungsgrad fUr den Cyan-Wasserstoff erzielt, der bei 90 - 99% lag. Der organisch gebundene Schwefel wurde zu 30 - 60% umgesetzt.A degree of leaching was achieved for the cyano-hydrogen which was 90 - 99%. The organically bound sulfur was converted to 30-60%.

Die Lösung wurde anschließend in einem Oxydeur behallaelt. Dabei betrug die Potentialdifferens zwischen 10 - 300 mV.The solution was then treated in an Oxydeur. It was fraudulent the potential difference between 10 - 300 mV.

Der Schwefel wurde aus der Lösung flotiert, soweit er elementar abfiel.The sulfur was floated out of the solution as far as it fell elementally.

Der wesentliche, durch die Erfindung erzielbare Vorteil liegt in der weitgehenden Vereinfachung der Aufbereitung von insbesondere Kokereigasen bei der Entfernung von Schwefel und Cyan-Wasser aus den Rohgas.The main advantage that can be achieved by the invention lies in the extensive simplification of the treatment of coke oven gases in particular Removal of sulfur and cyan water from the raw gas.

PatentansprücheClaims

Claims (3)

P a t e n t a n s p r ü c h e 1. Aufbereitungsverfahren, z.B. für Kokereigas, bei dem aus dem von dem Vorkühler kommenden, komprimierten Rohgas, das Ammoni@k, Schwefelwasserstoff, Cyan-Wasserstoff und organische Verbindungen aufweist, mit einem Lösungsmittel, das Arsen enthält, ausgewaschen wird und mit dem dabei absorbierten Schwefel aus H2S und NH3 Ammoniumpolythionate gebildet werden, die unter enwesenheit von Wasserlöslischen Chinonderivaten oxydiert werden, worauf elementarer Schwefel aus demLösungsmittel entfernt wird, g e k e n n z e i c h -n e t d u r c h seine Anwendung Zur Entfernung von Oyan und organisch gebundenen Schwefel aus din Rohgas, wobei der im Lösungsmittel physikalisch gelöste Cyan-Wasserstoff zu Rhodanid umgesetzt und aus dem organisch gebundenen Schwefel wasserlöslisohe Sauerstoffverbindungen gebildet werden. P a t e n t a n s p r ü c h e 1. Processing method, e.g. for Coke oven gas, in the case of the compressed raw gas coming from the pre-cooler, the Contains ammonia, hydrogen sulfide, hydrogen cyanide and organic compounds, is washed out with a solvent that contains arsenic and with that absorbed sulfur are formed from H2S and NH3 ammonium polythionates, the are oxidized in the absence of water-soluble quinone derivatives, whereupon more elementary Sulfur is removed from the solvent c h its application To remove oyan and organically bound sulfur from din raw gas, with the cyanogen hydrogen physically dissolved in the solvent being added Rhodanide implemented and from the organically bound sulfur wasserlöslisohe oxygen compounds are formed. 2. Aufbereitungsverfahren nach Anspruch 1 , g e k e n n -s e 1 c h n e t d u r c h die Aufrechterhaltung einer Redospotentialdifferens von ca. 10 - 300 mV im Oxydeur.2. Processing method according to claim 1, g e k e n n -s e 1 c h n e t d u r c h the maintenance of a redo potential difference of approx. 10 - 300 mV in the Oxydeur. 3. Aufbereitungsverfahren nach Anspruch 1 , d a d u r c h g e k e n n X e i c h n e t , daß das Gas bei einer Temperatur der Waschlösung von ca. 300 a gewaschen wird.3. Processing method according to claim 1, d a d u r c h g e k e n n X e i c h n e t that the gas at a temperature of the washing solution of approx. 300 a is washed.
DE19722205796 1971-03-12 1972-02-08 Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate Pending DE2205796A1 (en)

Priority Applications (10)

Application Number Priority Date Filing Date Title
DE19722205796 DE2205796A1 (en) 1972-02-08 1972-02-08 Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate
GB504374A GB1387257A (en) 1971-03-12 1972-03-02 Separation process
GB990772A GB1379624A (en) 1971-03-12 1972-03-02 Separation process
AU39801/72A AU3980172A (en) 1971-09-10 1972-03-08 a PROCESS FORTHE REMOVAL OF HYDROGEN SULPHIDE AND AMMONIA FROM OTHER GASES
AR24086872A AR195165A1 (en) 1971-03-12 1972-03-09 TREATMENT PROCEDURE, FOR EXAMPLE OF COKE GASES
FR7208447A FR2128831B1 (en) 1971-03-12 1972-03-10
BE780509A BE780509A (en) 1971-03-12 1972-03-10 TREATMENT PROCESS FOR REMOVING SULPHYDRIC ACID AND AMMONIA FROM GASES WHICH ARE POLLUTED THEREOF
SE310072A SE366558B (en) 1971-03-12 1972-03-10
IT6778472A IT960890B (en) 1971-03-12 1972-03-11 PROCESS OF PROCESS TO ELIMINATE AMMONIA AND HYDROGEN SULFURATE FROM GAS WITH THEM COUNTING MINES
US00259225A US3777640A (en) 1971-06-24 1972-06-02 Remote indicator for diaphragm setting or the like

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19722205796 DE2205796A1 (en) 1972-02-08 1972-02-08 Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate

Publications (1)

Publication Number Publication Date
DE2205796A1 true DE2205796A1 (en) 1973-08-16

Family

ID=5835327

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19722205796 Pending DE2205796A1 (en) 1971-03-12 1972-02-08 Ammonia hydrogen sulphide removal from coking gases - by arsenic catalysed reaction to ammonium polythionate

Country Status (1)

Country Link
DE (1) DE2205796A1 (en)

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