EP0709116B1 - Procédé pour le traitement thermocatalytique des agents de combat chimiques - Google Patents

Procédé pour le traitement thermocatalytique des agents de combat chimiques Download PDF

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Publication number
EP0709116B1
EP0709116B1 EP95116796A EP95116796A EP0709116B1 EP 0709116 B1 EP0709116 B1 EP 0709116B1 EP 95116796 A EP95116796 A EP 95116796A EP 95116796 A EP95116796 A EP 95116796A EP 0709116 B1 EP0709116 B1 EP 0709116B1
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EP
European Patent Office
Prior art keywords
warfare agents
arsenic
gas
process according
reactor
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.)
Expired - Lifetime
Application number
EP95116796A
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German (de)
English (en)
Other versions
EP0709116A1 (fr
Inventor
Walter Dr. Katzung
Klaus Friedrich Dr.-Ing. Koehler
Manfred Prof. Dr. Gutmann
Heinrich Dr. Klare
Siegfried Prof. Dr. Nowak
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.)
SVEG STOFFVERWERTUNGS- UND ENTSORGUNGSGESELLSCHAFT
Original Assignee
SVEG Stoffverwertungs- und Entsorgungsgesellschaft mbH
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Publication of EP0709116A1 publication Critical patent/EP0709116A1/fr
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Classifications

    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
    • A62D3/37—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by reduction, e.g. hydrogenation
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/40—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by heating to effect chemical change, e.g. pyrolysis
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/02—Chemical warfare substances, e.g. cholinesterase inhibitors
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/04—Pesticides, e.g. insecticides, herbicides, fungicides or nematocides
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/22—Organic substances containing halogen
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/24—Organic substances containing heavy metals
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/26—Organic substances containing nitrogen or phosphorus
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2203/00—Aspects of processes for making harmful chemical substances harmless, or less harmful, by effecting chemical change in the substances
    • A62D2203/02—Combined processes involving two or more distinct steps covered by groups A62D3/10 - A62D3/40
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2203/00—Aspects of processes for making harmful chemical substances harmless, or less harmful, by effecting chemical change in the substances
    • A62D2203/10—Apparatus specially adapted for treating harmful chemical agents; Details thereof

Definitions

  • the invention relates to a thermal gas phase process for the complete processing of chemical warfare agents, their Additive and decomposition products.
  • DE-A-3940567 describes a process for thermal decomposition of warfare agents suggested the evaporation and decomposing the warfare agents as such or in a matrix through a succession of gas-heated fluid beds made of aluminum oxide particles causes a hydrogenation by the used Hydrogen should take place and a subsequent one Combustion of the gases is provided.
  • the present invention is based on the object a process for the complete reprocessing of chemical warfare agents provide without burning the warfare agents what is required is the remainder of the processing on landfill must be stored and before processing of the warfare agents a long transport of the warfare agents is necessary is.
  • the present invention enables destruction or processing of liquid and solid chemical warfare agents, from ammunition and storage containers, independently whether alone, as a liquid or solid mixture with each other or mixed with organic solvents or formulated in blowing and smoldering mixtures.
  • the warfare agents can also be connected to a flammable or non-flammable matrix be bound, e.g. B. when it comes to the rehabilitation of armaments and legacy of war goes.
  • the matrix can be a medium (e.g. a solution, soil or a material), a metallic Surface (e.g. a container or ammunition) or an additive his.
  • the chemical warfare agents are preferably halogen, sulfur, nitrogen, phosphorus or arsenic organic warfare agents, their addition and decomposition products, very preferably organic arsenic Warfare agents, including non-military arsenic compounds Origin should be understood to include an environmental impact runs out, such as Pesticides.
  • this gas is directly combined with a mixture of evaporated organic solvent and water vapor fed into the reactor and the thermal catalytic Refurbished, i.e. at a temperature of 500-1000 ° C, preferably 700-800 ° C under the catalysis of a calcium aluminate catalyst reductively implemented, resulting reaction gases burned or used as heating gas after any hydrides that may have formed, Halogen, ammonium, sulfur and phosphorus compounds as exhaust gases, Liquids or solids have been separated.
  • the reaction gases also become elementary solids Connections such as Arsenic, separated.
  • the exhaust gases to be separated from the reaction gases are preferably chlorine, bromine, fluorine, hydrogen sulfide or ammonia.
  • the pyrolyser can preferably be a rotary kiln, a combustion chamber be a radiation pipe with indirect heat coupling.
  • the Pyrolyser as well as the locks for the feed materials and the Pyrolysis residue with an inert gas, preferably nitrogen, argon or loaded with carbon dioxide. That is for every 10 liters of reaction space System charged with 1 to 5 liters.
  • inorganic residues in particular of arsenic, if present in the weapon
  • the warfare agents used may contain heavy metals.
  • This pyrolysis residue is for special systems for recovery of arsenic and metals smeltable.
  • the extractive treatment of the pyrolysis gases (step b)) and, if applicable, of the flying dust which occurs is carried out in an extractor with an organic solvent, preferably an aliphatic alcohol up to C 4 , a C 3 -C 5 ketone or an ester of a C 1 -C 4 -Carboxylic acid, very preferably with methanol, ethanol, propanol, methyl formate, ethyl formate, methyl acetate, ethyl acetate, methyl propionate, acetone or butanone.
  • organic solvent preferably an aliphatic alcohol up to C 4 , a C 3 -C 5 ketone or an ester of a C 1 -C 4 -Carboxylic acid, very preferably with methanol, ethanol, propanol, methyl formate, ethyl formate, methyl acetate, ethyl acetate, methyl propionate, acetone or butanone.
  • the solution from step b) or A) or one converted into the gas phase Warfare agent is at temperatures from 500 to 1000 ° C after the addition of Steam from a superheater is fed into a fixed bed reactor and there to the respective end products under the catalysis of a Calcium aluminate catalyst degraded.
  • the solvent-water vapor ratio is between 0.5 - 2: 1, preferably 1: 1 in the case of organic arsenic compounds as starting materials.
  • the resulting hydrogenating or hydro-splitting hydrogen leads depending on the starting materials for the formation of hydrogenated, or partially or non-hydrogenated End products such as hydrogen sulfide, ammonia, hydrogen halide and with elemental arsenic warfare agents Arsenic.
  • End products such as hydrogen sulfide, ammonia, hydrogen halide and with elemental arsenic warfare agents Arsenic.
  • the reaction temperatures above 700 ° C prevent this Formation of arsine.
  • catalysts based on calcium aluminate are used, preferably TZ 70 (alumina cement with 70% Al 2 O 3 ) and calcium aluminates with other aluminum oxide contents, such as 3 CaO * Al 2 O 3 (C 3 A).
  • the advantage of the method is that the reductive Gas phase medium, the regression of dioxins is excluded.
  • the water generated in the fixed bed reactor is circulated and supplemented or removed if necessary.
  • the residual exhaust gases contained in a gas-liquid separation are fed to a combustion upstream of the DENOX system.
  • the amount of gas generated is 1.4 m 3 per kg, for example when using methanol.
  • the gas has the composition of about 55% by volume of hydrogen, 10% by volume of carbon monoxide, 11.5% by volume of carbon dioxide, 11% of methane and a remainder of inert gas.
  • Pyrolysis residues containing arsenic from step a) or from step c) or B) arsenic can be smelted for recovery of inorganic arsenic compounds.
  • Figure 1 shows a schematic representation of a plant for disposal Arsenic warfare agents.
  • the pyrolyzer (1) consists of a radiation tube. He gets the Heat indirectly from the heat generator (2) by electrical or by gas heating.
  • the inert gas e.g. Nitrogen becomes direct from (3) fed.
  • the loading with solid arsenic-organic warfare agent e.g. Adamsite
  • Ignition and explosive charges are to be introduced.
  • In the Pyrolysers can also introduce liquid feedstocks via (5) become.
  • the pyrolysis residue is discharged through a lock into the line (6).
  • the pyrolysis gas passes through line (7) to a cyclone (8) (dust separation), passes a heat exchanger (9) and then enters an extractor (10).
  • the organic Solvents e.g. methanol
  • the non-extractable gases such as hydrogen, methane, carbon monoxide or carbon dioxide filtered (12) and a combustion or DENOX system (13, 14) fed from which they are released.
  • the solvent flow is in the extractor to a certain degree of enrichment in the circuit (15) and a secondary flow as a superheater (16) supplied, from (23) water vapor supplied via (19) becomes. Gases and vapors generated in the superheater reach the Fixed bed reactor (17), in which it is at about 750 ° C using a calcium aluminate catalyst to be split. (16) and (17) are represented by supplies a heat generator (2).
  • the water vapor / gas mixture obtained in (21) passes through the line (22) a heat exchanger (23) which the circulation evaporator (24) for Process water (25) from the gas-liquid separation container (26) operated.
  • the gas separated in (26) is fed to a filter (12) and then fed to the combustion (13, 14).
  • the water vapor located in (23) is the line (19) Superheater (16) and then fed to the fixed bed reactor (17).

Landscapes

  • Business, Economics & Management (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Management (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Fire-Extinguishing Compositions (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Treating Waste Gases (AREA)

Claims (7)

  1. Procédé de recyclage d'agents de combat chimiques caractérisé en ce que des agents de combat chimiques transposés dans la phase liquide sont convertis par réduction dans un réacteur à une température de 500-1000 °C sous l'effet de la catalyse d'un catalyseurs d'aluminate de calcium, les gaz réactionnels générés étant incinérés ou utilisés comme gaz de chauffe après séparation de composés d'halogènes, de soufre, d'ammonium, de phosphore et des hydrures éventuellement produits, sous forme de gaz de rejet, de liquides ou de solides.
  2. Procédé selon la revendication 1, caractérisé en ce que des agents de combat chimiques solides ou situés sur/dans une matrice solide ou des agents de combat chimiques liquides sont soumis à pyrolyse à une température de 300-1000 °C dans une atmosphère de gaz inerte, et ce que le gaz de pyrolyse ou le gaz de pyrolyse et les cendres volantes sont traités par extraction avec un solvant organique, en ce que la solution est dirigée sur une étape de vaporisation et en ce que le produit vaporisé est converti par réduction dans le réacteur.
  3. Procédé selon la revendication 1, caractérisé en ce que des agents de combat chimiques liquides ou des agents de combat chimiques solides mis en suspension sont mélangés à un solvant organique ou y sont remis en suspension et dirigés sur une étape de vaporisation avant que la conversion par réduction ait lieu dans le réacteur.
  4. Procédé selon la revendication 2, caractérisé en ce que la pyrolyse est exécutée à une température de 400 à 700 °C et en ce que comme gaz inerte, on utilise de l'azote, du dioxyde de carbone ou des gaz rares.
  5. Procédé selon la revendication 2 ou 3, caractérisé en ce que comme solvant organique, on utilise des alcools aliphatiques jusque C4, des esters d'acides carboxyliques en C1-C4, ou des cétones en C3-C5.
  6. Procédé selon la revendication 1, caractérisé en ce que les températures de réaction au sein du réacteur se situent de 700 à 800 °C.
  7. Procédé selon la revendication 1, caractérisé en ce que selon l'agent de combat chimique mis en oeuvre, on sépare et on élimine du gaz réactionnel, dans le cas de composés organiques d'arsenic, de l'arsenic, dans le cas de composés de chlore-azote-arsenic, de l'arsenic et du chlorure d'ammonium, sous forme de solides.
EP95116796A 1994-10-27 1995-10-25 Procédé pour le traitement thermocatalytique des agents de combat chimiques Expired - Lifetime EP0709116B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4438414A DE4438414C2 (de) 1994-10-27 1994-10-27 Verfahren zur thermisch-katalytischen Aufarbeitung chemischer Kampfstoffe
DE4438414 1994-10-27

Publications (2)

Publication Number Publication Date
EP0709116A1 EP0709116A1 (fr) 1996-05-01
EP0709116B1 true EP0709116B1 (fr) 2000-01-19

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EP95116796A Expired - Lifetime EP0709116B1 (fr) 1994-10-27 1995-10-25 Procédé pour le traitement thermocatalytique des agents de combat chimiques

Country Status (4)

Country Link
EP (1) EP0709116B1 (fr)
AT (1) ATE188878T1 (fr)
DE (2) DE4438414C2 (fr)
RU (1) RU2156631C2 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10157165B4 (de) * 2001-11-22 2006-11-23 GFE GmbH & Co. KG Gesellschaft für Entsorgung Verfahren und Anlage zur Entsorgung von Materialien, die arsenorganische Kampfstoffe und Metallschrott enthalten
DE10157162B4 (de) * 2001-11-22 2008-09-18 GFE GmbH & Co. KG Gesellschaft für Entsorgung Verfahren und Vorrichtung zur Entsorgung von Materialien, insbesondere von chemische Kampfstoffe enthaltenden Granaten
DE10157163A1 (de) * 2001-11-22 2003-06-18 Gfe Gmbh & Co Kg Ges Fuer Ents Verfahren und Vorrichtung zur Entsorgung von hochenergetische Stoffe enthaltenden Materialien, insbesondere von Granaten
CN113148954B (zh) * 2021-02-05 2021-11-30 山东滨农科技有限公司 一种农药生产用废气回收工艺

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2032036A1 (de) * 1966-03-03 1972-01-05 Werner Dr. Dosch Entgiftung toxischer Verbindungen
DE3940567A1 (de) * 1989-12-08 1991-06-13 Gsu Systemtechnik Gmbh Verfahren zur thermischen zersetzung von organischen und anorganischen kampfstoffen
EP0518379A3 (en) * 1991-06-13 1993-06-30 Kalkwerke H. Oetelshofen Gmbh & Co. Process for the removal of organic and inorganic toxic products from gaseous liquid and/or solid materials
DE4131471A1 (de) * 1991-09-21 1993-03-25 Rheinmetall Gmbh Verfahren zur hydrierung von nitroaromatischen sprengstoffen

Also Published As

Publication number Publication date
DE59507640D1 (de) 2000-02-24
DE4438414A1 (de) 1996-05-02
ATE188878T1 (de) 2000-02-15
EP0709116A1 (fr) 1996-05-01
RU2156631C2 (ru) 2000-09-27
DE4438414C2 (de) 1997-12-18

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