EP0709116A1 - 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
EP0709116A1
EP0709116A1 EP95116796A EP95116796A EP0709116A1 EP 0709116 A1 EP0709116 A1 EP 0709116A1 EP 95116796 A EP95116796 A EP 95116796A EP 95116796 A EP95116796 A EP 95116796A EP 0709116 A1 EP0709116 A1 EP 0709116A1
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EP
European Patent Office
Prior art keywords
warfare agents
arsenic
gas
reactor
gases
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.)
Granted
Application number
EP95116796A
Other languages
German (de)
English (en)
Other versions
EP0709116B1 (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
Gesellschaft fur Kampfmittelbeseitigung Dr Ing Koehler Mbh
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Publication of EP0709116A1 publication Critical patent/EP0709116A1/fr
Application granted granted Critical
Publication of EP0709116B1 publication Critical patent/EP0709116B1/fr
Anticipated expiration legal-status Critical
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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 workup of chemical warfare agents, their addition and decomposition products.
  • the present invention is therefore based on the object of providing a process for the complete reprocessing of chemical warfare agents without the need to incinerate the warfare agents, the remainder of the reprocessing must be stored in hazardous waste landfills and a long transport of the warfare agents is necessary before the reprocessing of the warfare agents.
  • the present invention enables the destruction or processing of liquid and solid chemical warfare agents, namely from ammunition and from storage containers, regardless of whether they are present alone, as liquid or solid mixtures with one another or mixed with organic solvents or formulated in propellant and smoldering mixtures.
  • the warfare agents can also be bound to a combustible or non-combustible matrix, for example when it comes to the remediation of armaments and war contaminants.
  • the matrix can be a medium (for example a solution, soil or a material), a metallic surface (for example a container or ammunition) or an additive.
  • the chemical warfare agents are preferably halogen-, sulfur-, nitrogen-, phosphorus- or arsenic-organic warfare agents, their additive and decomposition products, very preferably arsenic-organic warfare agents, whereby also arsenic-organic compounds of non-military origin are to be understood by which an environmental pollution goes out, such as Pesticides.
  • a liquid warfare agent has been subjected to vaporization and is then in the gas phase
  • this gas is fed directly into the reactor together with a mixture of vaporized organic solvent and water vapor and subjected to the thermal-catalytic workup, 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 are burned or used as heating gas after any hydrides, halogen, ammonium, sulfur and phosphorus compounds as Exhaust gases, liquids or solids have been separated.
  • the waste gases to be separated off from the reaction gases are preferably chlorine, bromine, fluorine, hydrogen sulfide or ammonia.
  • the pyrolyser can be a rotary tube furnace, a combustion chamber, preferably a radiation tube with indirect heat coupling.
  • the pyrolyser as well as the locks for the feed materials and the pyrolysis residue are charged with an inert gas, preferably nitrogen, argon or carbon dioxide.
  • the system is charged with 1 to 5 liters per 10 liter reaction space.
  • Pyrolysis coke incorporates inorganic residues (especially arsenic, if present in the warfare agent), as well as the heavy metals that may be contained in the warfare agents used. This pyrolysis residue is smeltable for special plants for the recovery of arsenic and metals.
  • the extractive treatment of the pyrolysis gases (step b)) and, if appropriate, the fly dust obtained is carried out in an extractor with an organic solvent, preferably an aliphatic alcohol to C4, a C3-C5 ketone or an ester of a C1-C4 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 to C4, a C3-C5 ketone or an ester of a C1-C4 carboxylic acid, very preferably with methanol, ethanol, propanol, methyl formate, ethyl formate, methyl acetate, ethyl acetate, methyl propionate, Acetone or butanone.
  • solvents are also suitable for step A) above.
  • the solution from step b) or A) or a warfare agent converted into the gas phase is fed at temperatures of 500 to 1000 ° C. after the addition of water vapor from a superheater into a fixed bed reactor and there to the respective end products under the catalysis of a calcium aluminate. Catalyst dismantled. For example, treating a solution in which methanol, acetone or an ester was the solvent produces hydrogen, methane, carbon monoxide and carbon dioxide.
  • the solvent-water vapor ratio is between 0.5 - 2: 1, preferably 1: 1 for arsenic organic compounds as starting materials.
  • catalysts based on calcium aluminate are used, preferably TZ 70 and calcium aluminates with other aluminum oxide contents, such as e.g. 3 CaO * Al2O3 (C3A).
  • the advantage of the process is that the reductive gas phase medium precludes the formation of dioxins.
  • the water generated in the fixed bed reactor is circulated and, if necessary, supplemented or discharged.
  • any hydrides, halogen, sulfur, ammonium and phosphorus compounds which have formed as waste gases or liquids or solids and also any elementary compounds which have occurred have to be removed. This is the case, for example, when working up arsenic organic compounds arsenic and when working up chlorine-nitrogen-arsenic organic compounds ammonium chloride and arsenic.
  • adamsite phenarsazine chloride
  • the Lewisite (2-chloroethenyldichlorarsine) or Clark (diphenylchlorosine) produces elemental arsenic hydrogen chloride.
  • the residual exhaust gases contained in a gas-liquid separation are fed to a combustion upstream of the DENOX system.
  • the amount of gas is e.g. when using methanol 1.4 m3 per kg.
  • the gas has the composition of approximately 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.
  • Arsenic-containing pyrolysis residues from step a) or the arsenic obtained in step c) or B) can be sent to smelting for the recovery of inorganic arsenic compounds.
  • Figure 1 shows a schematic representation of a plant for the disposal of arsenic-organic warfare agents.
  • the pyrolyzer (1) consists of a radiation tube. He receives the heat indirectly from the heat generator (2) by electrical or gas heating.
  • the inert gas eg nitrogen, is fed directly from (3).
  • the loading with solid arsenic-organic warfare agent eg Adamsite
  • An ammunition filled with warfare agents which is free of propellants, detonation and explosive charges, can also be introduced for loading.
  • Liquid feedstocks can also be introduced into the pyrolyser via (5) will.
  • the pyrolysis residue is discharged through a lock into line (6).
  • the pyrolysis gas passes through line (7) to a cyclone (8) (dust separation), passes through a heat exchanger (9) and then enters an extractor (10).
  • the organic solvent e.g. methanol, is sprayed into the extractor from (11).
  • the non-extractable gases such as hydrogen, methane, carbon monoxide or carbon dioxide, are filtered (12) and fed to a combustion or DENOX system (13, 14), from which they are released.
  • the solvent flow is conducted in the extractor to a certain degree of enrichment in the circuit (15) and fed to a superheater (16) as a secondary stream, water vapor being fed in from (23) via (19). Gases and vapors generated in the superheater reach the fixed bed reactor (17), in which they are split at approx. 750 ° C using a calcium aluminate catalyst. (16) and (17) are supplied by a heat generator (2).
  • Used liquid warfare agents (5) and warfare agent mixtures or solutions can be fed directly (16) and (17) after mixing (18) with the solvent (11) via line (19).
  • the water vapor / gas mixture obtained in (21) passes via line (22) a heat exchanger (23) which serves the circulation evaporator (24) for process water (25) from the gas-liquid separation container (26).
  • 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 fed via line (19) to the superheater (16) and then to the fixed bed reactor (17).

Landscapes

  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Business, Economics & Management (AREA)
  • Emergency Management (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Catalysts (AREA)
  • Fire-Extinguishing Compositions (AREA)
  • Treating Waste Gases (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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
DE4438414 1994-10-27
DE4438414A DE4438414C2 (de) 1994-10-27 1994-10-27 Verfahren zur thermisch-katalytischen Aufarbeitung chemischer Kampfstoffe

Publications (2)

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

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
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)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113148954A (zh) * 2021-02-05 2021-07-23 山东滨农科技有限公司 一种农药生产用废气回收工艺

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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

Citations (3)

* 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
DE4131471A1 (de) * 1991-09-21 1993-03-25 Rheinmetall Gmbh Verfahren zur hydrierung von nitroaromatischen sprengstoffen

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (3)

* 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
DE4131471A1 (de) * 1991-09-21 1993-03-25 Rheinmetall Gmbh Verfahren zur hydrierung von nitroaromatischen sprengstoffen

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
I.A-. UMJAROW ET AL.: "Methoden der Vernichtigung und Utilisation der Bestaende an Lewisit und Yperit", J. RUSS. CHEM. GES. "D.I. MENDELEEW", vol. 37, no. 3, 1993, pages 25 - 29
K.K. BABIEVSKY: "Methods of Destruction of Chemical Warefare Agents", SIPRI: CHEMICAL DISARMAMENT. NEW WEAPONS FOR OLD, 1975, STOCKHOLM, pages 102 - 103
NATIONAL RESEARCH COUNCIL: "Alternative Technologies for the Destruction of Chemical Agents and Munitions", 1993, NATIONAL ACADEMIY PRESS, WASHINGTON

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113148954A (zh) * 2021-02-05 2021-07-23 山东滨农科技有限公司 一种农药生产用废气回收工艺
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

Also Published As

Publication number Publication date
ATE188878T1 (de) 2000-02-15
DE4438414C2 (de) 1997-12-18
DE59507640D1 (de) 2000-02-24
DE4438414A1 (de) 1996-05-02
RU2156631C2 (ru) 2000-09-27
EP0709116B1 (fr) 2000-01-19

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