WO2000054846A1 - Process for chemical destruction of sulphur mustard - Google Patents
Process for chemical destruction of sulphur mustard Download PDFInfo
- Publication number
- WO2000054846A1 WO2000054846A1 PCT/IN1999/000040 IN9900040W WO0054846A1 WO 2000054846 A1 WO2000054846 A1 WO 2000054846A1 IN 9900040 W IN9900040 W IN 9900040W WO 0054846 A1 WO0054846 A1 WO 0054846A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sulphur
- destruction
- thiophilic
- mustard
- chemical
- 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.)
- Ceased
Links
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
-
- 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
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
Definitions
- the invention relates to an improved process for chemical destruction of Sulphur Mustard (SM) through chemical conversion of SM into non-toxic products.
- SM Sulphur Mustard
- Sulphur mustard chemically known as * , 1 ' -thiobis- (2-chloroethane) is a highly toxic and persistent liquid vesicant.
- Methods known in the art for destruction of SM consist in high temperature reactions which involves destruction of SM by heating at high temperature. Such method comprise incineration, pyrolysis, plasma torch and molten metal system. Among all these high temperature reaction methods, incineration is a well proven method and is widely used. However, this method is attended with certain disadvantages. The main disadvantage is that very high temperature of the order of 800-1200°C is required to incinerate SM completely. Another disadvantage is that in the downstream of the process, large quantity of sodium hydroxide solution is required, through which toxic gases such as hydrogen chloride and sulphurdioxide formed in the reaction, have to be passed to neutralise them.
- Still another disadvantage is that despite neutralisation of toxic gases by passing through sodium hydroxide solution, uncondensed gases like carbon monoxide, carbon dioxide etc. goes into the atmosphere which leads to pollution and as such the process is not ecof ⁇ endly. Yet another disadvantage is that large quantity of liquid effluent is generaged by the neu t ralisation of toxic gases by sodium hydroxide solution which causes environmental pollution. A further disadvantage s that the cost of destruction s very high.
- Another method known in the art for destruction of SM is chemical neutralisation technology which includes hydrolysis, oxidation and reductive degradation of SM. The chemical neutralisation method based on hydrolysis is also attended with several distinct disadvantages.
- sulphone of SM which is one of the product formed by oxidation, has vesicant properties and it is toxic in nature.
- Another disadvantage is that large quantities of gaseous, liquid and solid wastes are generated.
- Yet another disadvantage is that the cost of destruction of SM is very high as large quantity of oxidising agents are required.
- oxidising agents such as hydrogen peroxide, p-chloro perbenzoic acid, chloramine-T and N-chloro compounds are unstable, thereby requiring constant upstream supply of these oxidising agents.
- SM is detoxified into gaseous products by reaction of sodium in the presence of liquid ammonia.
- This method is also known as solvated electron system.
- a disadvantage of such a process is that large quantity of sodium is required to neutralise SM completely and sodium poses considerable difficulties in storage and handling due to its high reactivity and fire hazards.
- Another disadvantage is that large quantity of alcohol is required to destroy the unreacted sodium after the reaction with the result that large quantity of effluent is generated and also large quantities of inflammable hydrogen gas is also generated which poses fire hazards.
- Still another disadvantage is that to make liquid ammonia required for such a method, the liquification of ammonia requires large quantity of liquid nitrogen which makes overall process very costly.
- thiophilic agents are used as non-corrosive destruction agents for chemical destruction of SM.
- the thiophilic agents are formed by dissolving sulphur in liquid ammonia or alkyl amine.
- One of the method known in the art for preparation of thiophilic agent is by dissolving sulphur in diethylenetri- amine.
- SM is then converted into cyclic compound by reacting thiophilic agent with SM at room temperature for a period of 24 hours.
- Hexane is used for isolation and extraction of cyclic product after chemical conversion of SM.
- a major disadvantage of such process is the long reaction time of the order of 24 hours, and that diethyle- netriamine used in the process cannot be recovered and recycled with the result that unreacted amine goes into the effluent which poses environment hazards.
- Another disadvantage is that hexane used as an organic solvent in the process has a low boiling point which poses fire hazard.
- Still another disadvantage is that the use of large quantities of hexane and the inability to recover and recycle the unreacted diethylenetriamine, makes the process costly, particularly for upscaling.
- the primary object of the present invention is to propose an improved process for chemical destruction of SM through chemical conversion into non-toxic products.
- Another object of the present invention is to propose a process for destruction of SM in which SM is converted completely into non-toxic and non-corrosive products which can be handled easily.
- Still another object of the present invention is to propose a process for chemical destruction of SM which is eco- friendly.
- Yet another object of this invention is to propose a process for destruction of SM which does not require the use of any toxic corrosive organic solvents.
- a process for destruction of sulphur mustard reacting sulphur mustard with a thiophilic agent prepared by dissolving sulphur in ethylenediamine and/or ethanol diamine Further according to this invention there is provided a thiophilic reagent comprising sulphur dissolved in ethylenediamine and/or ethanol diamine and at a concentration of 3 to 10 w/w.
- the present invention envisages a process destruction of SM through chemical conversion of SM into non-toxic cyclic and polymeric products. The chemical process involves reacting SM with a thiophilic reagent.
- the thiophilic agent of this invention is prepared by dissolving sulphur in ethylenediamine or ethanol diamine or a combination thereof whereas the processes known in the art use diethylenetriamine.
- the ethylenediamine used in the present invention can be recovered and recycled making the process ecofriendly and cost-effective.
- the process of the present invention is highly time-efficient as it takes only 30-60 minutes for complete destruction of SM.
- the process of the present invention enables 100% conversion of SM into non-toxic products, whereas in the known process, the conversion of SM into cyclic products is of the order of 99-99.8% only. In the known process, conversion of SM is carried out at room temperature whereas in the present invention, the conversion of SM into non- toxic products is carried out at 50-70°G.
- the proposed process for the destruction of SM comprises following steps:
- thiophilic agent a. Dissolving the commercially available sulphur powder in ethylenediamine (commercally available, purity above 95%). Concentration of sulphur in ethylenediamine is kept between 3-10% preferably 4-6% w/w. b. Removing any undissolved portion.
- Ethylenediamine (1.5L) is taken in a round bottom flask equipped with condenser and dropping funnel to which sulphur (76 gms) is added with continuous stirring. The this sulphur mustard (250 gms) is added.
- sulphur 76 gms
- the reaction mixture is heated to 65°C for 60 minutes with continuous stirring. After 60 minutes, the reaction mixture is cooled at room temperature and filtered through nutche filter. The filtrate is kept for further reaction.
- the solid is analysed by Gas Liquid chromatography to find out the percentage conversion after extraction with chloroform.
- the dried solid so obtained can be stored as non-toxic solid. The 100% conversion of SM to non-toxic products is thus achieved.
- the non- toxic nature of the products are confirmed by animal experiments using mice and LD value was found to be grater than 5 gm per kg body weight.
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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Removal Of Specific Substances (AREA)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP99961270A EP1169096B1 (en) | 1999-03-15 | 1999-08-20 | Process for chemical destruction of sulphur mustard |
| US09/936,482 US6479723B1 (en) | 1999-03-15 | 1999-08-20 | Process for chemical destruction of sulphur mustard |
| DE69906391T DE69906391T2 (de) | 1999-03-15 | 1999-08-20 | VERFAHREN ZUR CHEMISCHEN ZERSTöRUNG VON SCHWEFEL-SENFGAS |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IN407/DEL/99 | 1999-03-15 | ||
| IN407DE1999 IN191232B (OSRAM) | 1999-03-15 | 1999-03-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2000054846A1 true WO2000054846A1 (en) | 2000-09-21 |
Family
ID=11089658
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IN1999/000040 Ceased WO2000054846A1 (en) | 1999-03-15 | 1999-08-20 | Process for chemical destruction of sulphur mustard |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US6479723B1 (OSRAM) |
| EP (1) | EP1169096B1 (OSRAM) |
| DE (1) | DE69906391T2 (OSRAM) |
| IN (1) | IN191232B (OSRAM) |
| RU (1) | RU2203118C1 (OSRAM) |
| WO (1) | WO2000054846A1 (OSRAM) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2330702C2 (ru) * | 2003-02-18 | 2008-08-10 | Дифенс Резерч Энд Дивелопмент Организейшн | Способ уничтожения загущенного иприта |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1613402B8 (en) * | 2003-03-12 | 2013-03-06 | Queen's University At Kingston | Method of decomposing organophosphorus compounds |
| US8618346B2 (en) | 2007-07-05 | 2013-12-31 | King Saud University | Process for the destruction of sulfur and nitrogen mustards and their homologous/analogous at ambient conditions |
| US20090187060A1 (en) * | 2008-01-22 | 2009-07-23 | E-Z-Em, Inc. | Method and Formulation for Neutralizing Toxic Chemicals and Materials |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3102746A1 (de) * | 1981-01-28 | 1982-09-02 | Bundesrep Deutschland | Verfahren und vorrichtung zur dekontamination von c-kontaminierten objekten |
| DE69019992T2 (de) * | 1990-11-02 | 1995-10-12 | Her Majesty The Queen As Repre | Metalloximat/polyethylenglykole chemisches dekontaminierungssystem. |
| FR2689021B1 (fr) * | 1992-03-26 | 1995-09-29 | France Etat Armement | Procede de decontamination de substrats contamines par des agents toxiques a l'aide d'une composition a base de persulfate. |
| US5387717A (en) * | 1992-08-12 | 1995-02-07 | Buckman Laboratories International, Inc. | Method for the detoxification of mustard gas, sulfur-containing quaternary ammonium ionene polymers and their use as microbicides |
| RU2073542C1 (ru) * | 1994-09-26 | 1997-02-20 | Саратовское высшее военное инженерное училище химической защиты | Способ утилизации отравляющих веществ группы люизита, иприта и их смесей |
| CZ130198A3 (cs) * | 1995-11-07 | 1998-12-16 | Commodore Applied Technologies, Inc. | Způsob likvidace chemických bojových látek a zařízení pro jeho provádění |
| US5760089A (en) * | 1996-03-13 | 1998-06-02 | The United States Of America As Represented By The Secretary Of The Navy | Chemical warfare agent decontaminant solution using quaternary ammonium complexes |
-
1999
- 1999-03-15 IN IN407DE1999 patent/IN191232B/en unknown
- 1999-08-20 RU RU2001127673/12A patent/RU2203118C1/ru not_active IP Right Cessation
- 1999-08-20 EP EP99961270A patent/EP1169096B1/en not_active Expired - Lifetime
- 1999-08-20 WO PCT/IN1999/000040 patent/WO2000054846A1/en not_active Ceased
- 1999-08-20 US US09/936,482 patent/US6479723B1/en not_active Expired - Lifetime
- 1999-08-20 DE DE69906391T patent/DE69906391T2/de not_active Expired - Lifetime
Non-Patent Citations (3)
| Title |
|---|
| CHEMICAL ABSTRACTS, 1 January 1900, Columbus, Ohio, US; abstract no. 112:133993, GU WEIZHANG, PENG ZHENHUA: "Decontamination system for a rapid destruction of mustard gas" XP002948764 * |
| CHEMICAL ABSTRACTS, 1 January 1900, Columbus, Ohio, US; abstract no. 128:3384, LUKOVIC Z, ET AL: "Kinetics of the reaction of 2,2'-dichlordiethylsulfide and 2-chlorethyl ethylsulfide with diethylenetriamine and triethylamin in 2-methoxyethanol" XP002948765 * |
| OTHMER K: "ENCYCLOPEDIA OF CHEMICAL TECHNOLOGY CHEMICALS IN WAR", KIRK OTHMER ENCYCLOPEDIA OF CHEMICAL TECHNOLOGY., XX, XX, vol. 05, no. 04, 1 January 1993 (1993-01-01), XX, pages 794 - 816, XP002948770 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2330702C2 (ru) * | 2003-02-18 | 2008-08-10 | Дифенс Резерч Энд Дивелопмент Организейшн | Способ уничтожения загущенного иприта |
| US7518029B2 (en) | 2003-02-18 | 2009-04-14 | Defence Research & Development Organisation | Process for destruction of gelled sulphur mustard |
Also Published As
| Publication number | Publication date |
|---|---|
| RU2001127673A (ru) | 2004-03-20 |
| IN191232B (OSRAM) | 2003-10-11 |
| RU2203118C1 (ru) | 2003-04-27 |
| DE69906391T2 (de) | 2004-02-12 |
| US6479723B1 (en) | 2002-11-12 |
| EP1169096B1 (en) | 2003-03-26 |
| DE69906391D1 (de) | 2003-04-30 |
| EP1169096A1 (en) | 2002-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4400552A (en) | Method for decomposition of halogenated organic compounds | |
| JP3090333B2 (ja) | 不安定化合物の熱水分解による環境上許容される廃棄物処分 | |
| JPS59131373A (ja) | 有機液からのpcb及び他のハロゲン化有機化合物の除去 | |
| EP1169096B1 (en) | Process for chemical destruction of sulphur mustard | |
| JP5134951B2 (ja) | ヨウ素の回収方法 | |
| US4326090A (en) | Destruction of PCB's | |
| US5608112A (en) | Process for reducing organic pollutants | |
| US4460797A (en) | Method for decomposition of halogenated organic compounds | |
| SK77699A3 (en) | Method for producing n-substituted 3-hydroxypyrazoles | |
| US5545800A (en) | Clean process to destroy arsenic-containing organic compounds with recovery of arsenic | |
| US4447667A (en) | Process for the dehalogenation of organic compounds | |
| US6010632A (en) | Hydrothermal oxidation of organic compounds with heterogenous neutralizing reagent | |
| US5290432A (en) | Method of treating toxic aromatic halogen-containing compounds by electrophilic aromatic substitution | |
| US6124519A (en) | Method of decomposing polychlorobiphenyls | |
| CA1242459A (en) | Process for the destruction of by-product tetranitromethane | |
| US6960701B2 (en) | Neutralization of vesicants and related compounds | |
| JP3247505B2 (ja) | ハロゲン化芳香族化合物を分解する方法 | |
| Kozlov | UTILIZATION OF HYDRAZINE. PART 1 CHEMISTRY BASIC PROCESSES | |
| JP3247543B2 (ja) | ハロゲン化芳香族化合物のアルカリ分解方法 | |
| JPH04503961A (ja) | 硝酸エステルの製造方法 | |
| JP5237806B2 (ja) | メチルアココビリン酸誘導体、アルキル化用組成物及び当該組成物を利用した有害化合物の無害化方法 | |
| EP1594577B1 (en) | A process for destruction of gelled sulphur mustard | |
| CN113787082B (zh) | 一种三氯吡啶醇钠合成过程产生的废催化剂无害化处理方法 | |
| JPH08141107A (ja) | ハロゲン化有機化合物の分解方法 | |
| KR100545687B1 (ko) | 산성용액을 이용한 폴리염화페닐 무해화 처리방법 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AK | Designated states |
Kind code of ref document: A1 Designated state(s): RU US |
|
| AL | Designated countries for regional patents |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE |
|
| 121 | Ep: the epo has been informed by wipo that ep was designated in this application | ||
| DFPE | Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101) | ||
| WWE | Wipo information: entry into national phase |
Ref document number: 1999961270 Country of ref document: EP |
|
| WWE | Wipo information: entry into national phase |
Ref document number: 09936482 Country of ref document: US |
|
| WWP | Wipo information: published in national office |
Ref document number: 1999961270 Country of ref document: EP |
|
| WWG | Wipo information: grant in national office |
Ref document number: 1999961270 Country of ref document: EP |