Title of Invention

"A 2-CHLOROBENZYLIDENEMALONONITRILE BASED COMPOSITION AND A PROCESS OF PREPARATION THERE-OF"

Abstract

This invention relates to a 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form comprising a mixture of 10 to 60% by wt of CS, 10-60% by wt of nitro-cellulose, 3 to 30% by wt of magnesium oxide, 1 to 25% by wt of zinc oxide, 5 to 35% by wt of titanium dioxide and 2 to 30% by wt of potassium nitrate, said capsule preferably contains the CS-pyrotechnic mixture in quantity 0.4 to 0.8 gm per capsule. Further this invention also relates to a process for the preparation of 2-chlorobenzylidenemalononitrile comprising the steps of preparing a mixture of pyrotechnic materials by taking 10-60% by wt of nitro-cellulose, 3 to 30% by wt of magnesium oxide, 1 to 25% by wt of zinc oxide, 5 to 35% by wt of titanium dioxide and 2 to 30% by wt of potassium nitrate, grinding as herein described and mixing 10 to 60% by wt of CS thoroughly for 10 to 60 minutes at 10 to 50°C temperature, filing of capsule with the CS-pyrotechnic mixture, preparing quick match as herein described and incorporating it in the capsule.

Full Text

FIELD OF INVENTION This invention relates to an ignitable 2-chlorobenzylidenemalononitrile (CS) based composition and a process of preparation there of, for safe dissemination for training the personnel for use of riot control agents and also for testing the leakage in various air purifying filters used in ships and canisters/facemasks. PRIOR ART 2-Chlorobenzylidenemalononitrile (CS) is a riot control agent. It is a white crystalline solid and is usually mixed with a pyrotechnic mixture in a grenade or canister for use. Its useful form is intended to be a smoke or fog of suspended particles. It is stable under all normal conditions of storage and does not corrode metals. It is ten times more potent irritant, but less toxic than -chloroacetophenone (CN) that is presently used as a riot control agent by the police in India. CS produces its full range of effects in 20-60 s in low concentrations and recovery is complete within 30 minutes. Various compositions based on 2-Chlorobenzylidenemalononitri!e (CS) for the dissemination as riot control agents are known in the art. These compositions are used in various forms, which include tear gas cartridges, ammunitions and hand grenades such as M7A1, M7A2 and M7A3 CS hand grenades, M25 series bursting-type grenades etc. One of the CS-based composition known in the art, according to US patent 3,729,350 comprises 50 -75 % CS and 25-50% high explosive such as RDX or HMX. The main disadvantage of the above composition and process is that the composition can be used in the form of cartridges, ammunitions and hand grenades, which are suitable for actual crowd control only and has limitations for the .actose 15%, and kaolin 15%. The ignition composition for this formulation consists of 50% polyester resin and 50% red phosphorus. The main disadvantage of the above composition is that such composition can be used in the form of cartridges, ammunitions and hand grenades, which are suitable for actual crowd control only and has limitations for the application for training purpose or for testing leakage in various air purifying systems. Yet another disadvantage of the known compositions is that the cost of the chemical composition is high as ingredients such as polyester resin is used. Still another important disadvantage of the above known processes is that the manufacturing process involves high risk and requires skilled persons. .Further disadvantage of the above composition is that the process involves the risk of accidental ignition by mechanical means such as pull-wire friction. Yet further disadvantage of the above composition is that the cost of the chemical composition is high as it involves costly ingredients such as polyester. Still further disadvantage of the above composition is that the handling as well as operation of the composition in the form in which these arq used, requires trained manpower. Another riot control agents-based composition known in the art', according to US patent 3 909 324, comprises of 20-70% riot control agent like CS, 12-40% fuels such as monoaminoguanidium nitrate or its di or triamino derivatives, ethylene bis(aminoguanidium) dinitrate or their condensation products, 8-30% inorganic oxidiser like potassium chlorate or ammonium chlorate along with 0.2-2% combustion catalyst like potassium chromate or iron(lll) oxide. > The main disadvantage of the above composition known in the art, is that the above composition can be used only in the form of cartridges/ammunitions and hand grenades, which are suitable for actual crowd control exercises only and has limitations for the application for training purpose as well as to test leakage .in various air purifying systems. Another disadvantage of the above composition is that the combustion temperature goes up from 340 to 770°C which results in partial decomposition of the main ingredient, Chlorobenzylidenemalononitrile with the resuk that the dissemination efficiency of the composition goes down to 60% . NEED FOR THE PRESENT INVENTION There is a need for ignitable 2-chlorobenzylidenemalononitrile (CS) based composition and process of preparation there of, in a small capsule form, which is easy to handle and safe, the smoke produced on dissemination is effective and non-toxic and dissemination efficiency remains unaffected during combustion. OBJECTS OF THE PRESENT INVENTION The main object of the present invention is to provide a non-hazardous dissemination formulation and a process for preparation thereof, wherein the formulation is based on the mixture of 2-chlorobenzylidenemalononitrile(CS) and pyrotechnic materials. Another object of the present invention is to provide an ignitable 2-chlorobenzylidenemalononitrile based formulation in capsule form, which is easy to handle, non-toxic and effective for use. Yet another object of the present invention is to provide a ready-to-use, 2-chlorobenzylidenemalononitrile based ignitable formulation. Still another object of the present invention is to provide ignitable 2-chlorobenzylidenemalononitrile(CS) based formulation which uses easily available materials. Further object of the present invention is to provide an ignitable 2-chlorobenzylidenemalononitrile based formulation, which involves low cost materials. Still further object of the 'present invention is to provide an ignitable 2-chlorobenzylidenemalononitrile(CS) based composition, in which temperature during combustion does not go high and therefore decomposition of active ingredient i.e. CS does not takes place; with the result that dissemination efficiency is unaffected during combustion and is therefore maintained to its maximum level. Yet further object of the present invention is to provide homogeneous CS-pyrotechnic mixture formulation, which produces irritating smoke uniformly on ignition. SCRIPTTON OF TNVENTTON According to this invention there is provided a 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form comprising a mixture of CS, nitro-cellulose, magnesium oxide, zinc oxide, titanium dioxide and potassium nitrate. Further according to this invention there is provided a process for the preparation of 2-chJorobeflzylidenetnalononitriJe comprising the steps of:- (a) preparing a mixture of pyrotechnic materials with CS powder (b) filling of capsule with the CS-pyrotechnic mixture (c) preparing quick match and incorporating it in the capsule. In accordance with the present invention the process for preparation of ignitable 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form, comprises following steps: 1. Preparation of CS-pyrotechnic materials mixture a) Preparing a mixture of pyrotechnic materials, taking Nitrocellulose 10 to 60% by weight preferably 20 to 40% by weight; magnesium oxide 3 to 30% by weight preferably 5 to 20% by weight; zinc oxide 1 to 25% by weight preferably 3 to 18% by weight, titanium dioxide 5 to 35% by weight preferably 8 to 20% by weight and potassium nitrate 2 to 30% by weight preferably 6 to 18% by weight. b. Grinding the mixture obtained in step (a) above in an electrically operated mechanical mixture at 10 to 50°C preferably at 20 to 40°C for a period of 10 to 60 minutes preferably for 20 to 40 minutes. c. Addition of CS in powder 10 to 60 % by weight preferably 20 to 40% by weight to the above pyrotechnic mixture and thoroughly mixed for a period of 10 to 60 minutes preferably for 20 to 40 minutes at a temperature of 10 to 50°C preferably 20 to 40°C. Preparation of CS based ignitable capsule a. Preparation of empty capsule: Gelatine capsules were prepared from gelatine, methylparaben, propylparaben, sodium lauryl sulphate and water. The composition was adjusted in such a way that moisture present should not effect the efficiency of the pyrotechnic mixture. To prevent capsule from catching fire on ignition, humidity, temperature and gelatine viscosity are controlled throughout the process of preparation. Further the length and diameter of the capsule is maintained as 1.7 to 2.5 cm length preferably 2.0 to 2.4 cm and 0.5 to 1 cm diameter preferably 0.6 to 0.8 cm. b. Preparation of quick match: Finely ground black powder (gun powder) is taken in a shallow container and water is added to it in drops with constant mixing with a glass rod. Water is added till a paste is obtained. This is coated on a cotton twine to make uniform thickness of 0.5 to 1 cm preferably 0.6 to 0.8 cm after complete drying. c. Filling of the capsule and incorporation of quick match: The capsule is filled with the 2-chlorobenzylidenemalononitrile based composition prepared by the step(1), filling 0.3 to 0.9 g preferably 0.4 to 0.7 g of the composition in each capsule. The quick match is incorporated through the centre of the capsule. It may be noted that though the present invention involves, mixing of ingredients at temperatures between 20 to 40°C but there is NO mere aggregation of properties but there is synergetic effect amongst the ingredients. None of the individual chemicals in the CS based composition .of the present invention, is ignitable whereas the mixture i.e. the composition is ignitable. Another synergetic effect exhibited by the composition is that none of the individual ingredients of the CS based composition of. the present invention produces, smoke on heating whereas the composition produces smoke on ignition. Yet another synergetic effect exhibited by the composition is that none of the individual component of the composition of the present invention, increases the temperature of the pyrotechnic mixture to burn the active ingredient of the composition namely CS into the atmosphere whereas the formulation on ignition, produces heat enough to bring about the safe dissemination of CS into the atmosphere without its decomposition. The invention will now be illustrated with a working example which is intended to be an illustrative example to illustrate the working of the invention and is not intended to be taken restrictively to imply any limitation on the scope of the present invention. EXAMPLE A pyrotechnic composition comprising 225 g nitro-cellulose, 150 g magnesium oxide, 135 g zinc oxide, 160 g titanium dioxide and 100 g potassium nitrate were grinded in an electrically operated mechanical mixer. It was mixed in such a way that there was no increase in temperature during the process. It was further mixed with powder of 230 g 2-chlorobenzylidenemalononitrile (CS) at the same temperature to generate a tiomogeneous mixture. The whole mixture was thoroughly mixed and transferred to an airtight container. Quick match was inserted into the gelatine capsule, and the capsule was filled with the above-prepared mixture of CS and pyrotechnic materials. The capsule is kept in a lock-type polythene bag and then stored in a cardboard box. It is understood that the process of the present invention is susceptible to modifications, adaptations and changes by those skilled in the field of present invention. Such modifications, adaptations and changes are intended to be covered within the scope of the present invention which is further set forth under the following claims:- WE CLAIM: 1. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form comprising a mixture of 10 to 60% by wt of CS, 10-60% by wt of nitro-cellulose, 3 to 30% by wt of magnesium oxide, 1 to 25% by wt of zinc oxide, 5 to 35% by wt of titanium dioxide and 2 to 30% by wt of potassium nitrate, said capsule preferably contains the CS-pyrotechnic mixture in quantity 0.4 to 0.8 gm per capsule. 2. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 wherein 2-chlorobenzylidenemalononitrile (CS) is preferably in quantity of 20 to 40% by weight of the mixture of pyrotechnic materials. 3. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 wherein nitro-cellulose in the said pyrotechnic materials mixture is preferably 20 to 40% by weight of the pyrotechnic material. 4. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 wherein zinc oxide is preferably 3 to 18% by weight of the pyrotechnic materials. 5. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 wherein magnesium oxide is preferably in quantity 5 to 20% by weight of the pyrotechnic materials. 6. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 in titanium dioxide in the said pyrotechnic materials mixture is preferably 8 to 20% by weight of pyrotechnic materials. 7. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form as claimed in claim 1 wherein potassium nitrate in the said pyrotechnic materials mixture is preferably used is 6 to 18% by weight of the pyrotechnic materials. 8. A 2-chlorobenzylidenemalononitrile (CS) based composition in capsule form substantially as herein described and illustrated in the examples. 9. A process for the preparation of 2-chlorobenzylidenemalononitrile comprising the steps of: (a) preparing a mixture of pyrotechnic materials by taking 10-60% by wt of nitro-cellulose, 3 to 30% by wt of magnesium oxide, 1 to 25% by wt of zinc oxide, 5 to 35% by wt of titanium dioxide and 2 to 30% by wt of potassium nitrate, grinding as herein described and mixing 10 to 60% by wt of CS thoroughly for 10 to 60 minutes at 10 to 50°C temperature, (b) filing of capsule with the CS-pyrotechnic mixture, (c) preparing quick match as herein described and incorporating it in the capsule. 10. A process for the preparation of 2- chlorobenzylidenemalononitrile (CS) based composition substantially as herein described and illustrated in the examples.

Documents:

252-DEL-2002-Abstract-(14-02-2008).pdf

252-del-2002-abstract.pdf

252-DEL-2002-Claims-(14-02-2008).pdf

252-del-2002-claims.pdf

252-DEL-2002-Correspondence-Others-(14-02-2008).pdf

252-del-2002-correspondence-others.pdf

252-del-2002-correspondence-po.pdf

252-DEL-2002-Description (Complete)-(14-02-2008).pdf

252-del-2002-description (complete).pdf

252-del-2002-form-1.pdf

252-del-2002-form-18.pdf

252-DEL-2002-Form-2-(14-02-2008).pdf

252-del-2002-form-2.pdf

252-del-2002-form-3.pdf

252-del-2002-pa-(06-01-2009).pdf