Title of Invention	"AN IMPROVED PROCESS FOR PREPARATION OF A PYROTECHNIC FAVOURED CASTABLE COLOUR SMOKE COMPOSITION"
Abstract	This invention relates to a process for the preparation of a pyrotechnic favoured castable colour smoke composition. According to the process a binder is prepared by mixing polyester resin, an accelerator and catalyst. A smoke composition is prepared by mixing of an oxidizer, sublimable dyes and fuel and the binder and smoke composition is mixed. Further this invention relates to an improved pyrotechnic favoured castable colour smoke composition. An improved composition has a binder of polyester resin, an accelerator and a catalyst and a smoke composition of oxidizer, sublimable dyes and fuel

Title of Invention

"AN IMPROVED PROCESS FOR PREPARATION OF A PYROTECHNIC FAVOURED CASTABLE COLOUR SMOKE COMPOSITION"

Abstract

This invention relates to a process for the preparation of a pyrotechnic favoured castable colour smoke composition. According to the process a binder is prepared by mixing polyester resin, an accelerator and catalyst. A smoke composition is prepared by mixing of an oxidizer, sublimable dyes and fuel and the binder and smoke composition is mixed. Further this invention relates to an improved pyrotechnic favoured castable colour smoke composition. An improved composition has a binder of polyester resin, an accelerator and a catalyst and a smoke composition of oxidizer, sublimable dyes and fuel

Full Text	FIELD OF INVENTION The present invention relates to an improved process of preparing pyrotechnic favoured castable coloured smoke which is suitable for generating coloured smoke using coloured dyes which sublime into vapour directly from solid state. PRIOR ART When a Smoke Composition utilizes the heat of chemical reaction between oxidizer and fuel, to vaporize the volatile ingredients present in the composition, it is known as Pyrotechnic Smoke Composition. In a Colour Smoke Composition the colour dye ingredients vaporize and subsequently the dye vapour condenses in atmosphere, giving Coloured Smoke. Some of the Pyrotechnic Colour Smoke Composition known in the art are made with binder or without binder. When a binder is used as a constituent of smoke composition, it is known as a Castable Smoke Composition. Pyrotechnic Favoured Castable Colour Smoke Composition have been used for signaling, marking, tracking, spotting and distress signaling. One of the Pyrotechnic Castable Colour Smoke Composition known in the art comprises by weight of 10 to 25% of alkali metal chlorate as oxidant, selected from the group consisting of Potassium Chlorate and Sodium chlorate, 10 to 30% of Guanidine Nitrate, 10 to 35% of synthetic-aliphatic epoxy resin, 1 to 15% of organic plasticizer, 0 to 3% of hardener, 25 to 50% of a sublimable organic dye, 0 to 5% of atleast one metal oxide and the carbazate. One of the disadvantages of the above is, that this composition has to be processed at elevated temperature of 60° C and above. Another disadvantage of the above composition is that, the binder is also to be prepared separately at elevated temperature of 60° C and above. Another Pyrotechnic Colour Smoke Composition known in the art. contains 1.4-benzenedicarboxylic acid between about 7 and 35% by weight, solvent red dye between about 30 and 50% by weight, fuel between about 13 and 25% by weight, potassium chlorate between about 17 and 30% by weight, sodium bicarbonate or magnesium bicarbonate between about 5 and 20% by weight, One of the disadvantages of the above composition is use of acetone in the preparation or the composition by the wet mixing method, as acetone is a fire hazard. This may result into injurv to workers and accidental fire during the course of its manufacture. Another disadvantage of the above composition is the use of special process equipment's required for its production/pelletisation Still another disadvantage of the above composition is that the density of the peilet being lower, production of smoke vis-a-vis per unit volume of the pellet is less. Still another disadvantage of the above composition is the that it poses dust hazard during processing due to the absence of binder. OBJECTS OF THE PRESENT INVENTION The primary object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not decompose when ignited in confinement under pressure of 0.5 to 0.6 Kg/Cm2 Another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition uses a synthetic aromatic polyester binder which is cheap and also abundantly available. Still another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not cause dust hazard during the process of manufacture. Yet another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can be pelleted-out at lower pressure while achieving higher pellet densities. Further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition favours the emission of smoke for longer period. Still further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition retains its colouring property while sublimating into vapour state. Yet further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces smoke which is visible from a greater distance, more particularly produces Orange colour smoke, which is distinctively visible. Even further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces voluminous smoke which hovers over the spot of its launch in calm wind conditions Yet further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces smoke which, does not rise very high to avoid loss of visibility due to dispersion Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can be produced without using special process equipment. Yet further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition has higher density and produces copious colour smoke per unit volume of the Composition Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not utilise hazardous substances for its production. Yet further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can he easily ignited . Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition is economical to produce. Even further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition which can be produced at ambient temperature. SUMMARY OF INVENTION According to the present invention there is provided a process for the preparation of a pyrotechnic favoured castable colour smoke comprising by the steps of: d) preparing a binder by mixing 5 to 10% by weight of polyster resin, an accelerator as herein described and catalyst as herein described, at a temperature of 25°C. e) Preparing a smoke by mixing 15 to 30% by weight of an oxidiser as herein described, sublimable dyes as herein described and 20 to 30% by weight of fuel as herein described in an aluminium tray to get a mixture of the ingredients, f) Mixing 5 to 8 parts of binder to 100 parts of the smoke composition. DESCRIPTION OF INVENTION The process of preparation of the formulation of present invention is as detailed as under: The relative humidity of the processing room during the entire processing is maintained at 50-60%. (a) Preparation of binder Accelerator, Cobalt Napthenate (Q-8021) and Catalyst, MEK peroxide (Q-8013), (in quantities required as per the specifications of the resin) are added to the polyester resin like HSR 8111. When the Accelerator and Catalyst are added to the polyester resin, the typical gelation duration obtained at 25° C is as below and depends on varying amount of Catalyst and Accelerator: Accelerator Catalyst Resin Gelatinizing Duration in ml in ml in Gms in minutes 1. 0.75 0.75 100 155 2. 1 1 100 65 3 1.5 1.5 100 23 The above are vigorously mixed/agitated to obtain a homogeneous binder (b) Preparation of the Composition The nominal ingredients percentage used in the Pyrotechnic colour smoke composition are as below: (Table Removed) The composition is prepared as per the following steps:- i) Required quantity of ingredients (excluding polyester resin which has been utilised for the preparation of binder) are mixed in an aluminium tray and sieved three times using preferably 600 micron IS sieve and then mixed for one hour using mechanical (drum mixer) means to get uniform mix. ii) Polyester resin prepared separately as per step(a) is added slowly to the smoke composition in an Aluminium tray and mixed for around thirty minutes using mechanical means like drum mixer, to get uniform mix. (iii) The composition is allowed to stabilise by retaining in the tray for about twenty four hours, thereafter the composition is pelletised. Filling Method 230 gms Pyrotechnic Favoured Castable Colour Smoke Composition is pressed at 530 kg/cm2 using 69 mm dia plunger to give perforated pellet. Four such pellets when assembled in a suitable container & ignited using priming composition or primed cambric and squib give Orange smoke for about 90 sec. Due to the Synergic effect of the constituents of the composition, a stable copius Orange coloured smoke is produced. However no smoke is produced by the constituents when ignited individually. WORKING EXAMPLES The composition of two samples prepared as per the present invention are as under: Wt% OF INGREDIENTS INGREDIENT SAMPLE-I SAMPLE-II 1. DyeRhodamine'B' 8 8 2. Dye Oil orange 52 52 3. Potassium Chlorate 20 20 4. Lactose 20 20 5.Binder(HSR8111) 5 parts 10 parts The performance parameters of the two samples as compared to the composition without use of binder are tabulated in Table-I: 1ABLE-I (Table Removed) The results indicate that the performance of orange coloured smoke compositions of Sample- I and Sample -I prepared as per the present invention is superior to the performance of coloured smoke composition without hinder The characteristics of coloured smoke composition with binder (Sample-1 and Sample-II) like average density, strain, stress are superior while the values combustion temperature and average burning rate are less as compared to orange coloured smoke composition without binder. The compositions disclosed in the present invention are susceptible to changes and modifications by those skilled in art. It is to be understood that such changes, modifications, adaptations are intended to be within the scope of the present invention which is further set forth under following claims: WE CLAIM: 1. A process for the preparation of a pyrotechnic favoured castable colour smoke composition comprising in the steps of: a) preparing a binder by mixing 5 to 10% by weight of polyster resin, an accelerator as herein described and catalyst as herein described, at a temperature of 25°C. b) Preparing a smoke composition by mixing 15 to 30% by weight an oxidiser as herein described, 5 to 15% of by weight sublimable dyes as herein described and 20 to 30% by weight of fuel as herein described in an aluminium tray to get a mixture of smoke composition, c) Mixing 5 to 8 parts of binder to 100 parts of the smoke composition. 2. A process as claimed in claim 1 wherein the polyester resin is HSR8 111 and present in an amount of preferably 5 to 8% by weight. 3. A process as claimed in claim 1 wherein said accelerator is cobalt napthenate. 4. A process as claimed in claim 1 wherein the said catalyst is MEK peroxide. 5. A process as claimed in claim 1 wherein said oxidizer is Ammonium Perchlorate and present in an amount of preferably 18 to 23% by weight. 6. A process as claimed in claim 1 wherein the said fuel is lactose and present in an amount of preferably 18 to 23% by wt. of the composition. 7. A process as claimed in claim 1 wherein the sublimable dyes used are preferably Dye Rhodamine 'B' and Dye Oil Orange. 8. A process as claimed in claim 1 wherein Dye Rhodamine 'B' is preferably 6 to 10% by weight. 9. A process as claimed in claim 1 wherein sublimable dye Oil Orange present in an amount of 40 to 60% by weight preferably 50 to 54% by weight. 10. A process for the preparation of pyrotechnic favoured castable colour smoke composition substantially described and illustrated herein.

Full Text

FIELD OF INVENTION
The present invention relates to an improved process of preparing pyrotechnic favoured castable coloured smoke which is suitable for generating coloured smoke using coloured dyes which sublime into vapour directly from solid state.
PRIOR ART
When a Smoke Composition utilizes the heat of chemical reaction between oxidizer and fuel, to vaporize the volatile ingredients present in the composition, it is known as Pyrotechnic Smoke Composition. In a Colour Smoke Composition the colour dye ingredients vaporize and subsequently the dye vapour condenses in atmosphere, giving Coloured Smoke. Some of the Pyrotechnic Colour Smoke Composition known in the art are made with binder or without binder. When a binder is used as a constituent of smoke composition, it is known as a Castable Smoke Composition. Pyrotechnic Favoured Castable Colour Smoke Composition have been used for signaling, marking, tracking, spotting and distress signaling.
One of the Pyrotechnic Castable Colour Smoke Composition known in the art comprises by weight of 10 to 25% of alkali metal chlorate as oxidant, selected from the group consisting of Potassium Chlorate and Sodium chlorate, 10 to 30% of Guanidine Nitrate, 10 to 35% of synthetic-aliphatic epoxy resin, 1 to 15% of organic plasticizer, 0 to 3% of hardener, 25 to 50% of a sublimable organic dye, 0 to 5% of atleast one metal oxide and the carbazate.
One of the disadvantages of the above is, that this composition has to be processed at elevated temperature of 60° C and above.
Another disadvantage of the above composition is that, the binder is also to be prepared separately at elevated temperature of 60° C and above.
Another Pyrotechnic Colour Smoke Composition known in the art. contains 1.4-benzenedicarboxylic acid between about 7 and 35% by weight, solvent red dye between about 30 and 50% by weight, fuel between about 13 and 25% by weight, potassium chlorate between about 17 and 30% by weight, sodium bicarbonate or magnesium bicarbonate between about 5 and 20% by weight,
One of the disadvantages of the above composition is use of acetone in the preparation or the composition by the wet mixing method, as acetone is a fire hazard. This may result into injurv to workers and accidental fire during the course of its manufacture.
Another disadvantage of the above composition is the use of special process equipment's required for its production/pelletisation
Still another disadvantage of the above composition is that the density of the peilet being
lower, production of smoke vis-a-vis per unit volume of the pellet is less.
Still another disadvantage of the above composition is the that it poses dust hazard during processing due to the absence of binder.
OBJECTS OF THE PRESENT INVENTION
The primary object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not decompose when ignited in confinement under pressure of 0.5 to 0.6 Kg/Cm2
Another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition uses a synthetic aromatic polyester binder which is cheap and also abundantly available.
Still another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not cause dust hazard during the process of manufacture.
Yet another object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can be pelleted-out at lower pressure while achieving higher pellet densities.
Further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition favours the emission of smoke for longer period.
Still further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition retains its colouring property while sublimating into vapour state.
Yet further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces smoke which is visible from a greater distance, more particularly produces Orange colour smoke, which is distinctively visible.
Even further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces voluminous smoke which hovers over the spot of its launch in calm wind conditions
Yet further object of the present invention is to have a Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition produces smoke which, does not rise very high to avoid loss of visibility due to dispersion
Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can be produced without using special process equipment.
Yet further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition has higher density and produces copious colour smoke per unit volume of the Composition
Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition does not utilise hazardous substances for its production.
Yet further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition can he easily ignited .
Still further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition is economical to produce.
Even further object of the present invention is to have Pyrotechnic Favoured Castable Colour Smoke Composition and process for preparation thereof wherein the composition which can be produced at ambient temperature.
SUMMARY OF INVENTION
According to the present invention there is provided a process for the preparation of a pyrotechnic favoured castable colour smoke comprising by the steps of:
d) preparing a binder by mixing 5 to 10% by weight of polyster resin, an
accelerator as herein described and catalyst as herein described, at a
temperature of 25°C.
e) Preparing a smoke by mixing 15 to 30% by weight of an oxidiser as
herein described, sublimable dyes as herein described and 20 to 30%
by weight of fuel as herein described in an aluminium tray to get a
mixture of the ingredients,
f) Mixing 5 to 8 parts of binder to 100 parts of the smoke composition.
DESCRIPTION OF INVENTION
The process of preparation of the formulation of present invention
is as detailed as under:
The relative humidity of the processing room during the entire
processing is maintained at 50-60%.
(a) Preparation of binder
Accelerator, Cobalt Napthenate (Q-8021) and Catalyst, MEK peroxide (Q-8013), (in quantities required as per the specifications of the resin) are added to the polyester resin like HSR 8111. When the Accelerator and Catalyst are added to the polyester resin, the typical gelation duration obtained at 25° C is as below and depends on varying amount of Catalyst and Accelerator:
Accelerator Catalyst Resin Gelatinizing Duration
in ml in ml in Gms in minutes
1. 0.75 0.75 100 155
2. 1 1 100 65
3 1.5 1.5 100 23
The above are vigorously mixed/agitated to obtain a homogeneous binder
(b) Preparation of the Composition
The nominal ingredients percentage used in the Pyrotechnic colour smoke composition are as below:
(Table Removed)
The composition is prepared as per the following steps:-
i) Required quantity of ingredients (excluding polyester resin which has been utilised for the preparation of binder) are mixed in an aluminium tray and sieved three times using preferably 600 micron IS sieve and then mixed for one hour using mechanical (drum mixer) means to get uniform mix.
ii) Polyester resin prepared separately as per step(a) is added slowly to the smoke composition in an Aluminium tray and mixed for around thirty minutes using mechanical means like drum mixer, to get uniform mix.
(iii) The composition is allowed to stabilise by retaining in the tray for about twenty four hours, thereafter the composition is pelletised.
Filling Method
230 gms Pyrotechnic Favoured Castable Colour Smoke Composition is pressed at 530 kg/cm2 using 69 mm dia plunger to give perforated pellet. Four such pellets when assembled in a suitable container & ignited using priming composition or primed cambric and squib give Orange smoke for about 90 sec.
Due to the Synergic effect of the constituents of the composition, a stable copius Orange coloured smoke is produced. However no smoke is produced by the constituents when ignited individually.
WORKING EXAMPLES
The composition of two samples prepared as per the present invention are as under:
Wt% OF INGREDIENTS
INGREDIENT SAMPLE-I SAMPLE-II
1. DyeRhodamine'B' 8 8
2. Dye Oil orange 52 52
3. Potassium Chlorate 20 20
4. Lactose 20 20
5.Binder(HSR8111) 5 parts 10 parts
The performance parameters of the two samples as compared to the composition without use of binder are tabulated in Table-I:

1ABLE-I
(Table Removed)

The results indicate that the performance of orange coloured smoke compositions of Sample- I and Sample -I prepared as per the present invention is superior to the performance of coloured smoke composition without hinder The characteristics of coloured smoke composition with binder (Sample-1 and Sample-II) like average density, strain, stress are superior while the values combustion temperature and average burning rate are less as compared to orange coloured smoke composition without binder.
The compositions disclosed in the present invention are susceptible to changes and modifications by those skilled in art. It is to be understood that such changes, modifications, adaptations are intended to be within the scope of the present invention which is further set forth under following claims:

WE CLAIM:
1. A process for the preparation of a pyrotechnic favoured castable
colour smoke composition comprising in the steps of:
a) preparing a binder by mixing 5 to 10% by weight of polyster resin, an
accelerator as herein described and catalyst as herein described, at a
temperature of 25°C.
b) Preparing a smoke composition by mixing 15 to 30% by weight an
oxidiser as herein described, 5 to 15% of by weight sublimable dyes as
herein described and 20 to 30% by weight of fuel as herein described
in an aluminium tray to get a mixture of smoke composition,
c) Mixing 5 to 8 parts of binder to 100 parts of the smoke composition.

2. A process as claimed in claim 1 wherein the polyester resin is
HSR8 111 and present in an amount of preferably 5 to 8% by weight.
3. A process as claimed in claim 1 wherein said accelerator is cobalt
napthenate.
4. A process as claimed in claim 1 wherein the said catalyst is MEK
peroxide.
5. A process as claimed in claim 1 wherein said oxidizer is Ammonium
Perchlorate and present in an amount of preferably 18 to 23% by
weight.
6. A process as claimed in claim 1 wherein the said fuel is lactose and
present in an amount of preferably 18 to 23% by wt. of the
composition.
7. A process as claimed in claim 1 wherein the sublimable dyes used are
preferably Dye Rhodamine 'B' and Dye Oil Orange.
8. A process as claimed in claim 1 wherein Dye Rhodamine 'B' is
preferably 6 to 10% by weight.
9. A process as claimed in claim 1 wherein sublimable dye Oil Orange
present in an amount of 40 to 60% by weight preferably 50 to 54% by
weight.
10. A process for the preparation of pyrotechnic favoured castable
colour smoke composition substantially described and illustrated
herein.

Documents:

308-del-2000-abstract.pdf

308-del-2000-claims.pdf

308-del-2000-correspondence-others.pdf

308-del-2000-correspondence-po.pdf

308-del-2000-description (complete).pdf

308-del-2000-form-1.pdf

308-del-2000-form-19.pdf

308-del-2000-form-2.pdf

308-del-2000-form-3.pdf

308-del-2000-gpa.pdf

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Patent Number

231691

Indian Patent Application Number

308/DEL/2000

PG Journal Number

13/2009

Publication Date

27-Mar-2009

Grant Date

08-Mar-2009

Date of Filing

23-Mar-2000

Name of Patentee

CHIEF CONTROLLER

Applicant Address

MINISTRY OF DEFENCE, GOVT OF INDIA, B-341, SENA BHAWAN, DHQ P.O. NEW DELHI-110011, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	HARIDWAR SINGH	HEMRL, SUTARWADI, PUNE-411 021, INDIA.
2	AMARJIT SINGHA	HEMRL, SUTARWADI, PUNE-411 021, INDIA.
3	PRAKASH JAGANNATHRAO KAMALE	HEMRL, SUTARWADI, PUNE-411 021, INDIA.
4	JAYANT NARAYAN KULKARNI	HEMRL, SUTARWADI, PUNE-411 021, INDIA.

PCT International Classification Number

C06D 3/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA