Title of Invention

"A PYROTECHNIC COMPOSITION FOR THE ENERGY RICH PROPELLANT AND THE PROCESS FOR THE PREPARATION THEREOF"

Abstract This invention relates to a pyrotechnic composition for energy rich propellant comprising magnesium powder as metal fuel and present in the amount of 22 to 50% by weight preferably 37 to 47% by weight, potassium nitrate as an oxidizer and present in an amount of 70 to 42% by weight preferably 55 to 45% by weight, and the remaining is 8 to 10% of binder as a solution of plasticised ethyl cellulose (PEC) in toluene and further according to this invention there is provided a process for the preparation of pyrotechnic composition for energy rich propellant which comprises in the steps of preparing a mixture of 22 to 50% by weight of magnesium powder with purity higher than 95% and 70 to 42% by weight of potassium nitrate, mixing 8 to 10% PEC solution with a mixture of magnesium powder and potassium
Full Text -2-
FIELD OF INVENTION
This invention relates to a pyrotechnic composition for energy rich propellant
and the process for the preparation thereof.
PRIOR ART;
The three main classes of propellants viz. Composite, double based and
composite modified double based, have to function at extremes of temperature
and some times at high altitude according to the end use. For stable
combustion, a certain amount of initial pressure is necessary which is different
for different types of propellants depending upon the flame characteristics of the
propellant. The critical combustion pressure required for composite propellants
is 10-15 Kg/cm2 for double based propellant is 30-35 Kg/cm2 and for composite
modified double based propellant it is 20-25 Kg/cm2.
Conventionally gun powder having high gas to solid ratio has been used as an
efficient igniter for ignition of double based propellants at ground level.
The disadvantage of using gun powder as igniter is that it fails to ignite at high
attitude.
Another disadvantage of using gun powder as igniter is that it is not a reliable
igniter for composite and composite modified double based propellants.
Yet another disadvantage of using gun powder as igniter is that it does not give
satisfactory ignition for composite propellants which have high auto ignition
temperature and poor mechanical properties.
Further disadvantage of using gun powder as igniter is that it is not very
efficient for propellants which have low structural integrity and require low
critical pressure for steady state of combustion.
A pyrotechnic composition usually contains a small percentage of binder which
may be of natural origin or man made organic polymer, which holds fuel (metal)
and oxidiser components in homogenous blend. Some other pyrotechnic
compositions with metal powders such as AI, Mg, B as fuel as KNOa as oxidiser,
with or without binder have also been used as igniter for the propellants.
However, disadvantage of using these pyrotechnic compositions without binder
is that on storage the ingredients of constituent composition are likely to
segregate.
Another disadvantage of using these pyrotechnic compositions without binder is
that the composition becomes sensitive to mechanical impulse.
Yet another disadvantage of using these pyrotechnic compositions without
binder is that the composition is susceptible to ingress of moisture which affects
the final performance.
Still another disadvantage of using these
pyrotechnic compositions without binder is that the
composition does not have pelleting property and thus are?
Further disadvantage <.rf using these pyrotechnic> compositions without binder is th.it the composition does not;
give reproducible and reliable results.
Still further disadvantage of using these
pyrotechnic compositions without: binder is that such
composi t ions do not have high coiftpressive? strength.
The disadvantage of using pyrotechnic composition
with organic polymer binder v.i,:'. Ethyl cellulose without
plastic isation,, the composition is prone to oxidation in
presence of light and temperature above the softening point
i1 5uP C ) .
Another disadvantage of using pyrotechnic
composition with ethyl eellulose without piasticisation, as
hinder is that on storage the composit.ion deteriorates and
pellet becomes brittle in nature.
OBJECTS. OF THE INVENT; I OH
The primary object. of the present invention is to
pi-" o pose a magnesium based pyrotechnic composition for energy
r .i c.! "i p i- o pe 1 3 a n t s „
Another object of the present invention is io
propose a magnesium based pyrotechnic: composition which is
stable,.
Still another object of the present invention is
to propose a magnesium based pyrotechnic composition which
gives reproducible per f or mane e.,
Yet another object of the present invention i.B propose a magnesium based pyrotechnic: compos;, i. tion with
iii.i i i i mum iqn :i 1: i on de lay .
Still another object of the present invention is
to propose a magnesium based pyrotechnic composition' with
BU -f '(ic i 01111 y 1 Diio s>"iel f 1 i f e.
F'urtf'ier object of the present invention is to
propose a formulation of magnesium based pyrotechnic
composition that gives desired i (.in it ion to various classes erf
p i'" o pel J a n * s .•
: 5 :
DESCRIPTION OF INVENTION
According to this invention there is provided a pyrotechnic composition
for energy rich propellant, comprising: -
(a) magnesium powder as metal fuel and present in the amount
of 22 to 50% by weight preferably 37 to 47% by weight,
(b) potassium nitrate as an oxidizer and present in an amount
of 70 to 42% by weight preferably 55 to 45% by weight, and
(c) the remaining is 8 to 10% of binder as a solution of
plasticised ethyl cellulose (PEC) in toluene.
Further according to this invention there is provided a process for
the preparation of pyrotechnic composition for energy rich propellant
which comprises iri the steps of:-
a) preparing a mixture of 22 to 50% by weight of magnesium powder
with purity higher than 95% and 70 to 42% by weight of potassium
nitrate,
b) mixing 8 to 10% PEC solution with a mixture of magnesium powder
and potassium nitrate.
In accordance with the present invention, the preparation of magnesium
based pyrotechnic composition comprises of the steps of:-
a) Preparation of Plasticised Ethyl Cellulose
Plasticised ethyl cellulose (PEC) is prepared by plasticisation of ethyl
cellulose with diethyl phthalate taking 70 to 80% preferably 75 to 77.5%
by weight of ethyl cellulose and 30 to 20% preferably 25 to 22.5% by
weight of diethyl phthalate.
\-s.).. PO£P.$.r£\t-:.i.9.Q. P'f sp-ky.^iMl P...'.f '::\Li'"Lt.i.<:li ethyl cellulose> 8% to 10X solution of dried plasticised ethyl cells.! lose
(PEC) is prepared by dissolving PEC in toluene in a suitable
vessel with constant stirring to get uniform solution.
Lty.!l§:. P...1. !j^an.!§.§i.y.fij and E^fca£.E:.i.y.m. Nitrate
Powders
22 to 50X preferably 37 to 47X by weight of magnesium powder
(Gr.V) with purity higher than 95% is mixed with 70 to 42%
preferably 55 to 45% by weight of potassium nitrate?. The
mixture? is sieved 3-4 times to get homogeneity »
IT.!..).. t!.i.>ii.D.fl. 9.T.. !'l§S.O.S?.§i.y.ffl. §nd P.ota.sBiu.jji Q.i.t.r;ate. powder mijjjture
w i t h Pj::C; so 1 u.t i on
The compoB.it ion of the present invention is prepared by
m.ixinq around 50% of PEC solution with the mixture? of
magnesium powder and potassium nitrate as prepared above.
The remaining 50% PEC solution is poured over mix and i.s
throughly mixed to get homogenous mix. This mix is allowed to
become semi ..... solid which is then granulated by passina through
:.' sieve. These granu'les ca e dried in a watef jacketed oven
at 60-i-f' 't for about 2 to 6 hour's to reduce to volatile matter
to around .1.%..
The invention w:i 1 1 now be illustrated with an example winch
is if (tended to illustrate the working of the invention and is
no! .-; 1 1 ' ended to be taken respei trively to imply an 1'inv* l a l ion
fH'i tlje scope of the present ii > /ention .
-7-
Example 1
The plasticised ethyl cellulose (PEC) was prepared by 29% plasticisation of
ethyl cellulose N-200 with diethyl phthalate. A 10 % solution of dried plasticised ethyl
cellulose was prepared using 40g of dried plasticised ethyl cellulose and 400 cm3 of
distilled toluene as solvent in a suitable vesel wth constant stirring to get uniform
solution.
l10.0g of magnesium powder Gr.V with purity more than 95% & 350.0g of
potassium nitrate with particle size between 90 & 53 micrometer were weighed
accurately and mixed on a wax paper using hom spatula. This mix was then sieved 3
times through 600 micrometer sieve for better mixing. In a mixing vessel 50% of
plasticised ethyl cellulose (PEC) solution was taken in which the above mix of
magnesium & potassium nitrate was added carefully avoiding the spillage of material.
The remaining 50% of PEC solution was poured over mix and was thoroughly mixed
using horn spatula to get homogeneous mix.
The mix was poured on conducting polythene sheet kept in a tray and allowed
to become semisolid. The semisolid mass/dough was then granulated by passing
through 25 BSS (600 micrometer) sieve. The sieved granules were then retained on
52 BSS (300 micrometer) sieve and retained material was dried in water jacketed oven
at 60 ± 5° C for 2 to 6 hours to reduce the volatile matter to granules were used for characterisation. The qualified granules were used for making
pellets in a pelleting machine using appropriate die & punches. The pellets are used for
further tests.
Example No 2 to 7
In these examples the procedure for preparation is identical to that of example
1 except that magnesium was increased from 27 to 50% while Potassium Nitrate was
reduced from 65 to 42% keeping binder (PEC) constant at 8% by weight. These
formulations are given in Table 1
TABLE - 1
Magnesium Based Pyrotechnic Compositions Results
Exam
-pie
1
: 2
3
4
5
6
7
Percentage
Composition
Mg KNO3
22
27
32
37
42
47
50
70
65
60
55
50
45
42
Cal-val
cal/g
1607
1831
1928
2047
2008
1970
1897
Height of 50%
explosions
cm.
68
52
45
42
71
70
73
Ignition
temp
°C
510
517
479
490
536
479
477
Pressure
Maximum
(kg/cm2)
44.2
48.3
55.2
55.4
59.3
58.4
56.3
Ignition
delay
(ms)
350
34
24
19
16
18
16
-8-
The ignition temperature evaluated by Micro DTA for all the
examples were found to be in the range from 477°C to 536°C.
The formulated compositions referred at example 1 to 7 were
evaluated at loading density 0.01 g/cc in simple closed vessel (free
volume 700 cc) designed for this purpose. For initiation, these
igniter compositions were initiated smoothly by an electric squib.
The results are given in Table 1. Except the composition in
example 1, all other compositions gave satisfactory pressure-time
(p-t) profile with low ignition delay.
The binder plasticised Ethyl cellulose (8% by weight) gave
satisfactory structural integrity to the granules of the composition.
The composition could be pelleted in different sizes giving pellet
densities in the range of 1.40 to 1.78 g/cm3. The breaking strength
for these pellets was found in the range of 200-250N. The
structural integrity as well as the ballistic performance of these
compositions were found to be satisfactory even five years after
manufacture.
The composition of example 5, using 42% of Mg and 50% of KNO3
was successfully used for ignition of composite and composite
modified double based propellants which delivered smooth p-t
(pressure-time) profile with minimum ignition delay. This
composition is safe to handle, manufacture, pelleting and for
transportation, with the precautions necessary for handling
pyrotechnic compositions.
It is to be understood that the process of the present invention is
susceptible to modifications, adaptations, changes by those skilled
in art. Such modifications, adaptations, changes are intended to be
within the scope of the present invention, which is further set forth
under the following claims:-
The ingredient are not chemically in acting but gives synergetic
properties i.e. properties of the end product are synergetic.
I CLAIM;
1. A pyrotechnic composition for energy rich propellant, comprising:-
(a) magnesium powder as metal fuel and present in the amount
of 22 to 50% by weight preferably 37 to 47% by weight,
(b) potassium nitrate as an oxidizer and present in an amount
of 70 to 42% by weight preferably 55 to 45% by weight, and
(c) the remaining is 8 to 10% of binder as a solution of
plasticised ethyl cellulose (PEC) in toluene.
2. A process for the preparation of pyrotechnic composition for energy
rich propellant which comprises in the steps of:-
a) preparing a mixture of 22 to 50% by weight of magnesium powder
with purity higher than 95% and 70 to 42% by weight of potassium
nitrate,
b) mixing 8 to 10% PEC solution with a mixture of magnesium powder
and potassium nitrate.

3. A magnesium based pyrotechnic composition for energy rich
composite propellants as substantially described herein.
4. A process for preparation of a pyrotechnic composition
substantially as herein described and illustrated in the example.




Documents:

936-del-2000-abstract.pdf

936-del-2000-claims.pdf

936-del-2000-correspondence-others.pdf

936-del-2000-correspondence-po.pdf

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

936-del-2000-form-1.pdf

936-del-2000-form-19.pdf

936-del-2000-form-2.pdf

936-del-2000-form-3.pdf

936-del-2000-gpa.pdf


Patent Number 231074
Indian Patent Application Number 936/DEL/2000
PG Journal Number 13/2009
Publication Date 27-Mar-2009
Grant Date 28-Feb-2009
Date of Filing 16-Oct-2000
Name of Patentee THE ADVISER
Applicant Address DEFENCE RESEARCH AND DEVELOPMENT ORGANISATION, MINISTRY OF DEFENCE, GOVT OF INDIA, B-148, SENA BHAWAN, DHQ P. O., NEW DELHI-110011
Inventors:
# Inventor's Name Inventor's Address
1 PUNDLIK BABAN GHULE HIGH ENERGY MATERIAL RESEARCH LABORATORY, SUTARWADI, PUNE 411021.
2 HARISH JOIATAIRAM GANDHI HIGH ENERGY MATERIAL RESEARCH LABORATORY, SUTARWADI, PUNE 411021.
3 SHREERAM KESHAV SABNIS HIGH ENERGY MATERIAL RESEARCH LABORATORY, SUTARWADI, PUNE 411021.
4 VARSHA SANJEEV BHINGARKAR HIGH ENERGY MATERIAL RESEARCH LABORATORY, SUTARWADI, PUNE 411021.
PCT International Classification Number C06B 27/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA