Title of Invention

"POLYURETHANE BASED INHIBITION SYSTEM FOR NITRAMINE EXTRUDED DOUBLE BASE PROPELLANTS FOR REDUCED SMOKE APPLICATION AND PROCESS FOR PREPARATION THEREOF"

Abstract The present invention relates to an inhibitor formulation for nitramine extruded double base propellants and the preparation thereof and also discloses a chemical coating compound for nitramine double base propellants and its preparation; further, the present invention reveals a system comprising inhibitor formulation and chemical coating compound.
Full Text Field of Invention
This invention relates to an inhibition system for nitramine extruded double base
propellants and a process for preparation thereof wherein inhibition system
comprises of inhibitor composition and a formulation for chemical coating for
nitramine containing extruded double base propellants with low signature
features.
Background and prior arts
To achieve a definite pattern of propellant burning polymeric materials are applied on surface of propellant. Nitramine propellant is a low signature propellant. For low signature application of missile, apart from propellant, the inhibitors too are required to have minimum smoke/solid particles in rocket exhaust. Release of smoke/solid particles in exhaust reveals the launch location of the missile and in the case of optically guided missiles, the smoke masks the radiation coming from missile leading to the loss of control of the missile. Nitramine extruded double base (EDB) propellants basically comprise of nitrocellulose, nitroglycerine and nitramine such as cyclotrimethyl trinitramine (RDX) as high-energy materials in addition to other additives.
There are number of inhibition systems known in the art for double base propellants. However, a few inhibitor materials are known in the art for nitramine based propellants, however with following disadvantages.
Inhibition formulations for nitramine based cast composite modified double base propellants known in the art are based on hydroxy- terminated polybutadiene (HTPB), di-isocyanates, carbon black, antimony trioxide etc.
The above inhibition systems known in the art have the disadvantage of producing high smoke density and hence are not suitable for propellants selected for low signature application.
Inhibition formulation for nitramine containing extruded double base propellants having low signature feature is not known in prior art.
Objects of the present invention
The primary object of the present invention is to provide a polyurethane based inhibition system as a combination of an inhibitor composition and a formulation for chemical coating to nitramine based extruded double base (EDB) propellant, which exhibits extreme temperature operational capability.
Another object of the invention is to provide a polyurethane based inhibition system with low smoke level for nitramine EDB propellant.
Still another object of the invention is to provide a polyurethane based inhibition system, which has good mechanical properties for nitramine EDB propellant.
Yet another object of the present invention is to provide a polyurethane based inhibition system suitable for machining to achieve desired shape and configuration.
Still another object of the present invention is to provide polyurethane based inhibition system for Nitramine EDB propellant, which exhibits extreme temperature operational capability from -30°C to +55°C.
Yet another object of the present invention is to provide a formulation for chemical coating for nitramine EDB propellants, which minimizes plasticizer migration from propellant to inhibitor.
Yet further object of the present invention is to provide a polyurethane based inhibition formulation and a chemical coating for nitramine EDB propellants which has shelf life of a minimum of 8 years.
Statement of the Invention
Accordingly, the present invention relates to an inhibitor formulation for nitramine extruded double based propellant comprises polyether polyol, aliphatic di-isocyanate, melamine and ferric acetyl acetonate.
Summary of the invention
In view of the low signature application, present invention consists of inhibitor formulation and chemical coating for nitramine extruded double base propellants, which yields low smoke and withstands extreme environmental test conditions. The formulation uses polyether polyol as resin, isophorone di-isocyanate (IPDI) as curative and melamine as filler. A curing catalyst viz. ferric acetyl acetonate (FeAA) is used. The propellant on which this inhibitor formulation is to be applied is coated with an adduct of 1,2,6 - hexanetriol (HT) and hexamethylene di-isocyanate (HMDI). This adduct formulation substantially minimizes plasticizer, migration between propellant and inhibitor and improves the shelf life of inhibited propellants.
Brief description of figures
Figure 1: FTIR spectral graph of hexane triol (HT)
Figure 2: FTIR spectral graph of hexamethylene di-isocyante (HMDI)
Figure 3: FTIR spectral graph of HT-HMDI adduct [chemical coating compound]
Brief description of Table
Table 1: Characteristic of inhibitor formulation
Detailed description of the present invention
According to present invention relates to an inhibitor formulation for nitramine extruded double based propellant comprises polyether polyol, aliphatic di-isocyanate, melamine and ferric acetyl acetonate.
Another embodiment of the present invention is a process of preparing an inhibitor formulation nitramine extruded double based propellant, said process comprising the steps:
mixing 55-60 % by weight of polyether polyol with 14-16% by weight
aliphatic di-isocyanate to obtain a mixture,
adding a filler such as herein described in the range of 20 to 30% by weight
to the mixture of step (a) under continuous stirring for a period in the
range of 15 to 20 minutes to obtain reaction mixture,
adding ferric acetyl acetonate in the range of 0.005 to 0.01% by weight to
the reaction mixture of step (b) under constant stirring and subsequently
de-aerating the same to obtain inhibitor formulation. Still in another embodiment of the present invention the polyether polyol has viscosity in the range of 1000 to 1200 centi poise.
Yet in another embodiment of the present invention the polyether polyol has functionality in the range of 3.0 and 3.5 and hydroxyl value in the range of 130 to 140 mg KOH/g.
Further in another embodiment of the present invention the aliphatic di-isocyanate is having purity at least 98%.
Still in another embodiment of the present invention the aliphatic di-isocyanate is isophorone di-isocyanate.
One more embodiment of the present invention is a chemical coating compound for nitramine extruded double based propellant represented by formula 1.
(Formula Removed)
Further, in another embodiment of the present invention is a process for preparing chemical coating formulation for nitramine double based propellant, said process comprising reacting hexane-ol in the range of 3.8 to 5% by weight with aliphatic di-isocyante in the range of 14.2 to 18.5% by weight in a solvent in the presence of catalyst such as herein described in the range of 0.02 to 0.03% by weight for a period in the range of 2 to 3 hours to obtain the chemical coating compound of formula 1.
Yet in another embodiment of the present invention the hexane-ol is 1,2, 6-hexane triol (HT).
Still in another embodiment of the present invention the aliphatic di-isocyanate is hexamethylene di-isocyanate (HMDI).
Still in another embodiment of the present invention the solvent is dichloro methane.
One more embodiment of the present invention the catalyst is selected from a group comprising organo-tin compound.
Yet in another embodiment of the present invention the organo-tin compound is dibutyl tin dilaurate (DBTDL).
Still in another embodiment of the present invention is an inhibition system for
nitramine extruded double base propellants, said system comprising inhibitor
formulation of claim 1 and chemical coating formulation represented by formula
1.
Still another embodiment of the present invention the inhibition system based on
polyurethane for nitramine extruded double base propellants is prepared by the
process consisting of following steps:
a) Preparation of Inhibition Composition:
1. 47.6 to 71.5% of polyether polyol mixed with 12.38 to 18.56% by weight of curative preferably aliphatic di-isocyanate. Polyether polyol taken has viscosity between 1000 and 1200 cp, functionality between 3.0 and 3.5 and hydroxyl value (mg of KOH/g) between 130 and 140. Curator isophorone diisocyanate is taken with purity higher than 98%. The mixture is stirred well for about 5 minutes.
2. To the mixture of polyol and curator, 20-30% of melamine as filler is added in small fractions and stirring is continued for about 15 - 20 minutes. The mixture is de-aerated for 10-15 minutes. To the mixture 0.005- 0.01 part of ferric acetyl acetonate (FeAA) is added as a catalyst and stirring is continued for about 5 minutes. The inhibition material thus prepared is de-aerated for 5-7 minutes ( (b) Preparation of formulation of chemical coating
An adduct is prepared by mixing 25-30 parts by weight of 1, 2, 6-hexanetriol (HT) with 94-113 parts by weight of hexamethylene diisocyanate (HMDI). The reaction is carried out in dichloromethane solvent (450-550 ml) in presence of catalyst, wherein the catalyst is di-butyl tin dilaurate (DBTL) in a concentration in the range of 0.02 -0.03%.
(c) Method of application of coating and inhibition composition:
The coating of this adduct is then applied on the nitramine double base propellant and is dried at 50 ± 2°C for 2 hrs.
The adduct coated propellants thus prepared are inhibited with the inhibition formulation using Vacuum Casting Technique. The inhibited grains are then cured and machined to the required dimensions.
The invention will now be illustrated with a working example, which is intended 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:
The present invention is illustrated by the following examples, which are set forth to illustrate the present invention and are not to be construed as limiting thereof.
59.52% by weight polyether polyol is taken into mixing vessel and 15.47% by weight Isophorone di-isocyanate (IPDI) is added. The mixture is stirred well for 5-10 minutes. To the mixture of Polyol and curator 25 parts by weight of melamine is added in installments under stirring. Stirring is continued for further 15-20 minutes. The mixture is de-aerated for 10-15 minutes. Ferric acetylaetonate catalyst 0.008 part is added and mixture is stirred well for 5 minutes and de-aerated ( A coat of adduct prepared form HT and HMDI in dichloromethane is given on propellant surface and dried at 50 ± 2 °C for 2 hours. The inhibitor composition is cast over the propellant assembled in a mould under vacuum ( Cured inhibitor is also characterized for bond strength, mechanical properties, and glass transition temperature and smoke density measurement. Plasticizer migration is estimated by dipping adduct coated cured inhibitor samples in desensitized nitroglycerine (NG) for 72 hours at ambient. Shelf life of the inhibited propellant is assessed by accelerated storage trials at elevated temperature of 50 ± 2 °C. Inhibited grains were subjected to static evaluation at ambient, hot (+55°C) and cold (-30°C) conditions. P-t profiles obtained were as per prediction of desired performance. More than 95% transmission was achieved
in visible and IR region for this inhibitor formulation. Based on accelerated storage trials, minimum shelf life of 8 years was assigned for inhibited propellants.
Table 1 (Table Removed) It is to be understood that the process of present invention is susceptible to changes, adaptations and modifications by those skilled in the art. Such changes, adaptations and modifications are intended to be within the scope of the present invention, which is further set forth under the following claims.





We claim:
1. An inhibitor formulation for nitramine extruded double based propellant comprises polyether polyol, aliphatic di-isocyanate, melamine and ferric acetyl acetonate.
2. A process of preparing an inhibitor formulation nitramine extruded double based propellant, said process comprising the steps:

a) mixing 55-60 % by weight of polyether polyol with 14-16% by weight aliphatic di-isocyanate to obtain a mixture,
b) adding a filler such as herein described in the range of 20 to 30% by weight to the mixture of step (a) under continuous stirring for a period in the range of 15 to 20 minutes to obtain reaction mixture,
c) adding ferric acetyl acetonate in the range of 0.005 to 0.01% by weight to the reaction mixture of step (b) under constant stirring and subsequently de-aerating the same to obtain inhibitor formulation.

3. A process of preparing inhibitor formulation as claimed in claim 2, wherein polyether polyol has viscosity in the range of 1000 to 1200 centi poise.
4. A process of preparing inhibitor formulation as claimed in claim 2, wherein, polyether polyol has functionality in the range of 3.0 and 3.5 and hydroxyl value in the range of 130 to 140 mg KOH/g.
5. A process of preparing inhibitor formulation as claimed in claim 2, wherein the aliphatic di-isocyanate is having purity at least 98%.
6. A process of preparing inhibitor formulation as claimed in claim 2, wherein the aliphatic di-isocyanate is isophorone di-isocyanate.
7. A chemical coating compound for nitramine extruded double based propellant represented by
Formula 1. (Formula Removed)
8. A process for preparing chemical coating formulation for nitramine double based propellant, said process comprising reacting hexane-ol in the range of 3.8 to 5% by weight with aliphatic di-isocyante in the range of 14.2 to 18.5% by weight in a solvent in the presence of catalyst such as herein described in the range of 0.02 to 0.03% by weight for a period in the range of 2 to 3 hours to obtain the chemical coating compound of formula 1.
9. A process as claimed in claim 8, wherein the hexane-ol is 1,2,6-hexane triol
(HT).
10. A process as claimed in claim 8, wherein aliphatic di-isocyanate is hexamethylene di-isocyanate (HMDI).
11. A process as claimed in claim 8, wherein the solvent is dichloro methane.
12. A process for preparing chemical coating formulation as claimed in claim 8, wherein the catalyst is selected from a group comprising organo-tin compound.
13. A process as claimed in claim 12, wherein the organo-tin compound is dibutyl tin dilaurate (DBTDL).
14. An inhibition system for nitramine extruded double base propellants, said system comprising inhibitor formulation of claim 1 and chemical coating formulation represented by formula 1.
15. An inhibitory formulation and the preparation thereof, a chemical coating formulation and the preparation thereof and an inhibition system substantially such as herein described with figures, example and foregoing description.

Documents:


Patent Number 264434
Indian Patent Application Number 2523/DEL/2005
PG Journal Number 01/2015
Publication Date 02-Jan-2015
Grant Date 29-Dec-2014
Date of Filing 16-Sep-2005
Name of Patentee DIRECTOR GENERAL, DEFENCE RESEARCH & DEVELOPMENT ORGANISATION
Applicant Address MINISTRY OF DEFENCE, GOVERNMENT OF INDIA, WEST BLOCK-VIII, WING-1, SECTOR-1, R.K.PURAM, NEW DELHI-110 066, INDIA
Inventors:
# Inventor's Name Inventor's Address
1 BHALERAO, KISAN GOPALA C/O HIGH ENERGY MATERIALS RESEARCH LABORATORY, SUTARWADI, PUNE-411 021, INDIA
2 SINGH, RAJA VASTA C/O HIGH ENERGY MATERIALS RESEARCH LABORATORY, SUTARWADI, PUNE-411 021, INDIA
3 MONDAL, AMIT KUMAR C/O HIGH ENERGY MATERIALS RESEARCH LABORATORY, SUTARWADI, PUNE-411 021, INDIA
4 DIVEKAR, PANDHARINATH KRUSHNAJI C/O HIGH ENERGY MATERIALS RESEARCH LABORATORY, SUTARWADI, PUNE-411 021, INDIA
PCT International Classification Number C06B 31/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA