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CONFIDENTiAL

%j ~COPY N O iI#r.. PICATINNY ARSENAL TEC"ItCAL REPORT NO. 3497

DEVELOPMENT OF NEW CATALYSTS

FOR THE

* BURNING RATE CONTROLOF

HIGH ENERGY SMOKELESS NITRAMINE

-DOUBLE BASE PROPELLANTS (U)

JOSEPH S. STACK

AMLMS CODE 5221.11,585 DA PROJ IA2229OIA2t

PICATINNY ARSENALDOVER, NEW JERSEY

DOWNGRtADED AT 3 YEPAf INTERVALS 16

.;I D .CLA6SIFJIED A ,- 12 YEAIS LL , . ,1 1L I)D ) DIR .1200.10 ,)

flI1NFiflFNTlAI.

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S J

1. P/

Th~e findings~in this report are not'to be construed

as an official Department of the Army position, unless 'rso designated by other authorized documents.

DJSPOSITION

In addition to security requirements which, apply tothis ,document and must be met,,eaeh transmittal out-side &h Department of Deiepase must have prior ap-proval of Propellants Laboratory, Piatinny Arsenal,Dover, New Jeisey

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CONFIDENTIAL

This document coutains informationaffecting the national defense ofthe United States within the abao-ing of the Espionage Laws, Title18, U.S.C., Section 793 . 7-94-.The transmission or the revilatioaof its contents in any manner to anunauthorized person is prohibitedby law.

Technical Report No._ 348"-1

DEVELOPMENT OF NEW CAT4 ISTAFOR THE BURNING RATE COMMO

OF HIGH EN!~SKMKLS M RMDCLE-BArs PROPEULA4 T U)

By

Joseph S. Stack

November 1966

Propellants LaboratoryPicatinny ArsenalDover, New Jersey

CONFIDENTIAL

GJONFIDEN11AL.

(C) TABLE OF CONTTATS

Abstract 1

Conclusion 2

Recommendation 3

Intreductioa 4

Results and Dircussion 6

Experimental 14

Appendix A 17

Reference 19

TABLE I Ballistic Modifier (Lead Staunate) Analysis (C) 20

TABLE II Cheical Analysis of Ballistic Modifiers 21

TABLE III Physical Properties of Ballistic Modifiers 22

TABLE .V Ballistic Modifier (Bismuth Stannate) Analysis (C) 23

f2. X-Ray Diffraction Patterns - Untreated and Heat TreatedLead Stannate (C) 24

FIGURE 2 X-Ray Diffraction. Patterns - Lead Stannate - TDI Complexes,Lead StanWate - TDI (Reduced), Lead Stannate - TDI(Oxidized) (C) 25

FIGURE 3 X-Ray Diffraction Patterns - Lead Stannate - HDI Complex,Lead Stannate - HDI (Oxidized) (C) 26

FIGURE 4 X-.Ray Diffraction Patterns - Chemical and Heat TreatedBismuth Stannate (C) 27

FIGURE 5 X-Ray Diffraction Patterns - Bismuth Stannate - HDIComplex, Bismuth Stanuate - HDI (Oxidized) (C) 28

FIGURE 6 Ballistic Properties of Smokeless HMX Plastisol PropellantsContaining Chemically (HDI) and Heat Treated Lead Stannate(C) 29

FIGURE 7 Ballistic Properties of Smokeless HMX Plastisol PropellantsContaining Chemically (HDI) and Heat Treated Lead Stannate(C) 30

CONFIDENTIAL

CONFID TIAL(C) TABLE OF CONTENTS (Ceat'd)

FIGURE 8 Ball stic Properties of Smokeless HKX Plastisel PrepellantsContaining Chemically (TDI) and Heat Tieated Biithstaxnate (C) 31

FIGURE 9 Ballistic Properties of Smokeless HKX Plastisol PropellantsContaining Chemically (HDI) and Heat Treated BismuthStanfate (C) 32

FIGURE 10 Ballistic Properties of Extruded Smokeless PropellantsContaining 54% RDX Modifiers: Lead Beta Resercylate,Cupric Salicylate (C) 33

FIGURE U Ballistic Properties of Extruded Smokeless PrepellantsContaining 56% JIX Modifiers: Lead Beta Resercylate,Cupric Salicylate (C) 34

FIGURE 12 Ballistic Properties of Extruded Smokeless PropellantsContaining 54% RDX Modifier: Lead Stanate - TDI(Reduced) (C) 35

FIGURE 13 Ballistic Properties of Extruded Smokeless PropellantsContaining 54% RDX Modifier: Lead Stannate - TDI(Oxidized) (C) 36

FIGURE 14 Ballistic Properties of Extruded Smokeless PropellantsContaining 56% HMX Modifier: Lead Stannate - TDI(Oxidized) (C) 37

FIGURE 15 Ballistic Properties of Extruded Smokeless PropellantsContaining 56% Fine HMX Modifier: Lead Stannate - TDI(Oxidized) (C) 38

FIGURE 16 Ballistic'Preperties of Extruded Smokeless PropellantsContaining 56% HMX Modifier: Lead Stannate - TDI (Reduced)(C) 39

FIGURE 17 Ballistic Properties of Extruded Smokeless PropellantsContaining 56% Fine HMX Modifier: Lead Stannate - TDI(Reduced) (C) 40

FIGURE 18 Ballistic Properties of Smokeless HMX Plastisol PrepellantsModifier: Lead Staunate as received (C) 41

FIGURE 19 Ballistic Properties of a Cross-Linked Smokeless HX Plast-isol Propellant Modifier: Lead Stannate as received (C) 42

FIGURE 20 Ballistic Properties of A Smokeless HMX Plastisel PropellantModifier: Lead Stannate - TDI (Oxidized) (C) 43

I ONFIDENTIIAL

CONFIDENTIAL(C) TABLE OF CONTENTS (Contid)

FIGURE 21 Ballistic Properties of A Smokeless HKX Plastisol PropellantModifier: Lead Stanmate - TDI (Reduced) (C)

FIGURE 22 Ballistic Properties of A Cross-Linked Smokeless HKXPlastisol Propellant Modifier: Lead Stannate - TDI(Oxidized) (C) 45

FIGURE 23 Ballistic Properties of A Cross-Linked Smokeless HKXPlastisel Propellant Modifier: Lead Stannate - TDI(Reduced) (C) 46

FIGURE 24 Effect of Changes in Ball Powder/Casting Solvent RatioUpon the Burning Rate of Smokeless HMX Plastisel PropellantsModifier: Lead Stannate - TDI (Reducid) (C) 47

FIGURE 25 Effect of Changes in Ball Powder/Casting Solvent RatiTIUpon the Burning Rate of Smokeless HMX Plastisol PropellantsModifier: Lead Stannate as received (C) 48

FIGURE 16 Effect of HMX Concentration on Pressure-TemperatureDependency of Burning of High Energy Smokeless PlastisolDouble-Base Propellants 49

FIGURE 27 Effect of Concentration of Lead Stannate - TDI ( d.. )Upon Ballistic Properties of High Energy Smokeless HMXPlastisol Propellants (C) 50

FIGURE 28 Effect of Concentration of Lead Stannate - TDI (Reduced)Upon Ballistic Properties of 'High Energy Smokeless HXPlastisol Prepellants (C) 51

FIGURE 29 Effects of Changes in Calorific Levels Upon BallisticProperties of High Energy Smokeless HMX PlastisolPropellants (0) 52

CONFIDENTIAL

Studies leading toward the development of new ccmbustion ca talsts whichare very effective in reducing the temperature and pressure dependency ofburning rate of high energy (230 - 240 lb-sec/ib) amokeless nitramlne (RDX,HNX) propellants are discussed.

Described are the methods of manufacture, proposed reactions and analyticsland X-ray diffraction data of the new cobustion catalysts.

Strand burning rate data are presented for eztraded and plaoiol (cross-linked and uncross-linked) propellants. The results show the highly effectivenature of the new ccobustion catalysts in reducing the variability of burningrate to changes in temperature and pressure of these propellant types.Propellants investigated have application for close support and other ieaponsystems where high performance and smokelessness are required.

CONFIDENTIAL. . .. . ........ . . - NO R ,

CONFM nfL

Two now combustion cataysts have been developed which are extr .tY4'effective in reducing the variability of burning rate to changes in temperatureand combustion pressure of high energy (230 - 240 lb-sec/b) nitrocellulosebased rocket propellant formulations.

The catalysts are prepared by high temperature sintering of a complex oflead stannate and 2,4 - tolylenedjisocyanate and are identified as lead staiinate

TDI (Reduced) and lead stannate - TDI (Oxidised). They appear to be initurescomprised of an ammono complex of lead or tin of unknown structure and 6xrdesof lead and tin with and without carbon and metallic lead.

These combustion catalysts have been found to induce vastly improved burningrate behavior to high energy smokeless nitraine (RDX, WiX) double-base plastisoland extruded rocket propellants. Propellants with the new combustion catilystshave displayed substantially reduced variation in burning rate to temperatures(1600F to -400F) and presse over useful pressure ranges (plateau ballisticsand low temperature coefficients).

2

CONFIDEMAL(C) RFgQ1 IoKs

It is recommended that the high energy smokeless nitramine double-bas.propellants described in this report be considered as candidate propellantsfor advanced close support systems and other applications where mokelessnessand ballistic reliability are prime requisites.

It is also recommended that research concerning the new catalyst develop-ment and their evaluation in smokeless high energy propellants be activelypersued and that the work include (1) investigations with other metalo organicand inorganic combustion catalysts employing the chemical and heat treatingtechniques described in this report and (2) other related avenues of catalystresearch.

Furthermore, it is recomended that supply sources be established for thecombustion catalysts, lead stannate - TDI (Oxidized) and lead stannate - TDI(Reduced) to meet any future anticipated demands for these catalysts inpropellant systems.

3CONFIOENA -- -

____________ __________________

S" FIlENTIAL

(C) IN'TRODUCTION

One qf the critical factors effecting solid propulsion system design andoperational reliability over a wide temperature range is the ballistic behaviorof the propellant composition. Maximum performance is obtained with propellantswhich display a minimum variation of burning rate with combustion pressure andenvironmental temperature. For these reasons, propellants are constantly beingsought which have the lowest possible burning rate vs pressure isotherm slopesand the least variation of burning rate with operational temperatures.

During the 1940's it was discovered that aliphatic le;d compounds wouldmodify the burning rate (plateau and mesa burning) of doqble-base compositions.Since that time investigations with ballistic modifiers has continued unceasinglyand the number and types of compounds has been eiepded which yield ballisticmodification in double-base propellants. Almost exclusively, metalo organo andinorganic compounds of lead with chelated derivatfves were tound to be the mosteffective combustion catalysts for these propellant.s (Rf. 1,2).

Over the past ten years, research at Picatinny Arsenal in this area hasbeen with nitramine (RDX, HMX) nitrocellulose base propeflants of high volumetricimpulse of the following types:

(a) Extruded smokeless nitramine double-base propellants.

(b) Plastisol (cast-type) smokeless nitramlne double-base propellants.

(c) Cross-linked plastisol (cast-type) smokeless ni ,amine double-base propellants.

Efforts to improve the burning rate behavior of the$* high energy propellantswith ballistic modifiers ordinarily employed in double-base systems (metaloorganic and inorganic salts) met with only limited success (Ref. 3 and 4). Themost efficient ballistic modification was obtained with solvent extruded typesystems. Plastisol (cast type) systems, which employ Fluid Ball Powder as thepolymeric binder resisted nearly all attempts at ballisbic modification. Forthis system, lead and bismuth stannate dihydrate were found to be the mosteffective combustion catalysts (Ref. 3, 5, 6, 7, 8). Cross-linked plastisol(cast type) propellants resisted all attempts toward beiog ballistically controlledwith currently known combustion catalysts.

Difficulties in effective ballistic modification of high energy smokeless

nitramine double-base propellants was not unexpected since the efficiency ofballistic modification of different propellant types 1. known to vary because ofthe many factors which can influence modifying activity° The concentration,

proportion, and types of propellant ingredients, the type of baWstip iodifierand its relative distribution in a composition, the method c!,AMfacture, andenergy, are all significant in affecting the extent of modifyig activity.

CONFIDENTIAL

GONFENTLLThe subject matter of this report covers an area of combustion catalyst

research performed at the Propellant Laboratory, Picatinny Arsenal. Describedare the studios mede toward the developaent of now combustion catalysts forcross-linked and uncross-linked high energy smokeless nitramine double-basepropellants vhich would import to these systems the desirable ballistic qualityof invariance of burning rate to changing temperabure and combustion pressureconditions.

The mropellants evaluated are considered thermally stable according toshort term heat tests at 1200 C (no defla mtion after 500 zinutes exposure) andthey exhibited reasonably good to exceptionaUy good mechanical propertiesbetween 14OF and -40oF. (Tensile strength at 1400F ranged between 30 andand 130 psi and elorations at maxmlom load at -WOF were between 20 and 60per cent.)

5

CONOR

CONFIDENTIAL(C) DISCUSSION

The results of investigations with the combustion catalysts are presentedin three parts:

1. Synthesis and evaluation of new combustion catalysts.

2. Evaluation of new combustion catalysts as ballistic modifiers insolvent extruded type high energy smokeless nitramine double-base systems andhigh energy plastisol (cast type) smokeless nitramine double-base propellants.

3. Effect of composition parameters upon ballistic properties ofplastisol type propellants containing the new combustion catalysts.

Synthesis and Evaluation of New Combustion Catalysts

The investigation was oriented about the synthesis of organo isocyanatecomplexes of lead and bismuth stannate and the determination of the effects ofheat treatment upon the complexes and also the original lead and bismuth stannates.Hydrated lead and bismuth stannate were selected as the metalo inorganic saltsin these studies because they displayed the most effective modifying activity inhigher energy plastisol type compositions in previous investigations (Ref. 3,5, 6, 7, 8).

The following thirteen modifiers were investigated: (a) lead stannatedihydrate (as received), (b) lead stannate (heated at 450 - 5000C), (c) leadstannate - TDI complex, (d) lead stannate - TDI (oxidized), (e) lead stannate -TDI (reduced), (f) lead stannate - HDI complex, (g) lead stannate - HDI (oxidized),(h) bismuth stannate dihydrate (as received), (i) bismuth stannate (heated at 450- 5000C), (J) bismuth stannate - TDI complex, (k) bismath stannate - TDI (oxidized),(1) bismuth stannate - HDI complex, (m) bismuth stannate - HDI (oxidized). Thenature of lead and bismuth stannate dihydrate and their heated counterparts areself-explanatory. The remaining modifiers were synthesized in the laboratoryaccording to Procedures I, II, and III shown in Appendix A.

Proposed reactions for formation of the lead stannate - TDI complex andoxidized and reduced forms of lead stannate - TDI complexes are indicated below:

Reactions for Formation of Modifiers

PROPOSED REACTIOt FOR FOP14ALOtI OF LEAD STAtOIAT

j3 H3 H 0NhH..CO 25 - 55C ,1. PbSnO3 .22O + b Snof . -N-C-O

HO

?bHn 3 '~~ H2. PSn3o3 PbS003

HO

CONFIDENTIAL

CONDETIAL

M. + 25 - 5SC

. 1b8 *03.cu1 3 .

PIOINOSD REACI~l 1 I O S Ir0 TIOI 0? LD STA)IFAaTp

(2-4. TOLYIBE DIISOCYANATE 0XIDIZED)Clt3

4. PbS003 + ~ 00 25 5C PS0 ..1.'0 ?bn3 20 2 0+

i Ni I 200

(2. ) Pb + PbO + SnO2 + asmonium plumbate +2C 50 :2" PO+SO 102+2H .2

-Ny-C-O

CCH1

Por in copTex of LEAD STANNATE

unknown structGure (IDI OXIDIZED)

* Tace quantities of atoiumplumbate or tin complex of

unknown structure.

CONFIDENTIAL'7

CONFIDENTIAL

IROI ORD ZACTION FoR IOIMTOK 0" WAD STAuI.TZr(2-4. TOLYM DIISo CKTAl uipUCID)

3

CHR

(No Air)

. 2bS03 + + M +2500 25C 4 +0 + 2 1C + + 20bS 3

!11 for 3 hours

CHI

CR, (No Air)

2. 2PbSnO3 + 4C + 6N3+ 21C ++4K 500 125*C 2 C02 + 2.36+ jr+ It~ofor 3 hours 21C + Pb + PbO + Sn02 + Ammonium plumbate

then cooled at or tin complex ofambient T unknown structure18 hrs

Lead Stannate(TD Reduced)

Chemical, physical, IR and X-ray diffraction analysis performed on thepotential ballistic modifiers under study are shown in Tables I thru IV andFigures 1 thru 5. Though, complete analysis are not available for all the lotsof combustion catalysts prepared in this investigation, the data shown isexpected to be typical for these types of conbustion catalysts.

The IR and x-ray diffraction data obtained indicate that heat treat-ing orcomplexing the hydrates of lead or bismuth stannate with diisocyanates did notchemically alter the composition of inorganic salts as shown in Tables I and IIand Figures 1 thru 5. However, by heat treating the diisocyanate complex ofthese salts, some changes in the composition of the basic inorganic salts (leadstannate or bismuth stannate) did occur. The chemical changes obtained variedwith the type of organic fraction comprising the complex. Heat treatment of theTDI and HDI complexes of bismuth stannate resulted in the formation of a catalystcomprised of a mixture of bismuth stannate and stannic oxide. The organic fractionof these complexes was comprised essentially of a disubstituted urea withoutisocyanate termination. When the lead stannate - TDI complex was heated in theabsence or presence of air, a chemical change occurred in the base salt resultingin the formation of catalysts comprised of lead oxide (yellow) and stannic wcide

8CONFIDENTIAL

OMFIFIAL.with and without carbon and metallic lead and an am ono complex of load or tinof unknown structure. The organic fraction of the lead stannate - TDI complexwas an isocyanate terminated disubstituted urea. On the other hand, the leadstannate - HDI complex when heat-treated did not result in a chemical changeof the inorganic salt. In the case of this complex, the organic fraction was adisubstituted urea without isocyanate termination. On the basis of these datait. appears that the presence of -C-=O in sufficient quantity in the organicfraction of a metal inorganic salt - isocyanate complex is necessary to promotebreakdown of the salt to oxides of metalb during heat treatment. The reactionin the process of heating the metalo inorganic salt - isocyanate complexes is oneof (1) reduction then (2) subsequent oxidation of the reduced product to themetal oxides. The N=OdO in the organic fraction of the complex may (a) actas a catalyst to promote the formation of a reducing medium for reduction of theinorganic fraction of the complex or (b) during heating it may decompose and/orreact with other products of decomposition and be the prime contributor of thereducing medium for the reduction of the inorganic salt.

Evaluction of New Combustion Catalysts as Ballistic Modifiers in High EnergySmokeless Nitramine Double-Base Propellants

Preliminary Studies:

The thirteen (13) combustion catalysts, namely; hydrates of lead and bismuthstannate (as received and heated at 450 - 5000 C), le-d and bismuth stannate TDIand HDI complexes, lead and bismuth stannate - TDI &. HDI (oxidized) and leadstannate - TDI (reduced), were evaluated initially for their effectiveness aspotential ballistic modifiers in high energy smokeless HMX plastisol propellants.The results of strand burning rate studies, shown in Figures 6 thru 9, indicatethat only two of the combustion catalysts, lead stannate - TDI (oxidized) and leadstannate - TDI (reduced) were highly effective in reducing the dependency ofburning rate with pressure for the uncross-linked HMX plastisol propellants. Theremaining combustion catalysts exhibited "straight line" ballistics which borderedbetween being the minimum acceptable to non-acceptable in quality.

In view of the encouraging burning rate results obtained with the systemsmodified with lead stannate - TDI (oxidized) and (reduced), a more extensiveevaluation was made with these combustion catalysts in high energy smokelessextruded and cross-linked and uncross-linked plastisol (cast type) nitraminedouble-base propellants.

High Energy Extruded Smokeless Nitramine Double-Base Propellants

Of the three types of high energy propellants considered for investigation,the extruded type was chosen for initial scale-up evaluation of the new combustioncatalysts. With this propellant type (prepared by solvent or solvent-solventlessmethods), intimate distribution of the catalyst could be realized in thepropellant matrix. Consequently, any ballistic information generated with thesesystems would, to a great extent, indicate maximum ballistic activity impartedby these catalysts in high energy systems.

9CONFIDENTIAL

COINRElAL

Two versions of solvent extruded propellants were utilized in thesestudies, containing 54% and 56% RDX and HMX respectively. Previous ballisticresults with these systems with a combination of cupric salicylate and leadbeta resorcyate as modifiers is shown in Figures 10 and 3.1. Pressure exponentsexhibited by these systems were 0.48 (530 - 2000 psi) respectively at 70OF andtemperature coefficients of pressure at 1000 psi (p/r of 2500 and 2700) of0.16 and 0.44 between 160 and -40OF. The ballistic properties of these systemswere considered the maximu activity that can be realized with currently knownmodifiers. These data point out the inability of usual double-base combustioncatalysts to effectively control the ballistics of high energy smokeless nitraminedouble-base propellants.

In the evaluation of the new c(mbustion catalysts, a direct substitutionwas made for the original modifiers employed in the propellants. The RDX system,modified wlth lead stannate - TDI (oxidized) and lead stannate - TDI (reduced),showed a vast reduction in the temperature dependency of burning rate withpressure. The data, shown in Figures 12 and 13, indicate that of the two catalysts,the reduced form of lead stannate - TDI complex was the most effective combustioncatalyst. In addition to increasing the burning rate of the propellant, plateauballistics were indicated. A burning rate isotherm slope at 70°F of 0.00 (800 -1200 psi),, and a temperature coefficient of pressure of 0.02%/OF (1000L psi,P/r 2080)'between 160 and -40°F was obtained. The system with the bxidized formof lead stannate - TDI complex had a pressure exponent of 0.40 (100 - 1700 psi)at 70°F and a temperature coefficient of pressure of 0.045%/OF (1000 psi, P/r2500) between 160 and -400F.

Next, an evaluation was made of the combustion catalysts in 56% HMXcompositions containing a bimodal distribution of filler (75% 180u and 25% 2u)and all fine HNX of 2u average particle size. Strand burning rate data forthese systems, shown in Figures 14 thru 17, indicate that both the combustioncatalysts, lead stannate - TDI (oxidized) and lead. stannate - TDI (reduced),were highly effective in improving the ballistic properties of these propellants.In comparing the strand burning rate data, the systems with fine particle sizeH4X exhibited lower pressure exponents and lower temperature coefficients ofpressure than similar propellants containing a bimodal distribution of HX.

The data presented thus far show the effectiveness of the new combustioncatalysts lead stannate - TDI (oxidized) and lead stannate - TDI (reduced) asballistic modifiers for extruded type high energy sMokeless RDX and HIX containingdouble-base propellants with calorific levels of 1137 - 1148 cal/g and specificinpulses of 230 + lb-sec/lbo

High Enery Plastisol (Cast Type) Smokeless Nitr&VW,'l f e-Base Propellants

The plastisol propellants evaluated are of the pourable case bondedsmokeless nitramine double-base type. From a composition standpoint, the basic

difference between this propellant type and the ektruded version is the physicalappearance of the nitrocellulose binder in finished Propellants. This variation

CONFIDENI .

in the appearance of the binder results from differences in (1) the startingbinder materials (nitrocellulose) and (2) methods of manufacture. The extruded typesystems employ nitrocellulose of fibrous character. During manufacture, by either-solvent or solventleas techniques, it is well worked and efficiently colloided bysolvents resulting in a binder completely homogeneous in appearance. Also,because of the nature of the mixing techniques employed to manufacture thesepropellants, (prepared in horizontal sigma blade mixer) very thorough distributionof propellant additives can be realized within a propellant matrix.

The plastisol systems, on the other hand, employ as a binder material FluidBall Powder which is a regenerated form of nitrocellulose of 7 to 20 microns indiameter. The compositions of the Fluid Powder can vary from basically allnitrocellulose to a variety of liquid nitrate ester-nitrocellulose combinations.This latter type was employed as the binder ingredient in the systems reported.Plastisol propellants, because of their high fluidity are more conveniently preparedin vertical mixer types. This type of mixing provides good suspension of thepropellant ingredients but does not macerate sufficiently for efficient colloidingof the Fluid Ball Powder binder material. Actually, with these systems, colloidingoccurs between the high energy plasticizer and Fluid Ball Powder principallyduring the propellant cure cycle. Therefore, thorough distribution of thesolvated or colloided portion of the fluid ball powder throughout the propellantmatrix is inhibited. Because of these characteristics, ballistic modification ofthese systems becomes more difficult.

Cross-linking of plastisol type propellants complicafet allistic modificationeven further, Cross-linking is desired because of its ability to improvepropellant mechanical properties. However, in many cases, during the 6ross-linking process side reactions occur between diisocyanate cross-linkers andmetalo-organic and inorganic compounds. These interactions diminish the effect-iveaness of ballistic modifiers in these systems. Typical burning rate data foruncrosslinked and cross-linked high energy smokeless HMX plastisol propellantscatalyzed with lead stannate (as received) are shown in Figures 18 and 19. Forthe uncrosslinked system, straight line ballistics are indicated with a pressureexponent, "n", at 70OF of 0.40 (1000 to 1800 psi) and temperature coefficient ofpressure of 023%/OF at 1000 psi (P/r 2500) between 160 and -400F. The burningrate data for the oross-linked propellant shows a decided degradation ofballistic properties over the uncrosslinked system. Straight line ballisticsare indicated with a pressure exponent, "n", at 70°F of 0.61 (400 - 3000 psi)and temperature coefficient of pressure of 044%/OF at 1000 psi and P/r 3330between 160 and -400 F.

The highly effective modifying qualities exhibited by lead stannate - TDI(oxidized) and lead stannate - TDI (reduced) in uncrosslinked plastisol typesystems are shown in Figure 6. The results of more intensive studies with thesecatalysts in cross-linked and uncrosslinked formulations with 30% HMX are shownin Figures 20 through 23, The unerosslinked systems exhibited pressure rangeswhere burning rates were nearly independent of changes in pressure and temperature(Figures 20 and 21.)o Lead stannate - TDI (oxidized) and lead stannate - TDI(reduced) induced pressure exponents, "n" of 0°06 and 0.00 (800 - 1600 psi)

CONFIDENTIALII

____ ___ ___ ___ ____ ____ ____ __

at 70OF and temperature coefficients of pressure of 0.11 and 0.07%/OF at1000 psi (P/r 2325 and 2270) between 160 and -40OF respectively. The cross-linked-ystems, shown in Figures 22 and 23 also exhibited very favorable ballistics.Lead tiiate - TDI (oxidized) and lead staunate - TDI (reduced) induced pressureexponents, "n", of 0.16 and 0.10 (1000 - 1800 psi)*at 700 F anid temperaturecoefficients of pressure at 1000 psi of 0.14 and 0.22%/OF (P/r 2200 and 2500)between 160 and -40OF respectively. Improvements in the ballistic properties ofthe cross-linked formulations were not as good as that obtained with the uncross-linked systems. However, compared to the previous ballistic properties of cross-linked compositions, the new catalysts contribute substantial improvements inburning rate control.

Effect of Composition Parameters Upon Ballistic Properties of Plastisol TypePropellants

The following parameters were investigated: changes in (1) Fluid BanPowder/casting solvent ratio, (2) concentration of HEX, (3) concentration ofcombustion catalyst and (4) propellant calorific level. The burning rate resultsobtained in these studies are shown in Figures 24 to 29 and can be summarized asfollows:

Fluid Ball Powder/Casting Solvent Ratio

The burning rates at 1000 psi of high energy smokeless HMX plastisolpropellants containing lead stannate - TDI (reduced) can be varied by modifyingthe powder/solvent ratio (Figure 24). A 25% increase in burning rate (0.40'to 0.50 in/sec, at 70TF and 1000 psi) is reflected in the propellants with achange in powder/solvent ratio from 0.27 to 0.67. Previously the burning ratesof these propellants were essentially invarient to changes in powder solvent ratio(Figure 25).

HMX Concentration

The extent of temperature dependency of burning rate with pressure of highenergy smokeless HMX plastisol propellants containing lead stannate - TPI(reduced) is a function of concentration of HHX (Figure 26). As the concentrationof HMX in the propellants is increased, from 0 to 5 percent in 5 percentincrements, the burning rates become more independent to variations in temperatureand pressure. "Straight line" bk.istics are exhibited with the systems containing0 to 25 percent HMX, "plateau" ballistics at approximately 30 percent HWX and"mesa" ballistics at concentrations of HMX greater than 30 percent.

Combustion Catalyst Concentration

The mini* concentration for effective catalysis 6f the smokeless propellantsis approximately 2.0 percent of combustion catalysts lead stannate - TDI (oxidized)or lead stannate - TDI (reduced) (Figures 27 and 28). At 2.0% catalyst concen-tration, these systems exhibited pressure exponents at 70°F of 0.17 and 0.09 overpressure ranges of 700 to 1700 psi and 600 - 1350 psi respectively.

12

:OEIENIA

(C) EXPERDEWAL PROCEDURE

General

In the laboratory, one pound batches of propl)ants were prepared in theBaker Perkins (one pint capacity) vertical sigma bMdo mixer. The propellantswere mixed under a vacuum of 2 to ItoM Hg for approxImtel3 one hour. Thepropellant is cast into appropriate molds and cured at 600C for three days.Strand burning rate data was obtained by means of a Crawford Type 3trand rner.

Laboratory Procedure for Preparation of Cross-Linked and Uncrosslinked SmokelessNitramine Containing Plastisol Propellants

1. To casting solvent add resorcinol., if required, and Type B Fluid BallPowder and let stand overnight at 700F.

2. Add mixture in (1) to mixer.

3. Add HMX, modifier, "quick-gel" (Type C Fluid Ball Powder), and 2,4-tolylene diisocyanate, if required, with mixing between additionls.

4. Mix at a speed of 36 rpm for approximately one hour at 25 - 300 C anda vacuum of 2-4mm Hg.

5. Cast at a viscosity of approximately 40O000 cps and cure at 600 C forthree days. (Viscosity measured with Brookfield Viscometer - Spindle 6 andSetting 10).

Laboratory Procedure for Preparation of Extruded Smokeless Nitramine ContainingDouble-Base Propellants

The propellants are made according to small arms techniques. Mixing isperformed in a horizontal Baker Perkins Sigma Blade Mixer and the Propellantssolvent extruded and air dried.

13c FlDEITIAL

SNFDEN1AL

Materials

a. Fluid Ball Powders, Type B Lot 14528-30 and Type C Lot 2161Supplied by Olin Mathieson Chemical CorporationAverage particle size of Ball Powder Lot 14528-30, 7 micronsDetermined by Optical Count Method

Composition of Fluid Ball Powders Lot 14528-30 Lot 2161

Nitrocellulose, 12.6%N, % 90.0 74.0Nitroglycerin, % 8.0 24.02-nitrodiphemylamine, % 2.0 2.0Dioctylphthalate, added, % 0.2 0.1Carbon Black, added, % 0.3 -

b. 'Casting Solvent "IX" (High Energy Plasticizer)Prepared at Picatimy ArsenalTriethyleneglycoldinitrate supplied by Prope-lex & HerculesPowder Co.

Butanetrioltrinitrate supplied by Amcel Propulsion Co.

Composition of Casting Solvent "X"

Triethyleneglycoldiitrate 65.0Butanetrioltrinitrate 34.02-nitrodiphexylamie 1.0

c. HMX (cyclotetramethylenetetranitramine)Class E and Class AAverage particle size, 2 microns and 180 microns respectivelyDetermined by Optical Count MethodSupplied by Holston Ordnance Works

d. RDX (cyclotrimethylenetrinitramine)Class EAverage particle size, 14 micronsSupplied by Holston Ordnance Works

e. NitroglycerinSupplied by Picatinny Arsenal

f. Nitrocellulose, 12.6%NSupplied by DuPont deNemours Inc.

14

CONFIDENTIAL

CONFIDENTIAL

g. TDI (2,4-tolylene diisocyanate)Supplied by Eastman Organic Chemical Company

h. Lead stannate (Lot P 10707)Supplied by National Lead Co.

i. Lead stannate - TDI ComplexPrepared at Picatinny Arsenal according to Procedure I outlinedin Appendix A of this report

j.: Lead stannate - TDI (Oxidized)Prepared at Picatinny Arsenal according to Procedure IIoutlined in Appendix A of this report

k. Lead Stannate - TDI (Reduced)Prepared at Picatinny Arsenal according to Procedure IIIoutlined in Appendix A of this report

1. Lead stannate - Hexamethylene diisocyauate ComplexPrepared at Picatinny Arsenal according to Procedure Ioutlined in Appendix A of this report

m. Lead stannate - HDI (Oxidized)Prepared at Picatinny Arsenal according to Procedure IIoutlined in Appendix A of this report

n. Bismuth stannate - TDI ComplexPrepared at Picatinny Arsenal according to Procedure Ioutlined in Appendix A of this report

o. Bismuth stannate - TDI (Oxidized)Prepared at Picatinny Arsenal according to Procedure IIoutlined in Appendix A of this report

p. Bismuth stannate - HDI ComplexPrepared at Picatinny Arsenal according to Procedure Ioutlined in Appendix A of this report

15

CONFIDENTIAL

PONFIDENTIALI

q. Bismuth stamate - HDI (~Cidized)Prepared at Picatinny Arsenal according to Procedure IIoutlined in Appendix A of this report

r. Bismuth stannate

Supplied by Metal Thermite CorporationI

s. Cupric s&Uicylate and lead beta resorcylate

Supplied byOit*al Lead Co.

t. Carbolac, carbon black, resorcinol, 2-nitrodiphenylamine, andtriacetin are items used without purification

NOTE: The citation of trade names or manufacturers does notconstiture an official endorsement or approval of their use.

16

OONFIDENTIAL

(C) APPENDIX A

Procedure I

Premration of Lead and Bismuth StaMnte Complexes of 2.4-tolylene diisocyanateand• B ma"hlene diisocranate .

1. Add hydrate of lead or bismuth stannate to an excess of 2,4-tolylenediisocyanate or hexamethylene diisocyanate in increments while mass is agitating.

2. Mix for one hour at 25 to 550C.

3. Filter and wash filtercake once with acetone.

4. Place filtercake in suitable container, add acetone and agitate for10 minutes and filter.

5. Repeat step (4) three or four times.

6. Dry Filter cake for three hours at 1000C.

NOTE: Organic matter as determined by sintering a sample of the complex from (6)in air at 450 - 500C for one hour was as follows: lead stannate - TDI complex,17-25%; lead stannate - HDI complex, 11.6%; bismuth stannate - TDI complex, 9.3%;bismuth stannate - HDI complex, 15.3%.

Procedure II

Preparation of Lead and Bismuth Stannate - TDI and HDI (Oxidized).

1. Place lead or bismuth stannate-isocyanate complex (obtained in procedureI, step 6) in a suitable container and heat at 450 - 5000C in a muffle furnacewith door ajar until deomposition is complete (Decomposition is complete whensmoking ceases). Decomposition should not be accompanied by flame.

2. Remove the sintered product in (1) from the muffle furnace and turn themass over to permit underlying material to be near completely oxidized.

3. Place the semi-oxidized product from (2) in muffle furnace and heat forone hour at 450 - 5000C.

4. Remove from muffle furnace, cool at ambient temperature, then screen theoxidized combustion catalysts through a 400 mesh sieve.

Procedure III

Preparation of Lead Stannate - TDI (Reduced)

1. Place lead stannate - TDI complex (obtained in Procedure I, step 6)in a suitable vented vessel (container covered with aluminum foil with slits

CONFIDN AL1.7,

on top was found workable) and heat esentiall in the absence of air at 450 -5000C in a .. fflo furnace with door ajar until molking ceoase. Docc-uMsitionshould not be acccpanied br flam.

2. immediately after decomposition is cmplot (nmoking ceas), "closeTent on vessel containing modifier and heat at 500C + 250C in the absence ofair for approximately two hours. (Covering container containing modifier withalminum fail was found suitable).

3. After heoing is completed, remove covered container with lead stannate- TDI (Reduced) fzo muffle furnace and let .cool overnight at. ,abient tempe rture.

4. Screen lead stannate - TDI (Reduced) through 400 mesh- sieve.

A4

8

=.4

?*

(C) REFNCES

1. Robert P. Baumann, "Investigation of Ballistic Modifiers for High EnergySolid Rocket Propellants", Ptan Research Laboratories, Picatinny Arsenal,Technical Note No. FRL-TN-32, dated January 1961. (C)

2. Robert P. Baumann, "Investigation of Ballistic Modifiers for High EnergySolid Rocket Propellants", Iltman Research Laboratories, Picatinny Arsenal,Technical Note No. FRL-TN-127, dated February 1962. (C)

3. Robert P. Baumam, "High Volumetric Imulse Smokeless Rocket Propellants.Part I:" r Preliminary Investigation of HMX Cast Propellant (Plastisol),Feltman Research Laboratories, Picatinny Arsenal, Technical Report 2601,dated March 1959. (C)

4. William G. Clark and Edward Costa, "High Volumetric Impulse SmokelessRocket Propellants. Part II: Develorient of Solventless - ExtrudedTriple-Base Propellants", Feltman Research Laboratories, Picatinny Arsenal,Technical Memorandum 1004, dated March 1962. (C)

5. Bernard D. Strauss, "A Study of the Burning Rate Characteristicu of HighEnergy Smokeless Nitrocellulose Plastisol Rocket Propellants", PicatinnyArsenal, Technical Memorandum 1231, dated December 1963. (C)

6. Bernard D. Strauss, "An Investiation of Burning Rate Catalysts for HighEnergy Smokeless Nitrocellulose Plastisol Rocket Propellantv", PicatinnyArsenal, Technical M.:randum 1289, dated December 1963. (C)

7. Bernard D. Strauss, "Effect of Oxidizer Particle Size on SmokelessPlastisol Rocket Propellants ", Picatinny Arsenal, Technical Memorandum1624, dated April 1965. (C)

8. Benjamin D. Lehman, "Development of a High Energy Case Bondable SmokelessPlastisol Rocket Propellant", Picatinny Arsenal, Technical Memorandum1748, dated October 1965, (C)

9. Robert G. Wetton and Frank J. Masuelli, "Minutes of the Second QuarterlyReview (1965) of Rocket Propellant Supporting Research held at PicatinnyArsenal", 20 May 1965, Technical Memorandum 1690, Picatinny Arsenal,dated August 1965. (C)

19

GONFIDENTIAL

0 0 0 N N 0 0

0 0 0 x 0 0 0

0 0 x 0 0 0 0

zN

a U

(W~ U

zN 0 k 0 0 )N 0 U

0 ri z

iA

000

u

0 NO *

A 4 A

*AI- W Ito W r4

¢

- -

~11

0. 0 .

4!0 R0'

Ua

I I Izz

0 '0

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ra H UrnH V V V

0' 0

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I N A43

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2a CC.4 1 . rI ZL

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rp.

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b-4 0 .

co

040

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gp

1/~

'40

-4

S.0

Uc3 a

A61IW'~8 '4

44~S* 4 U641w

0 -4-,.a .4

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U -I

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....L... I I I I I I I I Io a a a 0 0 0 0 0 04 1~ N .-4 E~ N -4

~S3/u~uno~ A~guaIu~

LUL

0 E0

I-e.1.

0 0LMt369sino -A3 (42 (4

IOkca C4

04 P4

U2'

(n en

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0 004

P4 1 1-4 so

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309/sunoa'Allsalil

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M 4

pII

CONFIDENTIAL

BALLISTIC PROPERTIES OF SMOKELESS HMX PI.ASTISOL PROPELIANTrSCON~TAINING CHEMICALLY (TDI) AND HEAT TREATED LEAD STANNTE (C)

1.0

0.8 -(a) 0.00 800-1800

l~ 06 (d) 0.37 1000-1800

'~0.5 (e) 0.64 800-3000

~'0.4

S0.2

0.1 e

2 3 4 5 6 8 10 20 30

Pressure, XIOO, psi

IMOREDIENTS PERCENT COMPOSITIONFORMULATIO See a thru eBall Powder, 14528-30 18.5Ball Powder, 2161 1.0Casting Solvent "'46.5IHMX, 2u 30.0Ballistic Modifier 4.0

Ball Powder/Casting Solvent Ratio 0.42

JORMTATIBALLISTIC MODIFIER(a) 740-193-18-7 Lead Stannate -TDI( reduced)

Lot 740- 181-45-9(b) 740-193-18-1 Lead Stannate- TDI(oxidizel)

Lot 740-181-43-1(c) 740-193-16-2A Lead Stannate (as received)

Heated at 450- 500*C for one hourLot 740-181-43-4

(d) 740- 152-95-4 Lead Stannate (as received)

Lot P10707*(e) 740-152-95-2 Lead Stannate -isocyanate (TDI)

Complex

FDJRE 6 (C)

29

CONFIDENTIAL

CONFIDENTIAL

BALLISTIC PROPERTIES OF SMOKELESS HMX PIASTISOL PROPELIANTSCONTAINING CHEMICALLY (MDI) AND HEAT TREATED

LEAD STANNATE (C)

1.0 II I I I I

0.8 ___ Pr. Range(a) 0.50 200 - 1600(b) 0.52 200 - 2000

o 0.6- (c) 0.37 1000 - 1800

(d) 0.56 200 - 1200o 0.5-41

4 0.4

0.3

14 0.2 -

b

d

0.i I I I

2 3 4 5 6 8 10 20 30

Pressure, XlO0, psi

INGREDIENTS PERCENT COMPOSITION

FORMUIATION See a thru dBall Powder, Lot 14528-30 18.5Ball Powder, Lot 2161 1.0Casting Solvei&L ")V' 46.5HMX,. 2u 30.0Ballistic Modifier 4.0Ball Powder/Casting Solvent Ratio 0.42

FORMULATION BALLISTIC MODIFIER(a) 740-193-16-2E Lead Stannate -HDI(oxidized)

Lot 740-181-45-5(b) 740-193-16-2A Lead Stannate (as received)

Heated at 450-500C for one hourLot 740-181-43-4

(c) 740-152-95-4 Lead Stannate (as received)Lot P-10707

(d) 740-193-18-2 Lead Stannate - isocyanate (HDI)Complex Lot 740-181-45-6

FIGURE 7 (C)

30

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF SMOKELESS HMX PIASTISOL PROPELIANTS

CONTAINING CHEMICALLY (TDI) AND HEAT TREATEDBISMUTH STANIULTE (C)

1.0

0.8 1 i"l Pr. Range(a) 0.48 200 - 1600(b) 0.46 400 - 1400

0.6 (c) 0.55 200 - 1200

0.5 (d) 0.44 200 - 1000

0

0.4-

0.3-

0I

0.1 1 f I I I I I I

2 3 4 5 6 8 10 20 30

Pressure, X10, psi

INGREDIENTS PERCENT COMPOSITIONFORMULATION See a thru dBall Powder, Lot 14528-30 18.5Ball Powder, Lot 2161 1.0Casting Solvent 'T' 46.5HMX, 2u 30.0

Ballistic Modifier 4.0Ball Powder/Casting Solvent Ratio 0.42

FORMULATION BALLISTIC MODIFIER(a) 740-193-16-2B Bismuth stannate (as received)

Heated at 450-5000C for one hourLot 740-181-45-1

(b) 740-193-16-2D Bismuth stannate -TDI(oxidized)Lot 740-181-45-4

(c) 740-193-18-6 Bismuth stannate-isocyanate (TDI)Complex Lot 740-181-45-3

(d) 740-193-16-2C Bismuth stannate (as received)Thermite

FIWVRE 8 (C)

31

CONFIDENTIAL

CONFIDENTIAL

BAIST C PROPERTIES OF SMOKEESS HX PLASTISOL PROP LANTSCOTAINING CHEMICALLY (RDI) AN HEAT TREATD BISMUTH sTAT (C)

1.02 . I I I I I I I -

0.8 - Pr Range0.8 (04 0 8

(a) 0.46 400-1800(b) 0.46 400-1400

0.6 - () 0.44 200-1000(d) 0.54 400-1200

0.5

o' 0.o.4

- 0.34(a

-4 0.254

m= (d)

ic

0.1

2 3 4 5 6 8 10 20 30

Pressure, X100, psi

INGREDIENTS PERCENT COMPOSITION

FORMULATION See a thru dBall Powder, 14528-30 18.5Ball Powder, 2161 1.0Casting Solvent "X" 46.5HMX, 2u 30.0Ballistic Modifier 4.0

Ball Powder/Casting Solvent Ratio 0.42

FORMULATION BALLISTIC MODIFIER(a) 740-193-18-5 Bismuth Stannate-RDI(OXIDIZED)

Lot 740-181-45-8(b) 740-193-16-2B Bismuth Stannate (as received)

Heated at 450-500"C for one hour.Lot 740-181-45-1

(c) 740-193-16-2C Bismuth Stannate (as received)Thermite

(d) 740-193-18-4 Bismuth Stannate - isocyanate(HDI) complexLot 740-181-45-7

FIGURE 9 (C)

32

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF EXTRUDED SMOKELESS PROPELLANTS CONTAINING 547. RDX

(W)DIPIERS: LEAD BETA RESORCYLATE, CUPRIC SALICYLATE) (C)

0.6

0.5'

0.4

o~ .3

S0.2

0.1 BC -40*1

4 :3 4 36 b z 3

Pressure X100, psi

INGREDIENTS PERCENT COMPOSITIONFORMULATION 5313Nitrocellulose, 12.67. N 19.9Nitroglycerin 16.7BDX, 14u 54.0Triacetin 4.22-Nitrodiphenylaiine 1.0Lead beta resorcylate 2.1Cupric salicylate 2.1Carbolac I, added 0.03

Heat of Explosion. cal/jxmExpt 1104

vp at Constant P/ _____ Pressure Exponent, 70*FFrom -40*F to 160*F Press range. Psi Slope, "n"

530- .000 0.48Press, at 70OF pir itp. 7./*F

1000 2500 0.16

FIGURE 10 (C)

33

CONFIDENTIAL

CONFIDENTIALBLLISTIC PIOJETIES OF ZXTUUD MHI 13 PILWMU COETAIIr561 uI= (HM3IUS: TZAD MMT 3ZS(CY1ATK CUII SALCun) (C)

0.8

0.6-

*0.5

.~0.4-

40.3

A0.3-

0.00 A 1601FB 70*7C -40*f

1 2 3 4 56 8 10 20 30A Pressure X100. Psi

INQREDIEWlEC C M TO

Nitrocellulose, 12.61 If 20.0Nitroglycerin 15.0lHll: 757. 180 micron, 257. 2 micron 56.0Triacetin 4.02-Nitrodiphenylauine 1.0Lead beta resorcylate 2.0Cupric solicylate 2.0Carbon black, Added 0.03

Heat of Explosion. cal./aExpt 1121

IM at Constant P/r Pressure Exponent, 7017From -40*7 to 1609F Press range, Psi Slope. 'In'

500-3000 0.71

Press, at 70*F P/r lip 7 . /op1000 2700 0.44

FIGURE ni (C)

34

CONMFI DEN TIAL

CO10NFIDENTIALBALLISTIC PROPERTIES 0F EXTUDED S)EUIBSS PROPE LLANITS

COWIAINING 547. RDI (MODIFIER: LEAD STAIATZ -- TDI (REDUCED))()

1.0

0.8-

004-0.6-

0.5-

s~0.31

FORMUlATION 740-172-26-2 (5313)Nitrocellulose, 12.6. N 19.9Nitrqg~ycerin 16.7RDX: 14 micron average 54.0Triacetin 4.22-Nitrodiphenylamine 1.0Lead Stannatel- TDI(Reduced) 4.2

(740- 18 1-45-9)Carbolac I, Added 0.03

Heat of Explosion. cal/mExpt 1145

ivp at Constant pir Pressure Exponent, 70*FFrom -40*F to 160*F Press range, psi Slope, "n!"

800-1200 0.00Press, at 70*F n I. 7./OF

1000 2080 0.02

FIGMR 12 (C)

35

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF EXTRUDED SMIO2EISS PROPELLANTS

cCTA]MIX 54% RDX (MD]OI: ulD STANATE -TDI(OXIDE) (C)

1.0 0.8 II I I I I I

0.8

0.6I "0.5-

AJA

S0.23_

. ' A 160*lfB 70"&C -40*7

1 20. 56 8 10 20 30

Pressure. XI0. psi

UMEDENTS PERCENT CONPOSITIONFORMIATION 740-172-26-1I (5313)

"Nitrocellulose, 12.6% N 19.9"Nitr~g~ycerin 1.6.7

RDX: "14 micron average 54.0Ti~iacet in 0 4.2

2-Nitrodiphenylamine 1.0Lead Stannate -TDI(Oxidized) 4.2

(740-181-46-1Z)Carbolac 1, Added 0.03

l~Beat of Explosion, cal/miExpt 1147

p t ontat /rPrssreExnnnt,7* Prom -40*F to 160"F Press ranke, psi Slope, "n!'

Press, at 70*7 p/r 1(P, %/* 18001M 81 81000 250 0.045

FIGURE 13 (C)

36

CONFIDENTIAL

CONFIDENTIALIALLJTIC D.!UTIKS 0 EXIUDIED SMOMEIBSS NtO WA

couT&nf 56 ac (SDIV s: I AD s WU . 2DI(O I )) (C)

1.0

0.8

0.6

0.5

U0.4

-

"0.3-

4.S

A 1601!

AB 7o0 ]rC -40o

12 3 4 56 8 l zu 3Pressure 1100, psi

PCEECOMMOITION

LMMIOtl 740-172-6-3 (5118)Nitrocellulose, 12.61 N 20.0Xitrg 0yceron 15.0Mr e. 180 micron, 25. 2 micron 56.0Triacetin 4.02-itrodiphanylaine 1.0lead stanzate--T(Oxidized) 4.0

(740-181-46-1)Carbol e o I, Added 0.03

Heat of Explosion, cal/rnExpt 1148

p at Constant p/r Pressure lxponent. 70oIFrom -40*7 to 160"r Press rage. psi Slope, 'In!,

800-13QO 0.23Pres, at 7001 ../r . ./ii..1000 1920 0.09

nJmRZ 14 (c)

37

CONFIDENTIAL

COjNFIDENTIALBLILIST[C PIDFEUIS OF E=~UDBD -SIAISS ROPELLIMS

CMT&IKZN 561 IDE Ma (MgO~ZY : MAD STAIINAT- TD&UXZDIUD)) (C)

0.6

0.4 -

*0.3

0.2

VA 160173 7017C -40OF

3 456 !V0 20 3Pressure -1100. osi

FORM TION740-172-26-5 (511f8 fin)Nitrocellulose, 12.61 N 20.0Nitroglycerin i1 .0HOCC( 2:*icron average 56.0Triacetin 4.02-Nitrodiphenylanine 1.0Lead stannate-TI(oxidized) 4.0

(740- 181-45-i)Carbon black, Added 0.03

Ugat of Ixiosion. cal/lipt 1144

Ito a GontantR/f ressure Ixooneut. 70*7Iron -40*1 to 160*7 Press rne ot fiose. 'W'Pres, at 7=7 21-r 1"ZI 600.1300 0.11

1000 2380 0.05

FIGURE 15 (C)

383

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF EXUDED SMOKELESS PROPELIUMs

CONzTAING 567. HX (MODIIER: LEAD STANNATE -TDI(REDUCED) (C)

1.0

0.8

0.6

.. 1 0.5

w0.4

0.3

0.2- A 160FB 70"F

A C -40*F

o II I I I I I I1 2 3 4 5 6 8 10 20 30

Pressure XIOO psi

INGREDIENTS PERCENT COMPOSITION

FORMIATION 740-172-26-4 (5118)Nitrocellulose, 12.6% 1 20.0Nitrgglycerin 15.0mX :, 75% 180 micron, 257. 2 micron 56.0Triacetin 4.02-Nitrodiphenylamine 1.0Lea stannate -TDI(Reduced) 4.0

(740-181-45-9)Carbon black, Added 0.03

Heat of Explosion, cal/rnExpt 1143

ve at Constant P/r Pressure Exponent, 70OF

From -40*F to 160°F Press range psi Slopet n1000-1500 o.14

Press, at 70"F /r 1, %i9¥1000 1650 0.12

FIGURE 16 (C)

39

CONFIDENTIAL

CONFIDENTIAL

BALLISTIC POPEILTIES OF EXIRUDED SMULESS PKOPELIANTScoTAINIM 567 FINE HMX (MODIFIER: LEAD STANNATE-ITDUEDUCRI (C)

1.0

0.8-

0.6r

0.5-

0.4

9-0.3

A 160F

B 70*1C -40*F

.1I I I II I I2 3 4 5 6 8 10 20 30

Pressure X100. psi

740-172-26-6 (5118 fine)-Nitrocellulose, 12.6% N 20.0Nitrggycerin 15.0HMX : 2 micron average 56.0Triacetin 4.02-Nitrodiphenylamine 1.0Lead stannate -TDI(Reduced) 4.0

(740-181-45-9)Carbon black, Added 0 .03

Heat of Explosion, cal/gmExpt 1137

gp at Constant p/r Pressure Exponent, 701rFrom -40"F to 160"F Press -range, Psi Slope. "n"

&000-1800 0.08,Press, at 70"7 _£r. ., %/Or

1000 1850 0.07

FIGURE 17 (C)

40

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF SMELESS HMX PIASTISOL PROPELLANTS

(MODIFIER: LEAD STNAMTE (AS RECEIVED) ) (C)

1.0 I I i" I I

0.8

0.6

U 0.5

= 0.4.,4

6J 0.3

. 0.2

C -40*F

0.1 Iii , _•_:_ __II_ _1 2 3 5 6 8 10 20 30

Pressure XIOO, psi

INGREDIENTS PERCENT COMPOSITION

FORMULATION 740-193-21-2AFluid Ball Powder, Type B (14528-30) 18.5Fluid Ball Powder, Type C (2161) 1.0Casting Solvent "V' 46.5HMX, 2u 30.0Lead Stannate, P10707 4.0

lp at Constant p/rFrom -40OF to 160OF

Press, at 70*F ,.p/r. aJL/!1000 2500 0.23

Pressure Exponent, 70*FPress Range. psi Slope "n"

1000-1800 0.40

FIGURE 18 (C)

C41

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF A CROSSLINKED SMOKELESS HMX PIASTISOL PROPELLANT

MODIFIER: LEAD STANNATE (AS RECIVED) (C)

1.0I I II I I I

0.8

0.6U

I 0.5

0.4

0.3

0.2

A 160°F

A B '0F

B C -40'

0.1 1 C_____ I I I I1 2 3 4 5 6 8 10 20 30

Pressure XIOO, psi

INGREDIENTS PERCENT COMPOSITIONFORMULATION 740-193-49-1Fluid Ball Powder, Type B, 14528-30 -8.5Fluid Ball Powder, Type C, 2161 1.0Casting Solvent "X" 46.5HMX, 2u 30.02,4-tolylene diisocyanate, added 1.5Resorcinol, added 0.5Lead Stannate, P-10707 (as received) 4.0Ball Powder/Casting Solvent Ratio 0.42

vp at Constant p/r Pressure Er.pongnt, 70*FFrom -40OF to 160*F Press range, psi SloRen"

Press, at 70OF ir p.7/°F 400-3000 0.611000 3330 0.44

FIGURE 19 (C)

42

CONFIDENTIAL

CONFIDENTIAL

BALLISTIC PROPERTIES OF A SMOKELESS MM PLASTXSOL PROPELULAN(MODIFIER: IEAD STANNATE -TDI(OXIDIZED)) (C)

.0I I I II I "I .... I0.8

0.6

0.5

0.4

- 0.3

AF B

0.2 ,A 1601FB 70"FC -40*F

0.1 I I I I I_

1 2 3 4 5 6 8 10 20 30

Pressure X100, psi

INREDIENTS PERCENT COgPStITjO

FORMflIATION 740-193-48-AFluid Ball Powder,Type B4 ¢4528-30) L8.5Fluid Ball Powder,Type C, (2161) 1.0Casting Solvent "X' 46.5• MX, 2u 30.0Lead Stannate- TDI(Oxidized) 4.0

(740-181-65-3)

nI at Constant p/r Pressure Exponent, 70*1From -40"F to 160OF Press range, psi Slope, "n"

Press, at 70*F p/r ip. ,.,F 800-1600 0.061000 2325 0.11

'Ao

FIGURE 20 (C)

43

CONFIDENTIAL

CONFIDENTIAL

BALLISTIC PROPERTIES OF A SMOKELESS IHX PIASTISOL PROPELIANT(3IDIFIER: LEAD STjAtTE 7_TDI(RZDLED)) (C)

U0.8

"0.6

0.5

6 0.4

0.3

AB

0.2 CA 1B 7OFC -40*F

0.1 I I I a I II1 2 3 4 5 6 8 10 20 30

Pressure XO0, psi

INGREDIENTS PERCENT C0GKOSITIOtI

FORMUIATION 740-193-48-BFluid Ball Powder, Type B (14528-30) 18.5Fluid Ball Powder, Type C (2161) 1.0Casting Solvent "X" 46.5HKX, 2u 30.0Lead Stannate .TDI(Reduced) 4.0

(740-181-64-2)

, p at Constant p/r Pressure Exponent. 70"FFrom -40*F to 160@F Press range, psi Slope,"n

Press, at70"F .-.. a,/6 800-1600 0.001000 2270 0,071

FIGURE i (C)

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF A CROSS-LINKED SMKELESS HNX PLASTISOL PROPELLANT

MODIFIER: LEAD STANNATE -TDI (OXIDIZED) (C)

0.1

0.(

U0.!0.

S0.1

0.2 . A- 160OFB 70F1C -40OF

0.A I I I I I I I j1 2 3 4 56 a810 20 30

Pressure. X100, psi

-INGREDIENTS PERCENT COMPOSITION

FORMULATIO 740-193-24-1Fluid Ball Powder, Type B, 14528-30 18.5Fluid Ball Powder, Type C, 2161 1.0Casting Solvent "X" 46.5HMX, 2u 30.02, 4-tolylene diisocyanate, added 1.5Res.orcinol, added 0.5Lead Stannate -TDI(0xidized) 4.0

(740- 18 1-47-3)Ball Powder/Casting Solvent Ratio 0.42

A2D at Constanat 2/r ........essure Exponent, 70OF-Fromi -40*F to 160*F Press Ranize, psi Slope, "n"

1000 - 1800 0.1670esatZOF v23 Ri. 7./0F

1000 2500 0.14

FIGURE 22 (C)

45

CONFIDENTIAL

CONFIDENTIALBALLISTIC PROPERTIES OF A CROSS-LINKED SMOKELESS HMX PIASTISOL PROPELLANT

MODIFIER: LEAD STANlMTE - TDI(REDUCED) (C)

1.0I I I I I Ii

0.8

0.6

0.5

. 0.4

0.3

z 0.2g C,

A 1600 FB 700 FC -40*F

0.1 I I ! I i I I1 2 3 t 4 5 6 8 10 20 30

Pressure, XOO psi

INGREDIENTS PERCENT COMPOSITION

FORMUIATION 740- 193-24-2Fluid Ball Powder, Type B, 14528-30 18.5Fluid Ball Powder, Type C, 2161 1.0Casting Solvent "Xe' 46.5HMX, 2u 30.02, 4-tolylene diisocyanate, added 1.5Resorcinol, added 0.5Lead Stannate- TD(Reduced) 4.0

(740- 181-47-4)

Ball Powder/Casting Solvent Ratio 0.42

p at Constant p/r Pressure Exponent, 70*FFrom -40*F to 160*F Press Range, psi Slope, "n"

1000 - 1800 0.10Press at 70OF Pl. ip, O. F

1000 2220 0.22

FIGURE 23 (C)

46

CONFIDENTIAL

CONFIDENTIALEFFECT OF CHANGES IN BALL ?OWDER/CASTING SOLVENT RATIO

UPON THE BURNING RATE OF SMOKELESS HMX PJASTISOL PROPELLANTSMODIFIER: LEAD STANNATE TDI(REDtCED) (C)

0.9 _ 1 I 1

"n!" Pr. Range. Psi0..7 (a) 0.00 800- 1400

(b) 0.00 1000 - 1800

0.5 --

0.4

0.3.€ c

S0.2 ( .4!

I i I . i , I I i.2 3 4 5 6 8 10 20 30

Pressure, XlO0 psi

INGREDIENTS PERCENT COMPOSITIONFORMULATION 740-193-23-1B ta) 740-193-23-7B (b)

Ball Powder, Lot 14528-30 13.0 25.5Ball Powder, Lot 2161 1.0 1.0Casting Solvent "' 52.0 39.5HMX, 2u 30.0 30.0Lead Stannate- TD(reduced) 4.0 4.0

(Lot 740-181-46-3)

(a) Powder/Solvent Ratio 0.27(b) Powder/Solvent Ratio 0.67ie) Burning rates for systems with P/S ratios of 0.33, 0.42,

0.49, 0.556 and 0.58 fall between chat obtained for (a) and (b).

FIGURE 24 (C)

47

CONFIDENTIAL

CONFIDENTIAL* EFFECT OF CHANGES INT BALL POYDER/CASTING :SOLyENT RATIO

UPON THE BURNING RATE OF SMOKELESS HMX PJASTISOL PROPELLANTS)DIFTER: LEAD ST ANTE (AS R EEIVED) (C)

- 1.o I i ! / i " I I

0.8- "nt._ Pr. Range(a) 0.40 800 - 2000I (b) 0.48 400 - 3000

0.6

0.5-0.4-

0.3-02

oC

0.21

0.' , I 1, I- I I2 3 4 5 6 8 10 20 30

Pressure, XIO0, psi

INGFIDIENTS PERCENT COMPOSITION

FOR MUIATION .740-'193-61. 5

BallPowder, Lot 14528-30 13.0 23.3Ball Powder, Lot 2161 1.0 1.0Casting Solvent "' 52.0 41.7HMX, 2u 30.0 30.0Lead Stannate (as received) 4.0 4.0

(Lot P10707)Ball Powder/Casting S,lvent Ratio 0.27 0.58

(a) Burning rates for system with 0.27 ball powder/casting-solvent ratio.

(b) Burning rates for system with 0.58 ball powder/castingsolrent ratio.

(c) Burnin, rates at 1000 pai are similar for systems withball pcwder/casting solvent ratio& of 0.27, 0.33, 0.42,0.49, 0.556 and 0.58.

FIGURE 25 (C)

48

CONFIDENTIAL

Temperatukre Coefficient, n./ . -40 to 160

0W -4

.4

X 0

om .

x 04 0

LL.4 C- C4L

a z.

u un

NC;

Z /Oll I~do-r

CONFIDENTIAL

EFFECT OF CONCENTRATION OF LEAD) STANNATETDI O-XIDIZED)UPON BALLISTIC PROPERTIES OF

HIGH ENERGY SMOKELESS U)C PIASTISOL PROPELLANTS .C)

0.8 "an" Pr. Range1A 0.71 1000-2600

06 2A 0.17 700-1400*06 3A 0.12 800-1600

0.5 4A 0.06 850-16004,7A 0.03 1200-1600 4

~n 0.4

0.3

a 0.2

"4 2A

.5 1 2 3 4 56 810 20 3

Pressure X100, psi

INGJREDIENTS PERCENT COMPOSITION

FORMULATION 1 A 3 A 7

Ball Powder, 1428-30 18.5 18.5 18.5 18.5 18.5Ball Powder, 2161 1.0 1.0 1.0 1.0O 1.0Casting Scolvent "X'46.5 46.5 46.5 46.5 46.5HMX, 2u 33.0 32.0 31.0 30.0 27.0Lead Stannate- TDI(Oxidized) 1.0 2.0 3.0 4.0 7.0

(740-181-65-3)Ball Powder/Casting Solvent Ratio -0.42

FIGURE 27 (c

50

CONFIDENTIAL

CONFIDENTIAL

EFFECT OF CONCENTATION OF IAD STAMUTETDI(REDUCED) UPON BALLISTIC PROPERTIES OF

HIGH ENERGY SMOKE ESS HKX PIASTISOL PROPEUJAIM (C)

LoO ,__ _ _ _ _ _ _ _ _ _ _ _ _ _ __ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

0.8 "'..__Pr. Range1B0.4200-1800I 110.54

2B 0.09 600-13500.6 3B 0.05 800-1460

o 0.5 - 4B 0.00 800-16007B 0,16 800-1800

0.4-

0.3

°2Bw

0.2

'.4

I .I. I i LI i . i

1 2 3 4 5 6 8 10 20 30

Pressure X10 psi

IMPADIENTS PERCENT COMPOSITION740-193-56

FORMULATION B3 41 LB

Ball Powder, 14528-30 18.5 18.5 18.5 18.5 18.5Ball Powder, 2161 1.0 1.0 1.0 1.0 1.0Casting Solvent "Xe' 46.5 46.5 46.5 46.5 46.5HIMX, 2u 33.0 32.0 31.0 30.0 27.0Lead Stannate -.TDI(Reduced) 1.0 2.0 3.0 4.0 7.0Ball Powder/Casting Solvent Ratio .0.4Z

FIGURE 28 (C

51

CONFIDENTIAL

CONFIDENTIAL LEFFECTS OF CHANGES IN CAWORIFIC LEVELS UPON BALLISTIC

PROPERTIES OF HIGH ENERGY SMKELESSHMX PIASTISOL PROPELIANTS (U)'

2.0

" 70"F Pr. Range0.86 1000-3000

1.0

- 0.6 -

0.5 .

u 0.4 A 160*FtoB 70*F

-C -40!F0.3 ,j I J ' ,I- I i I~

I I I I I I I I I I *l'0.6 In" 70°F Pr. Range

-0.27 .000-14000.5 -v.%/F P/r Press (From 160F to -40F)

0.06 2410 1000

A0.3

-'A 160OFB B 70OF

0.2 C I I I I I I c -o' !1 2 3 4 5 6 8 10 20 30 40 50Pressure X1OO psi

FORMULATION 740-193-62-1 740-193-51- lBBall Powder, 14528-30 13.0 13.0Fall Powder, 2161 1.0 1.0Casting Solvent "X" 52.0HMX, 2u 30.0 30.0Lead Stannate-TDI(Reduced) 4.0 4.0

(740-181-64-2)Nitroglycerin 52.C....-Ball Powder/Casting Solvent Ratio 0.27 0.27Q, cal/g !420 1000

FIGURE 29 (C)

52

CONFIDENTIAL

Security Clasificalile

(Somieity et"sstfgcaton .f ti, be.dy .1 abaott'st 0-foind a~nno.mtation must ba ontoint often A*. evotell nPSo Is cleasifisd)1. 0OR101HATING ACTIVITY (Ceaport -0-i) 2s. REPORT SECURITY C LAIISI!ICATION

Picatinny Arsenal, Dover, New Jersey bGRU

S. REPORT TITLEDevelopment of New Catalysts5 for the Burning--Rat6 Control of HighEnergy Smokeless Nitramine Double-Base Propellants 10U)

7. DESCRIPTIVE NOTES CJ2,p. of atpou and inckastve dog*@)

S. AUTHOR(S) (Lost nsf 1900t name, Inidtia)

Stack, Joseph S.

4. REPORT DATE -7*. TOTAL NO. 0OF PAGES 7.NOOPRS

November 1966 52So. CONTRACT ORt GRANT NO. to. ORIGINATOR*S REPORT NUMUE(S)

Picatinny Arsenal Technical ReportbPROJECT NO. 1A22901A231 No. 3487

~AMCMS Code 5221.11.585 Sb. OTHER RIPORT NO(S) (Any o9,srnut.r that msy ba asstI&d

d.

10. AVAIL ANILITY/LIMITATION NOTICES

Qualified requesters may obtain copies of this report fromu DDC

I I. SUPPLENEKIITARY NOTES 12. SPONSORING MILITARY ACTIVITY

I3. A3SSTRACT

(C) Studies leading toward the development of new combustion catalysts whichare very effective in reducing the temiperature and pressure dependency of burningrate of high energy (230 - 240 ib-sec/ib) smokeless nitramine (RDx, HMM) propell-ants are discussed.

Described are the methods of manufacturoj, proposed reactions and analytical4 and X-ray diffraction data of the new combustion catalysts.

Strand burning rate data are presented for extruded and plastisol (cross-linked and uncross-linked) propellants. The results show the highly effectivenature of the new combustion catalysts in reducing the variability of burning rateto changes in temperature and pressure of these propellant types. Propellantsinvestigated have application for close support and other weapon systems wherehigh performance and smokelessness are required.

D D I AN6 1473 C0NPIDEWTIALSecurity Cl.. '-:'tion

/

Security Classification _

14. LIEY WORDS LNK A LINK S LINK C

ROLE WT ROLE WT ROLE WT

Coab ustion CatalystsBurning Rate ControlSmokeless Nitramine Propellants

Extruded PropellantsPlastisol Propellants

Cross-Linked Propellants~RDX

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security Classification