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DDC
DEC 2 119"

TECHNICAL REPORT
EUSTOMXRIC INSULATION FCR SOLID PROPELIANT

ROCKET MOTORS
By
D.

H. Sale

IO124401A

"Departent of the Army Project No.


AMC Code No.-

5025.11.8

Report No. 64-3158


1-9-100-2
EL
DISTRIBUTED BY THE
OFFICE OF TECHNICAL SERVICES
U. S. DEPARTMENT OF COMMER(CE
WASHINGTON 25. D. C.

42

03
Copy No.

Date

.
27 October 1964

rHIS REPORT MAY BE DESTROYED WHEN

NO LONGER REQUIRED FOR REFERENCE

The findings in this report are not to be construted


as an official Departm-nt of the- Army poxsitIon.

"(kxpies Available at Office of Technical Ser' ices S . 75

Repcrt No,
Copy No.

ELASTOMERIC

INSULATION FOR SOLID PROPELLANT


ROCKET MOTORS

By

D.

H. Sale

Apprcved by:

A. C. HANSON
Laboratory Dlrector

27 October 1964

DA Projec Nc.

1CO-24401-All0

AMC Code Nn.

5025 11.84203

Rock IslaDd Arsenal


Rock Islandd !lltnois

DDC AvaIlabilltv Notice:


Quailfied requesters may obtain
copies of this report from DDC.

64-3158

ABSTRACT
The development of flexible, elastomeric-based,
solid propellant rocket motor case insulation is discussed.
The effect on insulation properties of type of asbestos,
of liquid versus solid elastomers and of methods of dispersing fibrous compounding ingredients, are reported.
Oxyacetylene torch and static
motor firing test data
for some of the better insulation materials developed,
as well as for souie commercial materials, are presented.
The torch test, the principle screening tool used in this
study, conforms to the test currently being standardized
by the Flame Ablation Test Group of Section III-L of ASTM
Committee D-20.
A material with 40 percent elongation, 1.34 gm/cc
density, performance ind3x of 95 cm2 sec/gm and erosion
rate of 2.0 mils/sec was the most promising insulation
developed.
The material is a 55/45 butadiene/acrylonitrile
compound containing phenol furfural resin, asbestos
and oxyazoline wetting agent.
It has been satisfactorily
bonded to aluminum and to steel by conventional bonding
agent.
The thermal properties of this vulcanizate are
not affected by oven aging for one week at 70 0 C.

64-3158

RECOMMENDAT IONS
project be discontinued.
It is recommended that this
It is believed that the insulation materials developed
investigation represent an
during the course of this
and that further
of the art
advancement in the state
and
inves t lgations under the approaches outlined in this
improvements.
only
marginal
in
would
result
work
earlier
I-- is recommended that the oxyacetylent torch test
eqipment be retained in a usable condition, in order that
promising new commercial insulation materials might be
evaluated and that cooperative work to further improve
might be conducted, if necessary
*his screening test

64-3158

ii

ELASTOMERIC

INSULATION FOR SOLID PROPELLANT


ROCKET MOTORS
CONTENTS
Page No.

Object

Inttroduction

Procedure

Results ard Discussion

Literature References

14

Appendix I

16

Appendix II

17

Distribut icn

18

iii

64-3158

ELASTOERIC

INSULATION FOR SOLID PROPELLANT

ROCKET MOTORS
OBJECT
To develop improved,

flexible,

thermal case insulation

for solid propellant rocket motors.


INTRODUCTION
The need for flexfl rocket motor case insulation nas
Elastomers have played an
been well established,
important role in meeting this need, as evidenced by the
many types of elastomeric-based insulations which have been
developed for use in solid propellant missiles.
The wide
spectrum of commercially available insulation ranges from
but
lightly filled
rubbers with excellent flexibility
compounds
to
highly
loaded
resistance,
minimal ablation
with little Alexlbility but outstanding resistance to the
high temperatures and erosive gases found within rocket
motors.
Present day elastcmeric insulations are not considered
adequate for future neeas. especially needs related to the
It is anticipated that longer
use of end burning grains.
burning times at higher temperatures will necessitate more
thermally resistant insulations and that higher internal
A
pressures will require higher degrees of flexibility.
continuing need exists frr lighter weight materials,
I-,appears that maximum flexibility and resistance to
the environments within rocket motors are mutually
exclusive properties. insofar as rubber-based insulations

are concerned,

since tmprcvements in one property are

Earlier work
attainable only It the expense of the other.
at this Arsenal, -8,9) as well as more recent studies, has
led to the development of r-'bber-based insulations having
a compromise In these two properties, namely, the highest
degree of ablative resistance which could be attained
together with flexibility which, when measured in terms of
Results of these
elongation, amounts to 20 to 50 percent.
studies have led to the following conclusions:
combination for
1. By far the cost effective filler
imparting ablation resistance to rubber vulcanizates is a
combination of a phenolic resin and long fiber asbestos.

2.
high nitrile

This filler combination is most effective in a


content,

butadiene/acrylonitrile

elastomer.

Of the more than 400 combinations of elastomers,

64-3158

fillers

and other compounding ingredients tested, none has led to


a material having a better compromise between flexibility
resistance than that exhibited by the nitrileand abltion
phenolic resin-asbestos fiber system.
3.
The degree of ablation resistance of this, or any
other asbestos-containing rubber compound, is directly
related to the fiber length of the asbestos in the finished
product.
These findings largely influenced the direction of
Minimum effort has been
effort described in this report.
devoted to seeking more effective combinations of rubber
and fillers.
Major emphasis has been placed on developing
means for incorporating long fiber asbestos into rubberresin matrices without significantly reducing fiber length.
PROCEDURE
Insulation resistance was determined with an oxyacetylene torch test (Figure 1) using the conditons cited
in Table I. The equipment and procedures duplicate those
of the test currently in the final stages of standardization
by the Flame Ablation Test Group of Section III-L of ASTM
Committee D-20.
The effectiveness of candidate insulation materials
(1) the temperature
was meawured by two test criteria;
rise on the back side of the specimen while the front
side was exposed to the oxyacetylene torch flame and (2)
the time required for the flame to burn through the
These criteria
are reported as performance
specimen.
The index,
indices and erosion rates, respectively.
referred to as P 2 0 0 , is computed by dividing the time
(seconds) required for the specimen back side to reach
200 0 C. by the original specimen thickness (centimeters)
The erosion rate,
and by the specimen specific gravity
E, is computed by dividing the original specimen thickness
It should be noted that
(mils) by the burn through time.
high values of P 2 0 0 and low values for E are indicative of
Unless otherwise noted, the
good insulation properties.
performance indices and erosion rates reported are the
average of four test results
Rock Island Arsenal Laboratory has been an active
The torch
member of the aforementioned ASTM Test Group.
test facility at this Laboratory was among those utilized
The round robin results showed
in a recent round robin.
an average variance among laboratories of less than 5% for
The Rock Island Arsenal
eacn of the Iwo test criteria.
test facility produced results well within this variance.

64-3158

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TABLE I
TORCH TEST OPERATING CONDITIONS
Oxygen flow rate, standard cubic feet/hour

(SCFH)

Acetylene flow rate, SCFH


Volume ratio oxygen to acetylene

123

102
1 2

Impingement angle between flame and specimen,


Specimen size, inches
Distance from torch tip to specimen, inches
Method of determining moment of burn through

degrees 90
4 X 4 X 1/4
3/4
Visual

Several materials which exhibited excellent


to the torch test were evaluated (see Table VII)
motor firings conducted b,, the AtlantIc Research
and the Allegheny Ballistics Laboratory at their
test facilities.

resistance
In static
Corporation
respective

The major compounding ingredients for each material


tested may be found in the tables pertaining to the
material.
Curing systems are given in Appendix I. Test
specimens were compression molded in a four cavity mold.
The liquid polymer-based ccmpounds were mixed in a two
bladed sigma type mixer (Figure 2), with mi.xing arms
operating at differential speeds.
All solid polymerbased compounds were mixed on a two roll
rubber mill.
Stress-strain properties were determined in accordance
with applicable ASTM(lO) procedures
RESULTS AND DISCUSSION
Previous evalua.cn( 9 ' of several types of inorganic
and organic fibers had shown that asbestc3 was the most
effective for imparting thermal resistance tc rubber
vulcanizates
Curren, studies were made to determine the
effect of the type cf asbestcs on the properties of
insulation materials
Amosile, crocadolite and chrysotile
asbestos of approximately equal fiber length "major concentration of fiber lengths. 3/4 to 1 inch long) were
evaluated in a nitrile
r.ibber..phenol.c resin based compcuind
Chrysotile samples from three different suppllers were
included
The results in Table II show that the three

chrysotile-based vulcanizates differ from one another


considerably, but that all three are superior to either
the amosite or crocidolite-based

insulations.

The supe-

riority of chrysotile is attributed to its flexibility


(both amosite and crocidolite are brittle and tend to
suffer fiber breakdown during compounding), higher specific
heat and fusion temperature, lower density and higher
percent of bound waterHereinafter, the word "Asbestos"
4

64-3158

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The problem of obtaining a uniform dispersion of long


asbestos fibers in a rubber matrix while et the same time
minimizing the reduction in fiber length was attacked
through the use of the following classes of materials:
(1P wetting agents, to wet the asbestos fiber and thus
facilitate
fiber dispersion; (2) plasticizers, to soften
the rubber matrix; (3) liquid polymers, to reduce shearing
forces which prevail when solid polymers are mixed; (4)
s lvents, to dissolve the unvulcanized rubber prior to the
asbestos addition.
Evaluationsof wetting agents were made as shown in
The wetting agents were added to the mixture
Table 1I1.
Although most of the wetting
jus# prior to the asbestos.
agents tested were useful in dispersing the asbestos,
However, oxyazoline
not all
improved insulation properties.
#1. a heterocyclic cationic wetting agent, produced vulcanizates with excellent thermal properties.
A compound
ccntairning 30 PHR of this wetting agent produced a 25 percent
improvement In thermal properties and a 100 percent increase
in elongation over the control material containing no
wetting agent.
Oxyazoline #1 at 30 PHR concentration showed no evidence
of migration after aging for 7 days in an air oven at 700 C.
Aged specimens when evaluated in the oxyacetylene torch
"est. exhibited thermal properties equivalent to unaged
Insulation containing oxyazoline #1 has been
controls.
bonded to both aluminum and steel using a two part, room
Bond
temperature curing, general purpose epoxy adhesive.
greater
one
inch
lap
joints)
shear
on
(tensile
strengths
than the tensile strength (1730 psi) of the insulation
were achieved.
Data for plasticized solid elastomer-resin-asbestos
ccmpounds and unplasticized control compounds are presented
in Table IV. Small amounts (5 and 15 PHR) of phosphate
esters served to increase elongation but larger amounts
None of the vulcanizates had
decreased elongation.
improved thermal properties over the controls.
Liquid irgredients offer a means of compounding with
Data for liquid elastomer-asbestos
Icv shear forces.
vl;canizates, as well as the appropriate controls based
The data revealed
on solid polymers, are given in Table V.
vulcanizates based on liquid
the following results:
elastomers have better thermal properties, greater tensile
strength but shorter ultimate elongation than the controls
The liquid elastomers consisted
based on solid polymers.
cf low molecular weight, short chain molecules which required

64-3158

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a high state of cure to produce good thermal resistance.


the incorporation
Although these elastomers did facilitate
of fibrous asbestos without appreciable fiber breakdown, the
high degree of crosslinking required for proper vulcanization
produced lower elongations than are inherent with solid
polymers.
Further evaluation of liquid elastomers

included the

addition of thermosetting resins (liquid and solid) as


polar
The resins used in this stuoy were all
fillers.
and enhanced the erosion resistance of NBR-based compounds,
but they were too incompatible with the less-polar SBR
to be effective.
Because of the lack of non-polar resins
and the low elongations obtained with the liquid elastomers,
work with SBR and NBR liquid elastomers was di3continuedo
The two carboxy modified polymers listed in Table V
were vulcanized using an epoxy resin at a concentration of
The low elongations obtained from
13 PHR as a curative.
these two compounds eliminated the need for investigating
the effect of adding more resin.
The method of incorporating asbestos by adding it to
a methyl ethyl ketone solution of the polymer and other
The asbestos
compounding ingredients proved unsuccessful.
in the resultant vulcanizates was non-uniformly dispersed
and vacuum evaporation of the
in the rubber matrix after air
These vulcanizates had properties inferior to the
solvent.
properties of vulcanizates prepared by conventional milling
procedures.
Torch test data for several commercial insulation
Of these
materials tested are presented in Appendix II.
n-aterlals, one has properties comparable to the best
Rock Island Arsenal insulation, as shown in Table VI,
The work discussed he...in and work previously reported(8,9)
has resulted in several excellent thermal insulation materials.
The nine best of these, along with five poorer materials
motor
and two commercial products, were evaluated in static
Erosion rates,
firings by Atlantic Research Corporation.
densities, elongations and major constituents for each are
The erosion rates from the static
presented in Table VII.
firing tests correlate reasonably well with the torch
test erosion rates, at least for the best five or six and
The erosion rates from the static
the poorest compounds.
tests cover a range of only 2.4 units, as compared to 10.4
units for the torch test.
Unfortunately the insulation containing oxyazoline #1
wetting agent was not included with the above materials.

64-3158

11

TABLE V I
EVALUATION DATA FOR THE BEST ROCK
ISLAND ARSENAL
AND COMMERCIAL INSULATIONS
Property Measured

Rcck Island Arsenal

P200- Cm 2 sec/gm

Commercial #I

95

79

Time to backside
temperature of 2000C.
for 1/4" specimen, sec.

127

101

E,

2.0

2.0

mils/sec

Elongaticn,
Density,

gm/cc

Major constituents

40

50

1.34

1.28

Rubber,
Asbestos,

Resin,
Oxyazoline #1

Rubber.
Resin,

Asbestos

However, this material was submitted


to Allegheny Ballistics
Laboratory for evaluation in their
test
facilities
Their
data indicates that it compares
favorably yh
materials
they class as "current better materials."(11
t

12

64-3158

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LITERATURE REFERENCES
1.

Batchelor, J. D. and Vasileff, N., "Solid Propellant


Rocket Motor Insulation," Conference on Behavior of
Plastics in Advanced Flight Vehicle Environments,
WADD Technical Report 60-101, September 1960.

2.

Dervy, A. J., "Reinforced Plastics of High Strength/


Weight Ratio for Space Applications," Society of the
Plastics Industry, Inc., 17th Anrual Techn.Lcal and
Management Conference, Reinforced Plastics Division,
Chicago, Illinois; 6,7,8 February 1962.

3.

Epstein, G., Cecka, A. M. and Robbins, D. L., "Plastics


in Rocket Nozzle Environments," Conference on Behavior
of Plastics in Advanced Flight Vehicle Env:!ronments,
WADD Technical Report 60-101, September 1960.

4.

Epstein, G. and Jaffe, E. H., "Materials for Internal


Tnermal Protection of Rocket Motor Cases. A State-ofthe Art Survey," Society of the Plastics Industry, Inc.,
17th Annual Technical and Management Conference,
Reinforced Plastics Division, Chicago, Ill;
6,7,8
February 1962.

5.

Hazelrigg, W. K., "Design Criteria for Insulation


Materials " a paper presented to the Refractory Material
Working 6i-iup, Aerojet-General Corporation, Sacramento,
Califcrnia, 14 July 1960.

6.

Headrick,

R.

E., "Ablative Elastomeric Insulation


Directorate of Materials and Processes,
Wright-Patterson Air Force Base, ASD-TDR-62-400,
August 1962.
Materials,"

7.

Sewell. J. J. and Kuno, J. K., "Aerospace


Hardware and Thermal Insulation," Society
Industry, Inc., 17th Annual Technical and
Conference, Reinforced Plastics Division,
Illinois; 6,7,8 February 1962.

8.

Rack Island Arsenal Laboratory Report No. 61-2315,


2 August 1961. "Evaluation of Flexible Insulation for
Solid Propellant Rocket Motor Cases."

9.

Rock Island Arsenal Laboratory Report No. 62-2366,


6 July 1962, "Development of Flexible Insulation for
Solid Propellant Rocket Motor Cases."

14

Use of Plastic
of the Plastics
Management
Chicago,

64-3158

10.

American Society for Testing Materials, October 1961.


"*ASTM Standards on Rubber Products," 1916 Race Street,
Philadelphia,

il.

Pa.

Confidential Communication, Allegheny Ball.istics


Laboratory to Rock Island Arsenal, Subject:
'Evaluation of Car didate Insulation Material"(U),
25 June 1964.

64-3158

15

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D1)TRIBUTION
No.
A.

Copies

o0

Department oi befense
Office oi tfae Director ou Deiense
Research & -.'nineering
ATTN:
Mr. J. C. i3arrett
Room JD-10i5, The Pentagon
Washington 25,

D. C.

Co,-m,.ma n ,er
r

Delense Documentation Center


ATT 'N: T' -DR
Cameron - ation
Alexanuria, virginia
G.

22314

Department of the Arms

Technicai

20
.,ervices

Commanding General

U,..

Arny 41.ateriel Command

Room 25J2, Bldg. T-7


ATTN:
AMCRD-RS-CM
Washington, D. C.
20315

Commanding Officer
U... Army Coating and Chemical Laboratory
ATTN: Dr. C. Pickett
Techpical Library
Aberdeen Proving Ground, Maryland 213)5

1
I

Commanding General
U.:.

ATTN:

Army Tank Automotive Center

SMOTA-REM. 2

EMOTA- R'M. 3
Warren, Michigan
4b990

Commanoing enerai
U.s. Army Weapons Command

ATTN:

AMS WE-RD
AM'I WE-PPP

Rock Island Arseral


Rock Island, Illinols

18

64- 3158

D ITRIBUTION
No.
Commanding General
U.S. Army Missile Command
ATTN:
Documentation & Technical
Iniormation Branch
Mr. R. E. Ely, AMSMI-RRS
Mr. R. Fink, AMSMI-RKX
Mr. W. K. Thomas, AMSMI
Mr. Z. J. Wheelahan, AMSMI-RSM
35b09
Redstone Arsenal, Alabama
Commanding Officer
Frankford Arsenal
SMUFA-1330
ATTN:
Library-0270
19137
Philadelphia, Pa.

of Copies

2
1
1
1
1

1
I

Commanding Officer
U.3. Army Materials Research Agency
Watertown Arsenal
RPD
ATTN:
02170
Watertown, Mass.

Commanding Officer
Picatinny Arsenal
& Packaging Lab.
Plastics
ATTN:

Dover,

PLASTEC
New Jersey

1
07801

Commanding Officer

Springfield Armory
SWESP-TX
ATTN:
Springfield,

Mass.

01101

Commanding Officer
Watertown Arsenal
ATTN-.
SMIWT-LX
Watertown, Mass.

02170

Commanding Officer
Watervliet Arsenal

ATTN:
SWEWV-RDR
Watervliet, New York

12189

U.S. Army Munitions Command


07801
Dover, New Jersey

Commanding General

64-3.158

19

DIzTR IBUTION

No.

of Copies

Commanding Officer
U.S. Army Environmental Health Laboratory
Army Chemical Centvr, Maryland

Commanding Officer
U.S. Army Chemical Warfare Laboratories
ATTN:
Technical Library
Army Chemical Center, Maryland

Commanding Officer
Harry Diamond Laboratory
ATTN:
Technical Library
WashingtoxA, D, C.
20436

Commanding Officer
U.S. Army Engineer R&D Laboratories
ATTN:
Chemistry Research Section,
Materials Branch
Fort Belvoir, Virginia
Commanding Officer
U.S. Army Electronics R&D Laboratories
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