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U. S. NAVAL AMMUNITION DEPOr~Crane, Indiana

RDTR No. 5128 Qotobor 1966

BINDING PIROPg@RTIES AND OTHER CHARACTEISTICSOF SEVERAL POLYESTE-A RESIN BINDERS

USED ',W PYROTECHNIC FORMULATIONS

PREPAPED BYRy -A CheMiACal, Engineer

flEVIEWED BY L 4-./JvII; E. W'IU)lIDGE, Mfanager, S ukface and Air/ Devieces Branich

flEVjIF741D BY (a',* 1- ijcr'" -

P. P. CORWELL, Manager, Pr E't Development4DivisionRUI 12ASED BY 4

S.P.FAsIG , ir/ tor. R&D Department

flDTR No. 51i

ABSTRACT

The binding strengths of pellets subjected to tensile

and shear stresses, and the burning time and candlepower of

flares pressed from compound aged 0-6 hours in increments of

one hour prior to pressingwere determined after curing periods

of 5 and 30 days. Three formulations were used, each contain-

ing the same ratio of magnesium/sodium nitrate/binder; but,

with three different polyester resin bindors--Leminao 4110,

Laminae 4116, and Aropol 7720M.

The variation in physical strength, candlepower, and

burning time with respect to delay time between mixing and

pressing was found to be greatest for pellets and candles

containing Laminae 4110. Likewise, the physical strength

of pellets containing Laminae 4110 was significantly higher

than the other pellets after curing 5 days; however, tests

after 30 days indicated that by this time the Laminao 4116

had essentially fully cured, and now had binding properties

similar to Lazninac 4110. The physical strength of pellets

cured at 75 - 85°F with Aropol 77,0M was considerably less

than pellets containing the other binders.

All units cured for 16 hours at 150*F, and then tested

after 5 days exhibited considerably higher strengths than

i

RDTR No. 51

palleta not -subJeoted to an elevated temporature. Hovevr,

tests after SO dys showed that for the Laminao binders,

greater bind-ing strength is obtained by puring at room temp-

erature for th9 duration of the ouring cycle.

p

ii

RDTR No. 51

TABLE OF CONTENTS

Page

Objective .......... .6........ ... .......o,., .Experimental Method ...... 1......... ................... 1

Composition Formulation 1 1Pressing and Curing Procedure ...................... 1Testing Apparatus and Equipment . 2

Discussion ................ ........ ...........6... ... 3Binders ............... . ........ . 6..ii i 3Tensile -Strength . ... 60 .... t.... 5SharSregh .......... ...... ...*...... *6 VShear 7tegt

Effect of 150°F Curing Cycle ........ 9Burning Time and Candlepower of Flares ............. 10

Pellet Density ..................... . .... 11Conclusions ......................... ............ 12

ILLUSTRATIONS A, B & C ................ 4

TABLES

I T/nvile Test Experimental Data ................. 14II ," ge Failure Loads (Lb.) in Tensile ......... 15

IlYT TSt Experimental Data .................... 16IV v .azse Failure Loads (Lb.) In Shear ............ 17V h' .)rimentai Data - Pellets Cured at 150°F ...... 18

VI A,1-rage Tensile and Shear Failure Loads (Lb.)or Pellets Cured 9 1500F and Ambiontly ....... 19

VII j-" rimentol Data - Burning Tim- & AverageCandlepower of Candlnz ........................ 20

VIII Burning Time, Candlepower & Cendlepower-Secondsof Flares ............................. . 21

C IHS

I ..... 221I16 6 6 0 f *0 6 6 6 6 6 V~ 23

VI .. 0 6...6. .. 27

iii

RDTR No. 51

I. OB3ECTIVE

The purpose of this study was to determine the binding

properties of several polyester resins used in pyrotechnit

compositions as a function of the polymerization time before

and after pressing. Additionally, the variation in candle-

pcwer and burning time of the formulation under oonsideration

was to be investigated.

II. EXPERINENTAL METHOD

Composition Formulation

A pyrotechnic formulation containing 61.4% magnesium

(granulation 18), 33.8% sodium nitrate (Class 2), and 4.8%

binder was selected as the composition to be investigated.

Three different polyester binders were utilized--Lamineo 4110

and 4116 (American Cyanamid Co., Wallingford, Conn.), and

Aropol 772OM (Archer-Daniels Midland Co., Minneapolis, Minn.).

After mixing, the compound was stored in a closed container

until pressed.

Pressing and Curing Procedure

Pellets one inch in diameter and two inches long were

pressed immediately aftermixing, and in increments of one

hour after mixing up to a maximum of six hours. Each pellet

contained two increments of 22 grams each, pressed at a dead

1

RDTR No. 51

load of 8,000 -pounds. Twenty-four pellets were pressed

immediately aftsr mixing, and 12 during each time interval

thereafter. The diameter, length, and weight of each pellet

was recorded immediately after pressing, and in some cases

after five and 30 days curing. All pellets were cured in a

sealed can at 75 - 850F, except for 12 pellets pressed immedi-

ately after mixing which were cured for approximately 16

hours at 150F. The pellets were tested five and 30 days

after pressing.

Three flares wore pressed immediately after mixing, and

during each hour thereafter, up to six hours after mixing.

Each flare contained three 200 grain increments, pressed at

a deadload of 22,030 pounds into a fish paper tube which was

1.96" OD and 1.75" ID. The flares were cured at 75 - 850F,

and burned after 30 days.

Testing Apparatus and Equipment

The testing apparatus and equipment used in the determi-

nation of the shear and tensile binding properties of the

various resins areillustrated on the following page. The

testing machine used to perform both the tensile and shear

tests is shown in llu3tration A. The movable Jaws were

clamped together to hold the cables which were connected to

2

-71

RDTR No. 51

the test fixtures, and then the Jaws were moved vertically

apart to supply the requ! red fnrce. The shear and tensile

test fixtures are shown in li-zstrations B and C respectively.

For the shear test, the pellet wa3 placed in the test fixture

and then the assembi- was mouted in the test machine. In

the tensile test, e pellet with an end plate attached to each

end was held in the fixture by the removable pin, and then

the assembly we% placed in the testing machine.

Orbond 121- cas used to bond the end plates required for

the tensile test to the pellets. The tensile test data for

the Laminac 4116 units is rather incomplete because an

inadequate amount of adhesive was used to bond the end plate

to zhe pellet; thus, failure occurred at the picte-pllet

interface rather than at the increment.

BF. DISCUSSION

Binders

The binders selected for this investigation were ones

believed to be suitable for use in pyrotechnic flarn compo-

sitions, and which would essentially fully cure at temperatures

between 7 - 85OF when adequately catalyzed. Cobalt Naph-

thenate, which pranotes room temperature cure when catalyzed

by methyl ethyl ketone (Luporzol DDW), is present in a

3

RDT-R No. 51

ILLUSTRATION A

Riehie Testing MachinoMfg. b y American M~achine & Metals Co.East Moline, Illinois

ILLUSTRATION B

ILLUSTRATION C

Trensile Testing hvxure

Shear Testing Fixture with end plate

- ~ = _ ___ --- ~- ~ _ . .

RDTR No. 51

suffioienf amount in Lrminao 4110 to -effeet a coplete cure

at roo temperature. On the other hed, Lemlinao 4116 con-

tains a lesser amount- of Cobalt Naphthenate; therefore, this

resin will not cure as quickly as Lominac 4110, and in some

cases an elevated temperatare ray be required. The Aropol

resin does not contain any of the Cobalt promoter, hence,

the aromot r rist be added to obtain a room teaperature cure.

Company literature indicates that the gel ti-, for Leminao

4110 and 4116 with . 5% Lupersol TV-' catalyst, is approxi-

mately 15 minutes and 35 minutes respectively, and that

Aropol 772OU shojld goel in about 25 minutes when catalyzed

by 0.5f Cobalt flapthenato end 1.0%. Lupersol &XI. Although

the compozition was stored in closed containers betcan mix-

ing ari pressing, it would be suspected that the infuence

of the delay ti-M- betreoen mLxin erA prasrirs upon the physical

prop rtier and burning chaeracteristics of the pressed compo-

sition would be most notIOPble 'in the Loz-ina- 4110 cmpos-i-

tion. Mhe Uiterature also states that the tensile strength

of the fully- cuved L- ninao resins is approximately 9.000 PSi,

end about P,500 n3I for the Aropol binder.

Tensile St-reng*-h

Graph I shows a binder--binder comparison between the

5

RIDTR No. 51

tensile strength of the three formulations after five and 30

days curing, while Graph II illustrates the difference in

_tensile strength after five and 30 days for a given binder.

As stated previously, the experimental data for the Laminae

4116 units is incomplete because the end plate-pellet bond

proved to be weaker, in many oases, than the increment-to-

increment bond. All of the data considered was for failures

which occurred at the increment-to-increment junction. Table I

gives the experimental tensile failure loads after five and 30

days for the various mix-press delay times, and Table II con-

tains the average of the abeove figures for a given resin and

delay time.

Considering the accuracy of the testing equipment used,

and the variation in the data for a given binder and delay

tdim_ the del-- e- beutO&n ing and pressing does not

appear to have a significant effect upon tensile strength.

The tensile strength of the Aropol pellets did seem to exhibit

somewhat of a trend toward increasing as the delay time

increased; however, the magnitude of the increase can hardly

be judged significant. A binder-binder comparison shows that

the Laminac 4110 pellets sustained a 404 greater tensile force

belore failure than the Laminae 4116 units, and 80% greater

6

RDTR No. 51

than the Aropol pellets.

n the other hand, the difference in tensile strength

after five and 30 days ambient cure for a given binher was

found to be very significant. The Laminac 4110 units failed

at a 65% greater tensile load after 30 days than five days,

the Laminae 4116 pellets increased 100% in tensile strength,

and the Aropol pellets exhibited an increase of 50%. Oncoe

again, the Laminae 4110 pellets were superior to the other

units, since their tensile strength was 10% and 80% greater,

respectively, than the Laminae 4116 and Aropol 7720M pellets.

It is interesti ,g to note that the tensile strength of the

pellets increased substantially between the five Ind 30 day

period, and that aft,,r 30 days cure, the Laminae 4110 and

4116 pellets exhibited scmowhat ir- =p!ab'o tensile binding

properties. This data agrees with the rjp@ny litqrature

for the various binders, which indioaltd that Laminae 4116

does not cure as quickly as 4110, and that when fully cured,

the tensile strength of the two Laminae resins are basically

the same, and considerably greater than for, Aropol 7720M.

Shear Strength

The shear strength data is presented in Tables III and

IV. Graphs III and IV give a binder-binder comparison of

7

I

RDTR No. 51

shear strengths after flve and 30 day curing cycles, respeo-

tively and Graph V shows the variation in the shear strength

for a given binder, resulting from.a five and 30 day cure.

Referring to Graph V, it is seen that as the time from

mixing to pressing increases from 0 to 6 hours, the shear

strengths of the Laminae 4110 units increased rather consist-

ently, amounting to an overall increase of approximately 200%.

Such a trend was not evident after the 30 day cure in the

Laminac 4110 units, nor did it exist after either five or 30

days for the other binders.

After five days cure, the pellets containing Laminae 4110

failed at about a 50% greater shear load than the other two

pellet formulations. However, tests after 30 days revealed

that although the Laminae 4110 had a shear strength approxi-

mately 200% greater than the Aropol units, they nc faleau

at a 25% lower shear load than the Laminae 4116 pellets.

This data substantiates that found during the tensile tests,

in that although the physical properties of Laminae 4116 are

inferior to Laminae 4110 after a short ambient curing cycle,

as the curing period is increased, the physical properties

of the Laminae 4116 are enhanced until the two binders have

basically the same properties. The per cent increase in the

8

RDTR No. 51

shear strengths after five and 30 days was 125%, 350%, and

15 for the Laminac 4110, Laminae 4116, and Aropol resins,

respectively.

Effect of 150*F Curing C2ole

Table V contains the experimental data for pellets cured

approximately 16 hours at 150°F, immediately after pressing,

and then stored in closed containers at 75 - 85*F until

tested after five and 30 days. The average values for the

above data aregiven in Table VI, along with the correspond-

ing values of pellets cured at room temperature.

If the tensile and shear strengths of pellets subjected

to the elevated temperature are compared to those cured at

room temperature, it is seen that the elevated temperature

cure has a marked effect upon the physical properties of the

resins. After the 150*F ur, the Aropol uni.t.s... . tad .after

five and 30 days failed at tensile and shear loads which were

at least 75f. and 20% greater, respectively, than the Laminae

resin pellets. Referring to Table VI it is seen that the

Laminao pellets cured at an elevated temperature and then

tested after five days, possessed significantly greater tensile

and shear strengths than pellets not subjected to the 150OF

cure; however, the results of similar units tested after 30

9

RDTR No. 51

days indicated that binding strengths of units oured solely

at 75 - 85*F, were approximately 25% greater than those cured

for 16 hours at 150°F and the remaining time at 75 - 85*F.

Burning Time and Candlopower of Flares

There was found to be a significant variation in candle-

power, burning time, and the emitted candlepower-seconds with

respect to the delay time between mixing and pressing. A

similar difference also xisted between the three binders.

For the flares containing Laminae 4110, 4116, and Aropol 7720M,

an overall decrease of 6%, 5%, and 3 in burning time, an

increase of 144 8 and 8. in candlenower- and an increase

of 7%, 4., and 47 respectively in candlepower-seconds were

obtained for compound pressed between 0 - 6 hours after mix-

ing. This experimental data may be found in Table VII.

Average values are given in Table VIII and plotted on Graph Vi.

Generally consistent data was obtained for a given delay time

and formulation.

If an average value of the emitted oandleporer-soconds

is calculated, it is found that the Aropol and Laminac 4110

units are approximately equal, while the Laminae 4116 flares

emitted about 13f fewer candlepower-seconds. The pressed

length of flares of a given formulation were essentially the

10

RDTR No. 51

same; therefore, the variation in burning time is indicative

of the variation in burning rate existing for the various

units.

Pellet Density

No significant difference existed between the density or

weight of pellets containing a given binder for the various

delay times, nor between the pellets containing the three

binders. Likewise, no significant change in density occurred

after curing for five and 30 days. The density of the pellets

was approximately 1.700 gm/cc, with less than a 3% variation

! wt..n tWhe units uotinig the Three resins.

V. SUMIARY

Of the three resins investigated, the optimum binder for

use at room temperature curing conditions appears to be

Laminac 4110, when it is considered that the function of a

binder is to supply physical strength to the pressed compo-

sition while at the ssme time impart a minimum amount of

dogradation to the performance of the flars. The burning

performance of tho Aropol flares compared favorably with the

Laminae 4110 units; however, the relatively poor physical

strength properties of the Aropol pellets after both five

and 30 days curing, make this resin inferior to Laminac 4110.

11

RDTR- No. 51

A comparison between the two Laminac resins indicates that

after an eXtended curing period, the two compare favorably

in physical strength; however, after only five days ambient

cure, the Laminac 4110 units possessed superior strength

properties. Also, the number of candlepower-seconds emitted

by the Laminac 4110 flares was about 12 greater than for the

4116 units.

The results of this study also indicate that a short

elevated temperature cure will substantially increase the

tensile and shear strength of the compositions investigated,

compared to a short ambient cure. However, for the Laminae

resins, it appears that units cured 30 days ambiently have

significantly higher physical strengths than units subjected

to a 16 hour 150*F cure and then cured ambiently for the

remaining 29 days. Theoretically, the Aropol resin should

have cured at 75 - 850F; however, considering the physical

strength data after the 150°F cure. it is evident that this

resin did not cure substantially at room temperature.

VI. CONCLUSIONS

1. Laminec 4110 was found to be a superior binder com-

pared to Laminae 4116 and Aropol 7720M, considering both

physical strength and burning performance of pellets and

flares, respectively.

12

.RDTR No. 51

2. Aropol 7720M exhibited poor binding properties when

cured at room temperature but compared favorably with the

Laminac resins when cured at 150OF for 16 hours.

3. Of the three resins investigated, Laminae 4110 will

impart superior tensile and shear strength to the pressed

composition after several days ambient oure; however, after

approximately 30 days the two Laminac resins possess essentially

the same physical strengths.

4. Flares containing the Aropo ??20H and Laminac 4110

resins emitted a significantly greater number of candlepower-

seconds than the units containing Laminae 4116.

5. The burning time and candlepower of flares decreased

and increased respectively, a significant amount, as the delay

time between mixing and pressing increased.

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RDTR No. 51

TABLE V

EXPERIMENTAL DATA - PELLETS CURED AT 1500F

5 Day 30 DaYBinder Tensile Shear Tensile Shear

215 lbs. 1308 lbs. 210 lbs. 1230 lbs.

Laminac 4110 250 " 1425 " 180 " 1275 "- 1500 " - 1180

234 lbs. 1375 lbs. 260 lbs. 1455 lbs..iloaminac 4116 184 " 1215 " - 1395

- 1460 " - 1475 "

360 lbs. 1690 lbs. 570 lbs. 1740 lbs.Aropol 7720 427 " 1870 " 510 ' 1705

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U Security lass~iilcaton

1 I- ORIGIRATIN G ACTIVITY (C~e'WX* a mdhar) a Xj73CRT" A2FCTOU. S.0 Naval Anruniticn Depot TULS iCrane, ID~iana bGRU

3. EPRTTILEBinding Properties and Other Characteristics of Several PolyesterResin Binders Used in Pyroteohnio Formulations

4. DESCRIPTIVE NOTES (7flpe o at apo acd Inclsive. date&)

S. AUTHOR(SI (Lat name. Riet gna, jsitfi)

Haas, Davay

5. REPORT DATE 7a. TOTAL NO. Or PAGES 7lb. no. air vRFs

28 Cztobor 1966 J28a~sc. CONTRACT OR CRANT NO. it. ORIGtHATOnRs AREPRy Nu"39t)

b6 PROJECT NO. IRERTR .10. 51-2b. OTH=FREORT tic(S (Ani yoiernmeer fiat ft.7bo 8841f90

V-~ 10. AVAILABILITYLIMITATION NOTICESUnlimited

1 11. SUPPLEMENTARY NOTES M2 SPONSORING MILITARY ACTIVITYU. S. U'aval Amrsunition DepotCra3ne, LIndiane

13. 8STRCT he binding strenths of peillts subjected to tensile end. shear stresses,

and the burnins tim- and candlepower of" flares Dressed frc- ccompcund aged 0-6hcurz in incrementz of one hour prio to prsigDe~oe~ndatrcrnperiods of 5 erd 30 days. Three fonnula-tions were used, ench cona~ining the semmeratio of maegnesium/sodium nitrate/binder; buit, with threee different polyester

resin binder-sr-Lerninac- 41]0, Lainae 41-16, -and Aropol 7720~.1I The variationsin physical strength, :IarA~epo.zer, and butning -9z withrespect to delay time between mixing and pressing were £o'un4 -to be greates-v forpellets and candles containing J.zininac 4110. Likewise, the physical strength.4 of pallets containing Laminae 4110 was significantly higher thaan the other pallet4Rte curing 5 days; however, tests after 30 days indicated that by thi;s tZ~ hLamninac 4115 had essentially fully cured, ard now had binding properties similar1to Laminac 4110.. The- physical strength of pellets cured at 75 - 850-P with Ar-opol7IO onsdrably less that; pellets containing the- other bincders~.

f-All units cured for 16 ho-irs- at, 150cF, and then tested after 5 days4 exhibited oonsiderably higher strengths than pellets not subjected to an elevated1'tempe-rature. However, t.ests after 30 days showed that for the Umminao birders,

greater- binding strn-ngth is obtained by curing at room tenperature for the dura-I tion of tho curing cycle. -

[ DD zFORM 14'"200o.bo ~~siiSecurity ClassiUicatioO

W1___ _____________

S e c u rity C la s s ific a tio n ..... . ...... ...... .. .._ _14 . LINK A LINK B LINK C

KEYWORDS ROLE wT ROLE WT ROLE WT

1. Flares, Physioal Strength2. Flares, Burning Charateristics3. Flares, Binders4. Flares, Aging5. Flare Composition, Aging6. Binders, Physioal Properties i

INSTRUCTIONS

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2b. GROUP: Automatic downgrading Is specified In DoD Di- users shall request throughrective 5200. 10 and Armed Forces Industrial Manual. Enter uetthe group number. Also, when applicable, show that optional " Imarkings have been used for Group 3 and Group 4 as author- (4) "U. S. military agencies may obtain copies of this 3ized. report directly from DDC. Other qualified users -=

3, REPORT TITLE: Enter the complete report title in all shall request throughcapital letters. Titles in all cases should be unclassified. -."If a meaningful title cannot be selected without classifica-tion. show title classification in all capitals In parenthesis (5) "All distribution of this report Is controlled. Quai-

i'medlately following the title. ified DDC users shall request through

4, DESCRIPTIVE NOTES: If appropriate, enter the type of ,"report, e.g., interim, progress, summary, annual, or final. If the report has been firnished to the Office of TechnicalGive the Inclusive dates when a specific reporting period itt Services, Department of C0nmerce, for sale to the public, Indi-covered, cate this fact and enter th& price, if known.

5. AUTHOR(SY Enter the name(s) of author(s) as shown on IL SUPPLEMENTARY NOTES: Use for additional explna- _or in the report. Enter last asme, first name, middle initiaL tory notes.If military, show rank and banch of service. The name ofthe principal 1 -hor is an ahsolute minimum requirement. 12. SPONSORING MILITARY ACTIVITY: Enter the name ofthe departmental project offlce or laboratory sponsoring (pay-6. REPORT DATE: Enter the date of the report as day, ing for) the research and development. Include address. ---month, year, or month, year. If more than one date appears 1con the report, use date of publication. 13. ABSTRACT: Enter an abstract giving a brief and factual

summary of the document indicative of the report, even though l7a. TOTAL NUMBER OF PAGES: The total pkge count it may also appear elsewhere In the body of the technical ,,- 1should follow normal pagination procedures, Le., enter the port. If additional space is required, a continuation sheet (shall 5-4-0number f pages containing information, be attached.7b. NUMBER OF REFERENCES: Enter the total number of It is highly desirable that the abstract of classified ritports Ireferences cited in the report. be unclassified. Each parigraph of the abstract ahall end with

So. CONTRACT OR GRANT NUMBER: If appropriate, enter an indication of the military security classification of thu In-the applicable number of the contract or grant under which formation in the paragraph, represented as (TS), (S), (C), or (U).the report was written. There is no limitation on the length of the abstract. How- -_

8b, 8c, & 8d. PROJECT NUMBERo Enter the appropriate ever, the suggested length is from 150 to 225 words.military department identification, such as project number, t msubproject14. KEY WORDS: Key words are

technically meaningful termsor short phrases that characterize & report and may be used as

9a. ORIGINATOR'S REPORT NUMBEP'S): Enter the offi- Index entries for cataloging the report. Key words must be _Jcial report number by which the docurce a will be identified selected so that no security classification Is required. Identi--and controlled by the originating activ This number must tiers, such as equipment model designation, trade name, militarybe unique to this report. project code name, geographic location, may be used as key9& OTHER REPORT NUMBER(S): If the report has been words but will be followet' by an indication of technical con-

assigned any other report numbers (either by the originate text. The assigm! rrle, and weights Is optional.

or by the sponsor), oleo enter this number(s).

10. AVAI.ABILITY/LIMITATION NOTICES: Enter any l1m-Itations on further dissemination of the report, other than thosel

.Security___issii__ _ I

Security Classification J