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ADB803014
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CONFIDENTIAL
Approved for public release; distribution isunlimited.
Distribution authorized to U.S. Gov't. agenciesand their contractors;Administrative/Operational Use; 16 SEP 1943.Other requests shall be referred to Office ofScientific Research and Development,Washington, DC 20301.
OSRD list 31 dtd 5-9 Aug 1946; OTS index dtdJun 1947
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AIR DOCUMENTS DIVISION
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HEADQUARTERS AIR MATERIEL COMMAND
WRIGHT HELD. DAYTON, OHO
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^.GOVERNMENT IS ABSOLVED
FROM ANY LITIGATION WHICH MAY
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FRINGING ON THE FOREIGN PATENT
RIGHTS WHICH MAY BE INVOLVED.
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Division 8
NATIONAL DEFKSE RESEARCH COMMITTEE
of the
OFFICE OF SCIENTIFIC RESEARCH ADD DEVELOPMENT
•
: ■ i
I
1
053D Ko. 1804.
Cony Mo. 42
:
nONFJDFNT i*i
DIVISION 6
NATIONAL DEFENSE RESEARCH COMMITTEE
OF THE
OFFICE OF SCIENTIFIC Rl&EARCH AND DEVELOPMENT
Progress Report on "The Preparation of Pentaerythritol"
to "
September 1, 2.945 ,.'.,■■•;'■ by
Robert C. Elderfield
Report OSRD No. l8o4
■. Copy No. /J4
WWDENTIAL
0atw September 16, 1043
Copies No. l Copy No. 29 .
Copy No. 30 -
Copy No. 31 .
Copies No. 32
34 - 3" 3
NDRC
?f: U 39
Copy No, Copy No. Copy Ho. Copy Bo. Copy No. Copy No.
Copy No. 4o - copy No. 41 . Copy No. Kz . Copy No. £.3 _ Copy No. 24 - Copy No. 45 _ Copy No. 46 _ Copy No. 47 .
through 28 - Dr. Irvin Stewart Office of the Chief of Ordnance, Attnt Liaison Officer
Office of the Chief of Ordnance, Attni Dr. L. R. Littleton
Commanding Officer, Plcatlnny Arsenal, Attnt Technical Croup
and 33 - Chief of the Bureau of Ordnance, Attnt Ammunition Research Section Division 8 Files Dr. G. B. KistiaJcowsky Dr. Ralph Connor Dr. H. C. Elderfield Dr. Russell McGill
Office of the Chief of Ordnance, Attnt 'Mr* J. B. Washnock
Copy No Copy No 49-
Copy No. Copy No. Copy No. Copy No. Copy No. Copy No. Copy No. Copy No. Copy No.
50 51 52
Total Number of Copies - 58
11
CONFIDENTMff?
. ,,. Aft; ■■'& ~l
>
CONFIDENTIAL OSHD No. lSOij.
DIVItlOW 8
NATIONAL DEFENSE ifflBnffflH CO.IIMITTEE
OP THE
OFFICE OF SCIENTIFIC RESEARCH AND DEVELOPMELJT
Section 8.2
Progress Report on "The Preparation of Pentaerythritol'1
Service Directive OD-58
.
••
I • ■, * « ■. ■
. ■
1
■
Endorsement (1) Dr. Ralph Connor, Chief Section 8.2 to Dr. 0. B. Kistiakowsky, Chief Division 8. Forwarding re- port and noting:
"In connection with the work of Division 8 on OD-58, it seemed probable; that the by-products formed with pentaerythritol might be important in determining the thermal stability of PETN and Pentolite. The initial research on this work, there- fore, dealt with methods of preparation of pentaerythritol and methods for its - analysis.' This report describes these experiments, which were not, in themselves, significant but which contributed to the further study of this subject which has been reported in OSRD 1J4.I4. and will be further described in subsequent reports."
(2) from Dr. G. B. Kistiakowsky, Chief Division 8 to Dr. Irvin Stewart, Executive Secretary of the National Defense Research Committee. Forwarding report and concurring in the above endorsement.
This is a final report under Contract 8-19!;, OEHsr 221; with Columbia University.
,
CONFIDENTIAL 1
. 4*
0$® «Jfl^
' TAELü OF OOETENW
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■
; • ! , v < •
•
•
Introduction »Pago 1,
Dlacuaaion.. • •• «.Pago 2«
Exporlmonta on tho Prop-rr-tlon of Pontaorythritol... «Pago 8«
A 1 V 9
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mmopgcTiON
It has been noticed on several oeoaslons by those con-
cerned that the quality, in particular the stability, of
PSTN .and Pentolite is apparently adversely affected by the
presence of impurities in the pentaerythritol used for the
preparation of PSTN* Information at hand concerning the
nature of such impurities, and tho specific effect of
Individual impurities is scanty and conflicting* The present
report describes work directed toward the production of good
quality pontaorythritol by variation in tho experimental
conditions and reactions used»
In available studies on the preparation of pontaory-
thritol (British Report A.C. 117; Org»/Ex. 27; NDRC No. B-88; ■ ■ ■
British Report, R.D. Woolwich D. 906; NDRC No. B-171; NDRO
Serial No. 86), tho yiold of product has boon arrivod at
by estimation of tho amount prosont in solution at tho
ond of tho roaction and, with but a fow oxcoptions, tho
quality of tho product with rospoct to difficultly removablo
by-products has had no attention» In tho prosont study
tho product has boon lsolatod in all oasos and its purity
dotermlnod by a variety of methods*
NnL.'tWW
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I V •
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8.
DiacusaioM
Analytical Method»
A number of analytical methods have been used in the
past Tor estimating the purity of pentaerythritol. The
method finally adopted as standard in this work la the so-called
bensylidene method described In detail In British Report A.C.
117; Org./Ex. 27* In order to secure satisfactory reproducible
results slight modifications havo bean necessary. As finally
worked put, the procedure is as follows:
A sample of between 0.4800 and 0*5200 g. of pentaerythritol
(Note I) in a 125 ml. Erlenmeyer flask is dissolved in
5 ml« of water by warming, and the solution is cooled
to room temperature* To this solution is pipetted
10 ml* of a solution made up by dissolving 20 ml* of
freshly distilled bonsaldehydo in 100 ml* of 87J6"
alcohol (9*2 ml* of water addod to 100 ml* 95jf alcohol) '■
and 20 ml* of hydrochloric acid* sp* gr* 1*16 (22*5 ml*
of wator addod to 100 ml* of hydrochloric acid, sp* gr*
1*19* This reagent was made up fresh every sooond day*
Within a fow minutes, the benzylidono derivative of
pentaerythritol separates. The tightly stoppered flask
is allowed to stand for four hours (Note 2) at room
temperature with occasional shaking* To the crystal mush
is then added 30 ml, of potroloum othor (Skolly Solve B>
.&'-&'-»
■\
nnd the ndxturo is shaken very vigorously by hand»
Tho tomparaturo of tho mixture is thon brought to
250+1° (Koto 3) and tho procipltato of bonzylidono
dorivativo la filtorod by suction on a tared frlttod
glass Ooooh oruoiblo and waohod vdth 150 ml» of wator.
Aftor drying for 1 hr. at 95° tho procipltato is woighod«
From tho wolght of tho bonzylidono compound tho weight
of pontaorythritol la calculated with tho aid ot tho
graph shown in Figuro 1, (Hoto 4) and tho poroont of
pontaorythritol in tho sample is oalculatod. Tho
accuracy Is +0.4 porcont«
Mo to 1» It has boon found that if tho samplo taken bo outaldo
this rango, variable results aro obtained«
Noto 2, Four hours is tho minimum timo roquirod to give
satisfactory results« Hoto 3« It is important that tho procipltato bo filtorod
at this tonporaturo. Deviations thorofrom givo variable
rosuits. Chilling tho crystal muah to 0° in loo as has
boon rooommondod by Wolfrom ha» boon found to lead to
variablo rosults, oausod apparontly by varying timo of
filtration from dotornination to dotormination* In oasos of
slow filtration, tho ohillod solution warms up. This loads
to low rosults by virtue of inoroasod solubility of tho
prooipitato. Since an arbitrary onpirioal oorrootion for
!•' Igtrfl—!*
4.
•>
solubility ia applied, It Is therefore Important to filter
at the sane temperature consistently.
Note 4« This ourve differs somewhat from a similar one given
In British Report A.C. 117; Org./Ex. 27, and has been obtained
by repeated analyses of mixtures of known composition.
The above procoduro has boon used in somo 200 determina-
tions, all dono in duplicate. Tho results oro within the
limit given above«
I
Prior to the adoption of tho benzylidono method an
attempt was made to apply a conductorst/c method baaed on tho
report of Boosokon (Roc. Trav. Chim. 30, 400 (1911); Bor»
46. 2619 (1913) ) that dipontaorythrityl othor doos not
inoroaso tho oonduotlvity of a solution of boric aoid whoroas
pontaorythritol doos to a throo or four fold oxtont. In
sovoral oxporimonts, no significant difforonoo in oonduotlvity
of borio aoid eould bo notod on addition of oithor of tho
abovo substanoos.
Wo havo also usod tho tost nitration assay method and tho
spent aoid stability mothod suppliod by tho DuPont Company
in a fow oaaos. In this mothod tho yiold and molting point
of PETN is dotormlnod aftor a standard nitration and
purification procoduro. Tho spont add is hoatod at 60° C.
and tho time to tho appoaranoo of gas bubblos on tho walls
~ 'V&l $"":'• — \t" ■
■>
':''■'.
■v
of tho tu'oo is noted» Tho proooduro la at follows i
Ton grams of flnoly powdorod pontaorythritol is
addod to 46*8 g, of 95% whlto nitric acid at such a
rato that tho tomporituro doos not oxoood 32° C,
with good stirring« Extornr.l cooling Is nooossary«
This takos about 10 min. Tho mixturo Is thon stlrrod
for an additional 10 min., coolod to 80°, filtorod
on a sintorod glass funnol and suekod as dry as
possible* Tho spont add is troatod as
doscribod bolow. Tho PETN is washed on tho funnel
with two portions of wator, onoo with 6% sodium
oarbonato solution and finally with wator« Tho orudo
PFTN is dissolvod in hot aootono (about 100 ml«) and
0*5 g« of anhydrous sodium oarbonato is addod« While
still hot« 3 volumos of wator aro sprayod in to the
well stlrrod aootono solution« Aftor cooling to
80°, tho PETN is collected and dried in a desiccator.
Tho yield and molting point aro dotorminod«
Tho volume of spont acid is dotorminod and 6 ml»
aro withdrawn, placod In a tost tube and hoatod in
a boaleor of wator at 60°+l°. Tho tin» in minutes
to tho appoaranco of gas bubblos on tho walls of tho
tubo is noted«
Tho remainder of tho spont aoid la drowned in
4 volumos of loo« Aftor standing, tho somowhat gummy
'*•. A ■*»*#
» A
U- "">
6.
. i
preoipltate 1« filtered on a tared fritted glase
Ooooh crucible, dried In a deslcoator and weighed.
The comparative results of analyses of a number
of samples of pontaorythrltol by tho three methods
are given In Tablo 1, In which tho samplos Include
synthotlo mixturos, a commercial product suppllod by
DuPont, and sovoral laboratory batches which are
Identified In Tablo II. It appoars that some incon-
sistencies botwoon tho raothods oxist, from itoich wo
foel that tho benaylidono method gives the only
aoourato indication of tho percentage of pontaorythrltol
In a givon sample. On tho othor hand, tho spont acid
stability may bo dooidodly misloadng (oomparo Run 19a
with PE-dlPB containing 6% of di-PE). Likewise, tho
residue obtained on drowning tho spont add appoars to
bo variablo and is possibly lnfluonood by tho nature
of tho impuritios proaont.
^■■■pJ'fV-
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Pontaory- M.P. thritol of• Usod P.E.
Synthotio 252-4° mixturo
contg; 5% dl-PE.
Ditto ' 231-40 contg«
di-PE
Run 20 246-520
Run 19a 258-61°
Nlacot • 255-8° Chora. Co. Lot No. 300-570 Nitratod at Ropauno to PETN Lot No. 891.
Run 14 256-8°
Run 21 236-48°
LFH No. 2 256-8°
Tablo I.
Yield M.P 4 Spont Spont Bed.' of of Acid Acid Anal.
rocry- PETN Stabil- Rosiduo stal ity in (# of PETN rain. PE (in usod) points 1
227 139.5- 141. 40 25,0 4.6
201 139-141.5°
211 139.8-141.2°
228 140.3-141.3°
222 140.8-1420
11«5 10«2
• • 7.5 5.6
1 I
11.0 1.0
7,0 4.4
229 140.2-1410
201 140-141°
219 ,139.5-1400
88. 8#
97.25g
95,1%
3.0 2.4 92. 3#
15.5 7.4 87. 3#
2.9 95#
r ■\
8.
EXP3RIMEHT3 OH THB PREPARATION OP PBNTAERTTHRITOL
.«..
■
A largo numbor of oxporinonts havo boon porformod In ordor
to ascortain tho offoot of tho following varlabloo on tho quality
of tho PB produced: Ordor of addition of roactants, i«o.f
aldohydoa to lino or lino to aldohydos; uso of calcium oxide
vs. calcium hydroxide; uso of acotaldohydo as such or as aldol
or orotonic aldohydo; uso of fornaldohydo as formalin or
parofornaldohydo; influonco of tho so-callod "sooond reaction"
and tho tino olapsod aftor tho onsot of tho "sooond roaction"
boforo neutralization of tho roaction nixturo*
In all easos tho method of working up tho roaction mixturo
and of isolating tho product was tho sane: Sulfurlc acid
oquivalont to 96 porcont of tho calciun prosont was addod to
tho woll-stirrod roaction nixturo* Aftor filtration and thorough
washing of tho procipitatod calciun snlts, tho filtrato was
ooncontratod undor roduood prossuro until oxcossivo bunping .
causod by separation of PE provontod furthor concentration,
Aftor rofrigoration, tho PE was flltorod off and tho filtrato
furthor oonoentratod until tho final voluno was about 4 porcont
of tho original* A sooond crop of PE was ronovod and combined
with tho first* Tho orudo PE was rocrystallisod onoo fron tho
nininun amount of boiling wator with uso of docolorizing carbon*
Yiold, analysos and othor data woro takon on this onoo roorystalllz@4
material oxoopt as notod*
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In all runs the proportions of reaotants ware kept
eomtant and in the ratio or 5.5 mola of formaldehyde, 1 • • • mol of aoetaldehyde and 0*6 mols of lime in 1.5 L. of water«
In oases where formalin was used the formaldehyde oontent
was determined; when paraformaldohyde was used, it was assumed
to be equivalent to 100 percent formaldehyde; aldol and
orotonic aldehyde were assumed to bo equivalent to 100
percent aoetaldehyde. The runs were of threo sizes, those
through No. 17 except No. 14 boing done in 3200 oo. of water, a ■
from 18 to 85 and No« 14 in 10 L. of water« In order to get
a line on a still larger sized run, No. 86 was done in 58 L,
of nator.
The results of a numbor of typical runs are shown in
Table II. F refers to poraformaiaohydo, P to formalin«
Ao to aoetaldehyde, Al to aldol and Cr to orotonio aldehyde«
Comments
1. Order of addition of roaotantsi It appears from Runs
80 and 81 that addition of tho mixed aldehydes to the limo
water rosults in a somewhat highor yiold of PH. but that tho
quality of tho product la dofinitoly lower«
8. Calcium oxldo vs. calcium hydroxide: In all oasos
finely powdered limo was usod, so that it presumably hydrated
substantially instantaneously. No study of the uso of lump
limo was made«
yi. «i*--,**»
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10.
5. Acot-.aldohydo vs. aldnl vs. erotonlo aldehyde» All throo
give zooc. qaillty r£ although tho yiold obtalnod wiMi c-otonio
aldfifyte is nerkodJ.y loss than with acotaldohyäo or sldol»
For oonvonionco la handlir.3, nldol Is much to to preformed,
4^ Porafennaldehydc cr forrallr: Without further work
this point cannot to an&v;orod doflnitoiy, although tontatively
It can IXJ said bhat To./ dlfforoncos arico from bho uso of ono
or tho other with rospoct to qxallty. Tho yield Is battor
with paraformaldohydo, Howovor, tho uso of paraformaldohydo doos prosont ono
striking advantago from a practical point of vlow. Apparontly
tho dopolymorlzatlon of paraformaldohydo Is acoomponiod by
oonsldorablo absorption of ho at, which roduooa materially
if not oomplotoly tho rofrigoration roqulrod to control tho
reaction when formalin is usod. This is brought out by tho
dotails of Runs 22 and 23, In both oaaos tho roaction was
eorriod out in a 22-U Pyrox precipitating Jar, tho mixturo
being woll stirred mechanically and a ooil of copper tubing
was usod for tomporaturo control when nooossary. 3.0 L. of
wator, 288 g. of aldol, 1080 g. of paraformaldohydo (or an
oquivalont amount of formalin) and 246 g. of calcium oxido
wore usod. Tho limo was addod to tho mixod aldohydos gradually
as lndioatod»
!F¥
3.1»
Tino In tiiin« Tonpo Run 22
Tornp«. Run 23
0 27° 250 addition of 11,no sfcartod
2 23r5 24.5
4 23 27
6 24 30
8 27 33
12 35 42
14 43 —
16 46 -I [ Uno all in) 48
30 48.5 50.5
40 48.3 51 -(lino all in)
45 59
50 53 - 2nd r*o action 62 - ovor nddod HgS 04
Snd ro act ion ovor addod H„S0„
2 4
It is obvious that a riuch lowor tomporri-fcuro provailod In
Run 22. VVhilo no cooling was noooaaary in oithor run. on ex.
larger scalo a run sicilcr to Run 23 would probably roqairo
cooling. In Run 26. givon in dotail bolow, lnoating was nocossary
in ordor to raise tho tonporatviro sufficiently for tho second
roaotion to start«
Run No-. 26
Since this was tho largest run attonptod and can bo oxpoctod
to givo somo idoa or what can bo oxpoctod on a still largor scale,
f A i J W
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12.
tho rocord ia givon Jr. dotail.
Tho vossol wa3 a 25 gal. crook oquippod with good moohanical
agitation and a coppor coil for cooling or hoating. ->
Matorialot Si'. L, wator ""~~~~ 53CiC jjMe parafor-ialdohydo
15C0 gai aWol Jtochnlcol) ■ ' 1879 gn. oalciuri oxido, powdorod C.P.
Tho lino was addod gradually to tho 3lurry of aldohydos»
Tino in Hin.
0
5
10
20
30
40
50
60
70
75
90
110
115
117
120
To:.ip.
22°
20
«1
23
23
26
31
36
40
41
49
50
53
55
55.5
Ronorlu
Start adding lino.
All paraforn had di3solvod loaving a oloar solution.
lino all in.
Stoan put through coil.
Stoan turnod off.
Sooond roaotion 3tartod.
Stoppod by adding HgSO
• .'.
18.
"1
Tho flltrato from tho caloiun salts was workod up as
doscribod abovo, oxoopi; that bocause o.f tho mount of natorial
it was noccssary to connen'jrico in batoncs.» Tbo jriold of not
rocrystalllzod natortil .TH 2850 3. or fc-i to:-contr This was
roerystallizod fron 8 L. cf wator ;loic'i.tvg 1523 3. of PS which
noltod at 258-9° and c>nf.yjl 96, S J.. rO:ic r:oshor liquors woro
ooncontratod and gavo 824 ö-. noro PD •v'v.ch noltod at 248-54°
and as3ayod 91#. & third -;rop of r.ia\orinl -.loiting at 228°
and woighing 450 g. wa3 obtained on j/ur-rho.« concentration of
tho raothor liquors«
5. Tho "socond roaction": It appears tc to q-uito
dofinitoly oatablishod that unloss tho 30cond reaction ttJcos placo,
tho quality of tho PE suffors vory groatly and tho yiold docroason»
Whilo tho chonistry involvod in tiio sooond roaction i3 obscuro,
tho fact ronains that in no caso whoro tho socond roaction was
not allowod to tako placo, was a satisfactory product obtainod.
It is roconnondod that, if opportunity prosonts itsolf, a dotailod
study of this roaction bo undortakon.
Tho tino olapsod aftor tho onsot of tho socend roaction
until working up appoars to bo relativo?y -jiiinpor-car.t» Tho
roaction is charactorizod by a suddon riso in tonporaturo followod
shortly by tho dovolopnont of a yollow color in tho roaction nixtuii
It nakos littlo diff oronco whothor tho roaction is worked up a
fow minutos lator or as nuch as two hours later»
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Wotoa to Tablo II
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1. Crudo product "was sliny and oould not bo roadtly roorystdllzod« Yiold waa dotonnlnod in solution,
2. Hydrochloric acid usod to noutraliza instoad of sulfurio«
3. Twico usual eoneontration of all ro act ants.
4. Matorial fron Run 19 roorystallizod a sooond tino»
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ALrn;' 2992:~.-- . 11
... ~. ~---=tr--ce: :~:omr: L
TITLE: Progress Report on "The Preparation of Pen!Aerythritol" to September I, 1943 (NQJt.JS,-.1
1-""=••""· •""•"'"''(:,:~r.:,J•~-~ AUTHOR(S): Elderfield, Robert C. • ORIGINATING AGENCY: Columbia University, New York, N. Y. PUBLISHED BY: Office of Scientific Research and Development, NDRC, Dlv B PUIIUSHINO AGENCY NO,
OSRD-1B04 COUNnY
u.s. I I PAOU IIUUS~~~HS 16 ~<raohs
ABSTRACT:
The quality;'and in particular the stability, of PETN and Pentolite Is adversely affected by the presence of Impurities in the pentaerythritol used for the preparation of PETN. A description Is given of the work directed toward the production of good quality pentaerythritol by variation In the experimental conditions and reactions used. Experiments on the yield of pentaerythritol have shown that, the addition of the mixed aldehydes to the lime water results in a somewhat higher yield of PE, but that the quality of the product is lower. Aldol is preferred to acetaldehyde and crotonic aldehyde for ease of handling, and the yield obtained with acetaldehyde and aldol Is greater than that obtained with crotonic aldehyde. The yield was found to be greater with paraformaldehyde than formalin although there were few differences with respect to quality.
DISTRIBUTION: Copies of this report obtainable from Air Documents Division; Attn: MCIDXD
ClNcO~m"~menL~J -~-@J- I SUBJECT HEADINGS: Explosives- Production (34511); 6 = D 0 O o 11 Explos}ies - D~velop'fent (34504. 7) ·~ ,.,... j'
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