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United
S t a t e s P a t e n t 0
1
3 , 3 5 4 , 0 1 0
FLEXIBLE EXPLOSIVE CONTAINING RDX AND/
OR
HMX
AND
PROCESS THEREFOR
J o h n D . H o p p e r , S u c c a s u n n a , a n d
F r a n k l i n B .
W e l l s ,
H a c k e t t s t o w n , N . J . ,
a s s i g n o r s
t o
t h e
U n i t e d S t a t e s o f
A m e r i c a a s r e p r e s e n t e d b y t h e S e c r e t a r y o f t h e Army
No
D r a w i n g . F i l e d J a n . 2 7 , 1 9 6 7 , S e r . N o . 6 1 2 , 7 6 6
5
C l a i m s .
( C l . 149—18)
ABSTRACT OF
THE DISCLOSURE
A
ethod f o r t h e p r e p a r a t i o n
o f
a s e l f - s u p p o rt i n g h i g h
p o w e r ,
? e x i b l e s h e e t e x p l o s i v e o f l o w i m p a c t s e n s i t i v i t y
c o m p r i s i n g t h e s t e p s o f m i x i n g a
h i g h
e x p l o s i v e f r o m t h e
g r o u p
c o n s i s t i n g
o f c y c l o t e t r a m e t h y l e n e t e t r a n i t r a m i n e
(HMX),
c y c l o t r i m e t h y l e n e t r i n i t r a m i n e ,
(RDX)
a n d
m i x
t u r e s t h e r e o f ,
w i t h
a p l a s t i c i z e r t o
form
a
p a s t y m a s s ,
m i x i n g
i n t o s a i d p a s t y
m a s s a h i g h v i s c o s i t y ,
a l c o h o l - w e t
n i t r o c e l l u l o s e
c o n t a i n i n g a b o u t
12% n i t r o g e n a n d a p i g
ment
f o r camou?age p u r p o s e s , a d d i n g
e t h a n o l t o t h e mix
t u r e
t o form
a
s t i f f
dough
a n d
t h e n
m i x i n g and r o l l - m i l l i n g
s a i d
dough a t
a b o u t
1 3 5 °
F . t o
form
a ? e x i b l e
s h e e t
e x
p l o s i v e .
T h i s i n v e n t i o n i s a
c o n t i n u a t i o n - i n - p a r t
o f o u r p e n d i n g
a p p l i c a t i o n
S e r .
N o . 5 0 5 , 4 4 5 ,
? l e d
O c t . 2 7 ,
1 9 6 5 ,
now
P a t e n t No. 3 , 3 1 7 , 3 6 1 , and r e l a t e s t o an e x p l o s i v e com
p o s i t i o n and more p a r t i c u l a r l y c o n c e r n s a ? e x i b l e , s e l f
s u p p o r t i n g ,
w a t e r - r e s i s t a n t
e x p l o s i v e
a n d m e t h o d
f o r
i t s
p r e p a r a t i o n .
Our c o m p o s i t i o n c o m p r i s e s a p a r t i c u l a t e e x p l o s i v e
a n d
a p l a s t i c i z e d
b i n d e r ,
t h e c o m p o s i t i o n b e i n g u s e f u l
i n e x
p l o s i v e
m e t a l - f o r m i n g p r o c e s s e s
a n d a d m i r a b l y
w e l l s u i t e d
f o r d e m o l i t i o n p u r p o s e s . The c o m p o s i t i o n i s c h a r a c t e r i z e d
f u r t h e r
b y
s a f e t y i n h a n d l i n g , a n d i t may
b e f o r m e d
r e a d i l y
i n t o
a n y
d e s i r e d
s h a p e
a s b y r o l l i n g , e x t r u s i o n ,
c o m p r e s
s i o n - m o l d i n g , e t c . i n t o s t r i p s , b l o c k s , s h e e t s ,
a n d
t h e l i k e .
I t i s
t h e r e f o r e
an o b j e c t o f
t h i s
i n v e n t i o n t o
p r o v i d e
an
e x p l o s i v e h a v i n g t h e a f o r e m e n t i o n e d
c h a r a c t e r i s t i c s .
Another
o b j e c t o f
t h i s
i n v e n t i o n i s
t o p r o v i d e a
? e x i b l e
e x p l o s i v e
o f h i g h p o w e r ( a t l e a s t t h e e q u i v a l e n t o f TNT)
a n d b r i s a n c e ( r a t e o f d e t o n a t i o n a t
l e a s t
a b o u t 7 , 0 0 0
m . / s e c . ) .
S t i l l a n o t h e r
o b j e c t
o f
t h i s
i n v e n t i o n i s
t o p r o v i d e an e x
p l o s i v e
w h i c h ,
i n
s h e e t
f o r m ,
p o s s e s s e s
s u f f i c i e n t ? e x i b i l i t y
s o
t h a t
i t
may
e made
o
conform t o t h e contour of
u n
even
s u r f a c e s w i t h a minimum o f m a n i p u l a t i o n , t h u s a i d <
i n g
i n
t h e
c o m p l e t e
d e s t r u c t i o n o f t h e
d e v i c e
t o
b e d e
m o l i s h e d .
A
u r t h e r o b j e c t
o f t h e i n v e n t i o n i s
t o
p r o v i d e a ? e x i b l e
e x p l o s i v e h a v i n g
h i g h
r e s i s t a n c e t o i m p a c t a n d f r i c t i o n
w h i l e
r e t a i n i n g g o o d
c a p s e n s i t i v i t y
c h a r a c t e r i s t i c s .
A
t i l l
f u r t h e r o b j e c t
o f t h i s i n v e n t i o n
i s t o
p r o v i d e a
? e x i b l e
e x p l o s i v e
w h i c h
i s more h e a t - s t a b l e
t h a n
s i m i l a r
m a t e r i a l s c u r r e n t l y a v a i l a b l e .
Y e t a n o t h e r o b j e c t o f t h i s i n v e n t i o n
i s t o
p r o v i d e a ? e x
i b l e
e x p l o s i v e w h i c h i s
n o t a d v e r s e l y
a f f e c t e d b y w a t e r .
A n a l
o b j e c t
o f t h i s
i n v e n t i o n
i s t o
p r o v i d e
a n e x p l o
s i v e
o f s u ? i c i e n t r e s i l i e n c y s o t h a t ,
when
made
i n
b l o c k
o r
o t h e r
m a s s i v e f o r m ,
i t
w i l l
r e s i s t
b r e a k i n g
u p
upon
im
p a c t
w i t h a
h a r d s u r f a c e wh e n s t r i k i n g
s u c h a
s u r f a c e w i t h
a
v e l o c i t y
o f a t l e a s t
1 5 0
f e e t / s e c o n d .
O t h e r
a n d f u r t h e r o b j e c t s o f t h i s
i n v e n t i o n w i l l become
a p p a r e n t
a s
t h e i n v e n t i o n i s f u r t h e r d e s c r i b e d
h e r e i n a f t e r .
We a v e f o u n d t h a t t h e
f o r e g o i n g
o b j e c t s may
‘ b e a t
t a i n e d
t h r o u g h
p r o v i s i o n o f a n e x p l o s i v e c o m p o s i t i o n com
p r i s i n g
a b o u t 45-76%
o f t h e
c y c l i c p o l y n i t r a m i n e s
c y c l o
t e t r a m e t h y l e n e t e t r a n i t r a m i n e ,
h e r e i n a f t e r
r e f e r r e d t o a s
HMX, a n d / o r c y c l o t r i m e t h y l e n e t r i n i t r a m i n e , h e r e i n a f t e r
10
1 5
20
25
30
40
50
55
60
65
7 0
3 , 3 5 4 , 0 1 0
P a t e n t e d N o v . 2 1 , 1 9 6 7
1C6
2
r e f e r r e d t o a s RDX, t h e s a i d HMX n d / o r
RDX
a v i n g
an
a v e r a g e
p a r t i c l e
s i z e
o f
up
t o
a b o u t 2 5
m i c r o n s ,
p r e f
e r a b l y
n o t o v e r
1 3
m i c r o n s . One h u n d r e d p e r c e n t o f
t h e
HMX n d / o r
RDX u s t p a s t h r o u g h a #200
US.
S t a n d
a r d s i e v e ,
a n d
a t
l e a s t
90%,
a n d p r e f e r a b l y n o t l e s s t h a n
97.5%
t h e r e o f ,
s h o u l d
p a s s t h r o u g h
a
#325 US. S t a n d
a r d
s i e v e .
Our
c o m p o s i t i o n
w i l l
a l s o c o n t a i n
a b o u t 1 7 - 3 9 % ,
p r e f
e r a b l y
a b o u t 25-30%, o f a p l a s t i c i z e r s u c h a s t r i b u t y l
a c e t y l c i t r a t e ( p r e f e r r e d ) , d i o c t y l s e b a c a t e , t r i e t h y l e n e
g l y c o l d i ( 2 - e t h y l b u t y r a t e ) , o r
o t h e r s i m i l a r m a t e r i a l s ,
p r e f e r a b l y t h o s e h a v i n g p o u r p o i n t s o f —40° C .
o r b e l o w ,
a b o u t 5 — 1 5 % , p r e f e r a b l y 6 — 8 % , o f n i t r o c e l l u l o s e p r e f
e r a b l y c o n t a i n i n g a b o u t 1 2 . 1 - 1 2 . 5
%
i t r o g e n a n d
h a v i n g
s u c h a d e g r e e
o f
p o l y m e r i z a t i o n a s t o have
a
v i s c o s i t y ,
u s i n g a
4%
o l u t i o n o f n i t r o c e l l u l o s e and a ‘ L y l e - i n c h d i
a m e t e r
s t e e l
b a l l ,
o f
a t
l e a s t
90
s e c o n d s
and
p r e f e r a b l y
g r e a t e r t h a n 1 4 0 s e c o n d s , a n d
a b o u t
02 - 1 0% , p r e f e r a b l y
a b o u t 0,3418%, o f
a
p i g m e n t
t o
i m p a r t a n y d e s i r e d
c o l o r
t o t h e
? n i s h e d
p r o d u c t .
I n t h e d e t e r m i n a t i o n
o f
v i s c o s i t y
a f o r e m e n t i o n e d , t h e
s t e e l b a l l
s h a l l
w e i g h a b o u t 2 . 0 2 5 t o 2 . 0 4 5
g r a m s ,
t h e
v i s c o s i m e t e r s h a l l
c o n s i s t
o f a g l a s s t u b e 1 4 i n c h e s i n l e n g t h
w i t h a n
i n t e r n a l
d i a m e t e r o f 1 i n c h , t h e t u b e b e i n g im
mersed t o
t h e
h e i g h t o f i t s l i q u i d c o n t e n t i n
a
c o n s t a n t
t e m p e r a t u r e
b a t h
m a i n t a i n e d
a t 2 5 ° :0.2°
C . , a n d
t h e
t i m e
o f p a s s a g e o f
t h e
b a l l b e t w e e n
m a r k i n g s
s h a l l
b e n o t e d .
T h e
a f o r e m e n t i o n e d
v i s c o s i t y
t e s t
i s r u n
i n a c c o r d a n c e
w i t h S p e c i ? c a t i o n
MIL-N—224A, p a r a g r a p h 4 . 4 . 5
e t s e q . ,
d a t e d F e b . 1 3 , 1 9 6 2 , w i t h
t h e e x c e p t i o n t h a t t h e q u a n t i t i e s
o f m a t e r i a l s
u s e d
a r e :
8 grams n i t r o c e l l u l o s e ,
2 1 . 3
grams
e t h y l
a l c o h o l ,
a n d
1 7 0 . 7
g r a m s
o f a c e t o n e .
The
2 1 . 3
gram/
7 0 . 7
gram a l c o h o l / a c e t o n e r a t i o i s u s e d t o main
t a i n
t h e
1 / 8 r a t i o r e q u i r e d i n t h e
s p e c i ? c a t i o n .
W h i l e v a r y i n g t h e
p r o p o r t i o n s
o f a l l t h r e e
o f
t h e m a j o r
i n g r e d i e n t s o f o u r e x p l o s i v e r e s u l t s i n some v a r i a t i o n s i n
t h e p r o p e r t i e s t h e r e o f ,
we
have found
i n a
s e r i e s o f t e s t s
t h a t , i n g e n e r a l , t h e p r e s e n c e o f l e s s
t h a n
4 5 % o f t h e
p a r t i c u l a t e
e x p l o s i v e r e s u l t s i n r e d u c e d s e l f - s u p p o r t i n g
p r o p e r t i e s
and r e d u c e d
p o w e r ;
w h e r e a s
i n c l u s i o n
o f
more
t h a n 76% p a r t i c u l a t e
e x p l o s i v e
r e s u l t s i n r e d u c e d c o h e
s i v e n e s s . A o n t e n t o f l e s s t h a n
1 7 %
p l a s t i c i z e r r e s u l t s
i n
r e d u c e d s t r e n g t h a n d c o h e s i v e n e s s ;
w h e r e a s
t h e p r e s e n c e
o f more t h a n 3 9 %
p l a s t i c i z e r
r e s u l t s i n
a
s t i c k y
p r o d u c t
h a v i n g r e d u c e d s e l f - s u p p o r t i n g
p r o p e r t i e s .
L e s s t h a n
5 %
n i t r o c e l l u l o s e
i n t h e
p r o d u c t r e s u l t s
i n
r e d u c e d
s t r e n g t h
whereas
t h e p r e s e n c e o f
more
t h a n
1 5 %
n i t r o c e l l u l o s e r e
s u l t s
i n a
p r o d u c t
t h a t
i s n o t
s u ? i c i e n t l y
m o l d a b l e . We
have
f o u n d , a l s o , t h a t s u b s t i t u t i o n o f e v e n a
minor
p r o p o r
t i o n
o f t h e s p e c i ? e d n i t r o c e l l u l o s e b y o r d i n a r y l o w - v i s c o s
i t y
n i t r o c e l l u l o s e r e s u l t s i n a s t i c k y
p r o d u c t w i t h
r e d u c e d
s e l f - s u p p o r t i n g p r o p e r t i e s .
For p u r p o s e s o f c a m o u ? a g e , a n
o l i v e - d r a b
c o l o r a t i o n o f
t h e
e x p l o s i v e i s d e s i r a b l e . L e s s t h a n 0.2%
p i g m e n t
i s
i n
s u f f i c i e n t
t o g i v e a s a t i s f a c t o r y c o l o r a t i o n t o t h e
p r o d u c t
where
a c o l o r
o t h e r
t h a n w h i t e i s
d e s i r e d ,
and
more
t h a n
1.0% p i g m e n t i s n o t n e c e s s a r y
f o r
e f f e c t i v e c o l o r i n g . The
p r e f e r r e d
p i g m e n t , w h i c h i m p a r t s a n o l i v e - d r a b c o l o r a
t i o n t o o u r e x p l o s i v e c o m p o s i t i o n , c o m p r i s e s o n e p a r t
l a m p b l a c k a n d 8 p a r t s c h r o m e
y e l l o w ,
medium
( l e a d
c h r o m a t e ) .
A d d i t i o n
o f
0.4%
(5%
b a s e d
on
n i t r o c e l l u l o s e
p r e s e n t )
d i p h e n y l a m i n e ,
r e f e r r e d t o h e r e i n a f t e r a s D‘PA, t o our ex
p l o s i v e c o m p o s i t i o n r e s u l t s i n i m p r o v e m e n t o f
t h e
p r o d u c t
w i t h
r e s p e c t t o t h e r m a l
s t a b i l i t y
t o s u c h
a marked e x t e n t
t h a t when
t
i s
s u b j e c t e d t o
t h e 1 1 0 ° C .
Vacuum
S t a b i l i t y
T e s t f o r 40 h o u r s t h e volume o f g a s e v o l v e d i s o n l y
a b o u t
h a l f t h a t e v o l v e d
when
t h e
c o m p o s i t i o n
w i t h o u t
a d d e d
DPA s
s i m i l a r l y t e s t e d .
Q u a n t i t i e s
o t h e r
t h a n
0 . 4 DPA
l l
r e s u l t e d i n
a r e d u c e d s t a b i l i z i n g
e f f e c t . O t h e r
commonly
u s e d
n i t r o c e l l u l o s e s t a b i l i z e r s were
found
t o b e
l e s s
e f
8/20/2019 US3354010.pdf
http://slidepdf.com/reader/full/us3354010pdf 2/5
3 , 3 5 4 , 0 1 0
3
i ' e c t i v e . The
Va c u um
S t a b i l i t y T e s t i s d e s c r i b e d i n Method
5 0 3 . 1 o f M i l i t a r y S t a n d a r d MlL-STD-650.
Our p r o d u c t employing HMX and/or RDX
a s
t h e
p a r t i c u l a t e h i g h e x p l o s i v e b a s e p r o v i d e s u n e x p e c t e d a n d
u n p r e d i c t a b l e
a d v a n t a g e s o v e r
? e x i b l e e x p l o s i v e s c o n t a i n
i n g p e n t a e r y t h r i t o l t e t r a n i t r a t e , h e r e i n a f t e r r e f e r r e d t o a s
PETN, a s t h e p a r t i c u l a t e h i g h
e x p l o s i v e
b a s e .
C o m p o s i t i o n s
c o n t a i n i n g
HMX n d / o r
RDX b u t
no
DPA showed s u b s t a n t i a l l y g r e a t e r t h e r m a l s t a b i l i t y i n
t h e Va c u um
S t a b i l i t y T e s t t h a n d i d t h o s e c o n t a i n i n g
FETN.
A c c o r d i n g
t o
P i c a t i n n y A r s e n a l
T e c h n i c a l
R e p o r t
N o . 1 7 4 0 ,
R e v i s i o n
1 , A p r i l 1 9 5 8 , vacuum s t a b i l i t y v a l u e s
o f PETN, HMX, and
RDX t 1 0 0 ° C .
a r e
0 . 5 m l . , 0 . 3 7
m l . , a n d 0 . 7 m l . , r e s p e c t i v e l y . I t would b e e x p e c t e d , t h e r e
f o r e , t h a t ? e x i b l e e x p l o s i v e
c o m p o s i t i o n s
d i f f e r i n g o n l y
i n
w h i c h o f t h e s e t h r e e e x p l o s i v e m a t e r i a l s t h e y c o n t a i n
s h o u l d have a l m o s t i d e n t i c a l t h e r m a l s t a b i l i t i e s , b u t t h i s
h a s
not been found t o
be t h e c a s e . A e r i e s
o f
v a c u u m
s t a b i l i t y
r e s u l t s , n o t
i n c l u d e d i n
t h e
e x a m p l e s ,
show
t h a t
i n t h e
4 0 - h o u r
1 0 0 °
C .
Vacuum S t a b i l i t y T e s t , u s i n g 5
gram
s a m p l e s ,
t h e
PETN-based
? e x i b l e
e x p l o s i v e
com
p o s i t i o n y i e l d e d a b o u t 1 . 5 m l . o f
g a s , w h i l e
s i m i l a r
HMX
a n d / o r R D X - b a s e d ? e x i b l e e x p l o s i v e
c o m p o s i t i o n s
y i e l d e d
about
0 . 7 5 m l . o f
g a s . T h e advantage
o f
t h e u s e
o f
HMX
and/or
RDX ecomes
m u c h
more s t r i k i n g i n
t h e 1 1 0 ° C .
V a c u u m
S t a b i l i t y T e s t
i n
which
u n s t a b i l i z e d
HMX~ n d /
o r RDX-based
? e x i b l e e x p l o s i v e
c o m p o s i t i o n s
y i e l d e d
4-5
m l .
o f
g a s i n 4 0
h o u r s ,
and v a r i o u s
b a t c h e s o f
s i m i l a r
P E T N - b a s e d c o m p o s i t i o n s y i e l d e d 11+ m l . ,
u s u a l l y
i n
m u c h
l e s s t h a n 4 0
h o u r s .
The
c a p a c i t y
o f t h e a p p a r a t u s
used
i s
1 1
m l . T h e
improved
v a c u um s t a b i l i t y
found
f o r
t h e HMX- n d /
o r RDX-based
? e x i b l e e x p l o s i v e c o m p o s i
t i o n s , t h e r e f o r e , i s n o t
p r e d i c t a b l e
on
t h e
b a s i s
o f
t h e c i t e d
v a c u um
s t a b i l i t y v a l u e s
f o r PETN, HMX,
n d
RDX. Fur
t h e r i n d i c a t i o n s
o f t h e i m p r o v e d t h e r m a l s t a b i l i t y o b t a i n e d
through
t h e u s e o f HMX
nd/or
RDX
s
found
i n
t h e
s e v e r a l e x a m p l e s w h i c h f o l l o w .
T o f u r t h e r r e v e a l t h e s u p e r i or i t y o f o u r c y c l i c - p o l y
n i t r a m i n e - b a s e d p r o d u c t over a commercial PETN-based
? e x i b l e e x p l o s i v e , samples o f b o t h were
t e s t e d
i n
a c i r c u
l a t i n g - h o t - a i r oven a t 1 6 0 °
: 5 °
F . Some o f t h e s a m p l e s
o f
t h e
PETN-based
e x p l o s i v e
d e v e l o p e d w r i n k l e s
a n d
p u c k e r s i n 2-3 d a y s which grew t o p a t c h e s o f one
i n c h
or
more i n maximum dimension u n t i l t h e 7 t h
or
8 t h day
o f
t h e t e s t
a f t e r which t h e y remained s t a t i c . None o f
t h e
s a m p l e s
o f
o u r
c y c l i c - p o l y n i t r a m i n e - b a s e d c o m p o s i t i o n s
d e v e l o p e d a n y s u c h i m p e r f e c t i o n s d u r i n g t h e t e s t p e r i o d o f
6 w e e k s .
T h i s
f u r t h e r i l l u s t r a t e s a n
u n p r e d i c t a b l e
adv an
t a g e o f o u r c y c l i c - p o l y n i t r a m i n e - b a se d ? e x i b l e e x p l o s i v e .
A g a i n , i n e x u d a t i o n
p r o p e r t i e s ,
o u r
? e x i b l e e x p l o s i v e
w a s
found
t o
be s u p e r i o r
t o
t h e
PET‘d-based
? e x i b l e
e x p l o s i v e . T h e exudation t e s t a t 1 6 0 ° F . , a s
o u t l i n e d
i n
M i l i t a r y S p e c i ? c a t i o n
MIL-E-46776A
(MU), i s c a r r i e d
o u t a s f o l l o w s : A ample o f t h e
? e x i b l e e x p l o s i v e
1 A i - i n c h
t h i c k and 1 1 / 2 i n c h e s s q u a r e
i s
p l a c e d
on 1 5
l a y e r s
o f ? l t e r
paper i n
t h e
form o f
2 - i n c h
diameter d i s c s . A
orous
r e
l e a s e
p a p e r i s p l a c e d b e t w e e n
t h e
s a m p l e
o f
e x p l o s i v e
and
t h e
l a y e r s
o f ? l t e r
p a p e r .
A 2 5 - g r a m b r a s s w e i g h t , 1 1 / 2
i n c h e s s q u a r e ,
i s
p l a c e d on
t o p
o f t h e s a m p l e . T h i s
assem
b l y i s
then placed on a
wire
s c r e e n and s t o r e d i n a
f o r c e d
d r a f t oven f o r
24 hours
a t
160°
F .
Before assembly,
t h e
b r a s s w e i g h t i s w e i g h e d b y i t s e l f a n d t h e n r e w e i g h e d
w i t h
t h e
s a m p l e . A f t e r h o t s t o r a g e ,
t h e
s a m p l e
and b r a s s
w e i g h t
a r e
removed
from t h e ? l t e r
paper w h i l e
s t i l l
warm, no
a t t e m p t
b e i n g made t o
s e p a r a t e t h e b r a s s
w e i g h t
from t h e
s a m p l e ,
a n d
a l l o w e d
t o
c o o l
w i t h
t h e
s a m p l e u p p e r m o s t .
Whe n c o o l , t h e
s a m p l e
and b r a s s w e i g h t a r e
w e i g h e d
t o
g e t h e r .
T h e
t e s t
i s
r u n i n t r i p l i c a t e and
t h e
a v e r a g e
o f
t h r e e
r e s u l t s i s
r e p o r t e d
t o
d e t e r m i n e
c o m p l i a n c e
w i t h
t h e r e q u i r e m e n t .
Our c y c l i c - p o l y n i t r a m i n e - b a s e d m a t e ri a l r e a d i l y m e t t h e
0.10% maximum w e i g h t
l o s s
r e q u i r e m e n t o f
t h e
s p e c i ? c a
t i o n i n t h e a b o v e e x u d a t i o n t e s t
by
y i e l d i n g v a l u e s r a n g i n g
b e t w e e n 0.090%
and
0.094%; w h e r e a s t h e PETN-based
10
~ 1 1 )
50
55
60
7 0
75
d
? e x i b l e e x p l o s i v e f a i l e d b y y i e l d i n g
r e s u l t s r a n g i n g
1 o e
twecn
0 . 1 1 %
and
0.20%.
I n
cap
s e n s i t i v i t y t e s t s i t was found t h a t t h e commercial
P E T N - c o n t a i n i n g ? e x i b l e e x p l o s i v e s showed w i d e v a r i a
t i o n s i n
s e n s i t i v i t y t o i n i t i a t i o n ,
no
o n l y from l o t t o l o t ,
b u t a l s o w i t h i n
a
g i v e n
l o t .
T h i s
i s
exempli?ed by
two
extremes o f
one
l o t which both accepted and
f a i l e d
t o
a c c e p t
i n i t i a t i o n f r o m s t a n d a r d
3 ,
4 , 5 , a n d #6
c a p s a n d a c c e p t e d
i n i t i a t i o n c o n s i s t e n t l y
from s t a n d a r d
#8 c a p s , and
a n o t h e r
l o t which b o t h a c c e p t e d and f a i l e d
t o a c c e p t i n i t i a t i o n from s t a n d a r d
#1
c a p s
and
a c c e p t e d
i n i t i a t i o n
c o n s i s t e n t l y from s t a n d a r d 2
a p s .
Our HMX
b a s e d
m a t e r i a l , on t h e
o t h e r h a n d , a c c e p t e d i n i t i a t i o n
from
c a p s
c o n t a i n i n g 1 3 . 5 g r a i n s o f RDX s t h e
b a s e
c h a r g e ( M 6 c a p s ) . b u t f a i l e d t o
do
s o
from
s t a n d a r d 8
c a p s ,
which
have 8 . 5
g r a i n s o f
PETN
s t h e
b a s e c h a r g e .
Our RDX-based
m a t e r i a l
a c c e p t e d i n i t i a t i o n from s t a n d
a r d
8 a p s
b u t f a i l e d t o do s o from
s t a n d a r d
6 a p s .
The e r r a t i c
b e h a v i o r
o f t h e PETN-containing m a t e r i a l
w i t h
r e s p e c t t o
c a p s e n s i t i v i t y
c o n s t i t u t e s
a n u n e x p e c t e d
s a f e t y
f e a t u r e i n h e r e n t
i n
our
HMX-
and/or
RDX
c o n t a i n i n g
? e x i b l e
e x p l o s i v e s .
I n c a p s , a s
i s
w e l l known
i n t h e a r t , t h e
s m a l l e r
t h e
number o f
t h e c a p ,
t h e
s m a l l e r
t h e e x p l o s i v e c h a r g e c o n t a i ne d t h e r e i n .
T h e cap s e n s i t v i t y t e s t was
conducted a s
f o l l o w s :
s t r i p s
o f e x p l o s i v e m a t e r i a l
1 / 4
i n c h
t h i c k b y l
i n c h
w i d e
b y
1 2
i n c h e s l o n g
were
i n d e n t e d a t one end by b u t t i n g a notch
1 4 i n c h w i d e
and 3 . 4
i n c h d e e p
and
i n d e n t e d a t t h e
o t h e r end w i t h a s i m i l a r n o t c h 1 % ;
i n c h d e e p .
T h e
i n i t i a t i n g
c a p was
i n s e r t e d
i n t o
t h e
3 . 4 i n c h — d e e p n o t c h and t a p e d
i n
p l a c e . One end
o f a
3 - f o o t - l o n g p i e c e
o f S O - g r a i n
Primacord was i n s e r t e d
i n t o
t h e 1 . 4 i n c h
deep
n o t c h and
t a p e d i n p l a c e . T h e a s s e m b l y was
p l a c e d on a
smooth
c l e a n s t e e l
p l a t e and
t h e c a p ? r e d . Caps
which
i n i t i a t e d
t h e s t r i p o f e x p l o s i v e c a u s e d t h e
P r i m a c o r d
t o
? r e a n d
ma k e
a
r e a d i l y
d e t e c t a b l e
mark
on
t h e
p l a t e .
I n c a s e s
where t h e c a p f a i l e d t o
i n i t i a t e
t h e
s t r i p o f
e x p l o s i v e ,
t h e
undetonated
Primacord and a l a r g e p o r t i o n o f
t h e
t e s t
s t r i p were a l w a y s
p r e s e n t
a f t e r t h e t e s t .
We
have a l s o
d e v i s e d a method f o r
p r e p a r i n g
our i n
v e n t i v e c o m p o s i t i o n s which
o f f e r s
d i s t i n c t a d v a n t a g e s o v e r
c o n v e n t i o n a l
m e t h o d s . An
o u t s t a n d i n g
a d v a n t a g e
t o
b e
d e r i v e d from o u r method i s t h e g r a n u l a r form o f
t h e
p r o d
u c t which
r e n d e r s i t
p a r t i c u l a r l y w e l l s u i t e d
f o r
e x t r u s i o n
a n d
c o m p r e s s i o n - m o l d i n g p u r p o s e s .
I n a c c o r d a n c e w i t h t h i s m e t h o d , n i t r o c e l l u l o s e o f
t h e
h i g h v i s c o s i t y t y p e
a f o r e m e n t i o n e d
c o n t a i n i n g
a b o u t 1 2 . 1
t o 12.5% n i t r o g e n i s d i s s o l v e d
i n
a b o u t 30-70 p a r t s ( p r e f
e r a b l y
48-50
t i m e s i t s w e i g h t ) o f
a
s o l v e n t s u c h a s b u t y l
( p r e f e r r e d ) , p r o p y l ,
o r
e t h y l a c e t a t e
w i t h m e c h a n i c a l
a g i t a t i o n . Whe n s o l u t i o n o f t h e n i t r o c e l l u l o s e i s c o m p l e t e ,
t h e
s t a b i l i z e r i s
added
and
d i s s o l v e d
and
t h e
p l a s t i c i z e r , i n
t h e
amounts
a f o r e m e n t i o n e d ,
i s t h e n s t i r r e d i n t o t h e s o l u
t i o n .
T h e s t a b i l i z e r
p r e f e r a b l y
w i l l
b e 0 . 4%
DPA, a s
a f o r e m e n t i o n e d .
The HMX
n d / o r RDX n d
t h e
p i g m e n t
a r e s e p a r a t e l y s u s p e n d e d i n
a b o u t
2 0 - 8 0 ( p r e f e r a b l y
5 8
6 0 ) t i m e s t h e i r w e i g h t
o f
w a t e r h e l d a t 8 0 °
C .
i n an open
v e s s e l . T h e HMX r RDX a y b e s u s p e n d e d w i t h o u t t h e
presence
of
t h e
other or a mixture of t h e
two
i n any pro
p o r t i o n s
would a l s o
b e
s a t i s f a c t o r y . The
n i t r o c e l l u l o s e
s o l u t i o n
i s added
s l o w l y i n
a ?ne s t r e a m t o t h e v i g o r
o u s l y
a g i t a t e d HMX
and/or RDX
s u s p e n s i o n
s o
t h a t
i t i s w e l l d i s p e r s e d t h e r e i n . Whe n a l l t h e n i t r o c e l l u l o s e
s o l u t i o n h a s b e e n a d d e d , t h e t e m p e r a t u r e o f
t h e
c o n s t a n t l y
s t i r r e d
m i x t u r e
i s r a i s e d
t o
95-98°
C .
t o d i s t i l l o f f t h e s o l
v e n t , w h i c h ,
p r e f e r a b l y ,
i s c o l l e c t e d f o r r e u s e . The
mix
t u r e i s t h e n c o o l e d t o 40° C . a s r a p i d l y a s p o s s i b l e and
? l t e r e d , a f t e r which t h e
p r o d u c t i n
t h e form
o f
s m a l l
somewhat
i r r e g u l a r p e l l e t s i s a i r - d r i e d u n t i l a l l a p p a r e n t
m o i s t u r e
h a s
e v a p o r a t e d . I t
i s
t h e n o v e n - d r i e d
t o
c o n s t a n t
w e i g h t
a t
6 0 ° C .
The g r a n u l a r
p r o d u c t
t h u s o b t a i n e d
i s
r e l a t i v e l y f r e e - ? o w i n g when ? r s t
p r e p a r e d .
Upon
s t a n d
i n g , t h e
g r a n u l e s
t e n d t o a d h e r e l i g h t l y t o o n e a n o t h e r ,
b u t
t h e a g g r e g a t e
may b e b r o k e n
up
r e a d i l y , i f d e s i r e d .
I t
may
8/20/2019 US3354010.pdf
http://slidepdf.com/reader/full/us3354010pdf 3/5
3 , 3 5 4 , 0 1 0 v
b e
p r o c e s s e d i n
a n y d e s i r e d
manner
a s by e x t r u s i o n , r o l l
i n g ,
m o l d i n g ,
e t c .
The
p r o d u c t s
and p r o c e s s o f o u r i n v e n t i o n a r e f u r t h e r
d e s c r i b e d a n d
i l l u s t r a t e d
b y t h e e x a m p l e s
p r e s e n t e d h e r e
i n u n d e r . A l l
p r o p o r t i o n s
e x p r e s s e d
i n p a r t s b y w e i g h t
u n
l e s s
s t a t e d
o t h e r w i s e .
E x a m p l e
I
The ? e x i b l e e x p l o s i v e o f t h i s ? r s t e x a m p l e o f
o u r
i n v e n ~
t i o n
h a d t h e f o l l o w i n g
c o m p o s i t i o n :
Grams
HMX Grade I I , Class B)1
___________________
__ 315
Tributyl
acetylcitrate
________________________
_
1 4 1
N i t r o c e l l u l o s e , alcohol-wet
(dry
b a s i s )
_________ __
4 0
P i g m e n t
( 8 p a r t s c h r o m e
y e l l o w ,
medium/
p a r t
lampblack) ______________________________ _ 4
1
S p e c i ? c a t i o n
M I L - H - 4 5 4 4 4 A
(0rd) w/Arnendment
3
dated July 3 1 , 1 9 6 2 . T h e HMX sed
i n
t h i s
‘ a n d
subsequent
examples
c o n t a i n e d 1.55% RDX n l e s s o t h e r w i s e n o t e d .
The
HMX and t r i b u t y l a c e t y l c i t r a t e were
mixed f o r
t h r e e
m i n u t e s i n
a n
open
sigma
b l a d e mixer h e l d
a t 1 3 5 °
:5“
F .
The
h i g h
v i s c o s i t y n i t r o c e l l u l o s e
c o n t a i n i n g a b o u t
1 2 .
l - l 2 . 5 %
i t r o g e n
a n d t h e p i g m e n t w e r e t h e n a d d e d a n d
m i x e d i n a n d a b o u t
‘ 6 0
m l . o f e t h y l
a l c o h o l
a d d e d t o
l i g h t e n
t h e c o n s i s t e n c y o f t h e mix t o t h a t o f a
s t i f f d o u g h .
The
dough was mixed
a b o u t 1 5 m i n u t e s a t
135°i5° F .
i n t h e
open mixer and t h e n formed i n t o s h e e t s
on
a r o l l m i l l , a l s o
held
a t
135 °i5 F . T h e mix w a s ? r s t r o l l e d
a t
a r o l l
g a p s e t t i n g o f 0 . 0 1 0 i n c h
u n t i l
t h e a l c o h o l was d r i v e n o f f .
T h e
r o l l gap was
t h e n i n c r e a s e d
t o
0 . 2 1 0 i n c h
and t h e t h i n
s h e e t s c o n s o l i d a t e d b y
r e r o l l i n g
i n t o a smooth u n i f o r m
s h e e t a b o u t o n e - q u a r t e r i n c h
i n
t h i c k n e s s .
T h i s m a t e r i a l i s
p a r t i a l l y c h a r a c t e r i z e d b y t h e f o l l o w i n g t e s t r e s u l t s :
Vacuum
s t a b i l i t y t e s t
( 5 g .
f o r
4 0
h o u r s )
a t
1 1 0 °
C. ______________________
_
4 . 58 ml.
g a s .
Cap
e n s i t i v i t y t e s t
__________________
__
M6
a p . 1
1 In accordance with Speci?cation
MIL—C—45468A(MU)
w/Amendment 5 d a t e d M a y 1 5 , 1 9 6 4 .
E x a m p l e I I
The c o m p o s i t i o n
o f
t h e e x p l o s i v e o f
t h i s
e x a m p l e was
i d e n t i c a l w i t h t h a t o f Example I
w i t h
t h e e x c e p t i o n t h a t
t h e c y c l i c p o l y n i t r a m i n e u s e d
was
Type
B , C l a s s
E DX.1
T h i s m a t e r i a l
formed a . smooth
u n i f o r m s h e e t . I t i s
p a r
t i a l l y
c h a r a c t e r i z e d b y t h e
f o l l o w i n g
t e s t
r e s u l t s :
Vacuum s t a b i l i t y t e s t ( 5 g . f o r 40
h o u r s )
at 1 1 0 ° C. ______________________ _ 4. 94 ml. gas.
Cap
e n s i t i v i t y
t e s t _________________
__
8 a p .
A i m i l a r ? e x i b l e
m a t e r i a l
b a s e d on PETN and p r e
p a r e d b y t h e
Du
P o n t Company g a v e a vacuum
s t a b i l i t y
t e s t
v a l u e
o f 1 1 + m l . o f g a s
when
s i m i l a r l y t e s t e d . The
s u p e r i o r
t h e r m a l s t a b i l i t y o f o u r m a t e r i a l
i s
t h u s i l l u s
t r a t e d .
E x a m p l e
I I I
The c o m p o s i t i o n
o f
t h e ? e x i b l e
e x p l o s i v e
o f
t h i s exam—
p l e
was
i d e n t i c a l i n f o r m u l a t i o n w i t h t h a t o f
Example
I I
e x c e p t t h a t RDX o n t a i n i n g a b o u t
2.5% HMX
a s u s e d .
The c h a r a c t e r i s t i c s o f
t h e
r e s u l t a n t p r o d u c t were s u b s t a n
t i a l l y i d e n t i c a l
w i t h t h o s e o f
t h e
p r o d u c t o f
E x a m p l e I I .
E x a m p l e IV
The c o m p o s i t i o n o f t h e ? e x i b l e
e x p l o s i v e
o f t h i s e x
ample was i d e n t i c a l i n f o r m u l a t i o n w i t h
t h a t o f
Example
I
w i t h
t h e
e x c e p t i o n
t h a t
HMX
o n t a i n i n g
a b o u t
1 . 2 %
RDX was u s e d .
A mooth
homogeneous
s h e e t was ob
t a i n e d
h a v i n g c h a r a c t e r i s t i c s and
p h y s i c a l
p r o p e r t i e s s i m i
l a r t o t h o s e o f t h e
p r o d u c t
o f Example I . As i n Example
I , an
M6
ap was
r e q u i r e d
f o r i n i t i a t i o n
i n
t h e c a p s e n s i
t i v i t y
t e s t .
1 S p e c i ? c a t i o n MIL-R-3 9 8C d a t e d
Aug.
2 2 , ‘ 1 9 6 2 . T h e RDX
used i n t h i s
and
subsequent examples contained 7 . 3% HMX
u n l e s s
otherwise n o t e d .
1 0
1 5
20
2 5
3 5
40
4 5
50
55
60
6 5
7 5
6
‘
Example
V
The c o m p o s i t i o n o f t h e ? e x i b l e e x p l o s i v e o f
t h i s
e x
a m p l e
was i d e n t i c a l
w i t h
t h a t o f Example
I I e x c e p t t h a t i t
c o n t a i n e d
0 . 4
added p a r t o f DPA
b a s e d on
1 0 0 ‘ p a r t s
o f
? e x i b l e e x p l o s i v e
a s
p r e p a r e d
i n
Example
I I ) ,
w h i c h
was
d i s s o l v e d
i n
t h e a l c o h o l
u s e d t o wet
t h e
n i t r o c e l l u l o s e .
T h e
m i x t u r e g a v e
a
p r o d u c t
v e r y
s i m i l a r t o t h a t
o f Example
I I
e x c e p t t h a t
i t s v a c u um s t a b i l i t y v a l u e a t
1 1 0 °
C .
was
2 . 8 5
m l . o f
g a s
e v o l v e d , a
c o n s i d e r a b l e
improvement
o v e r t h e
v a l u e
f o u n d
f o r t h e u n s t a b i l i z e d m a t e r i a l .
E x a m p l e V I
The
c o m p o s i t i o n o f t h e e x p l o s i v e o f t h i s e x a m p l e
w a s ‘
i d e n t i c a l
w i t h
t h a t o f Example I w i t h t h e e x c e p t i o n t h a t
0 . 4 p a r t b y w e i g h t o f t h e s t a b i l i z e r DPA a s
a d d e d .
The
DPA
as
d i s s o l v e d i n t h e
a l c o h o l
w i t h which t h e n i t r o
c e l l u l o s e
was wet and
t h e
n i t r o c e l l u l o s e - a l c o h o l - D P A
mixture
was allowed
t o
age a t
l e a s t one
day
b e f o r e u s e .
The
c o m p o s i t i o n o f t h e m a t e r i a l o f t h i s
example
w a s :
P a r t s
HMX __________________________________ _ 63.0
H i g h v i s c o s i t y
n i t r o c e l l u l o s e
________________ __ 8 . 0
Tributyl a c e t y l c i t r a t e _______________________
_ 28.2
Pigment ( o f Example I ) ____________________ . . 0 . 8
DP ___________________________________
_ 0 4
The v o l u m e o f a l c o h o l u s e d
i n
t h i s
e x a m p l e
amounted
t o 1 . 7 5 m l . / . o f n i t r o c e l l u l o s e ,
0 . 5
m l .
t h e r e o f
b e i n g u s e d
t o d i s s o l v e t h e DPA
and
p r o v i d e
t h e
s o l u t i o n
u s e d
t o
m o i s t e n t h e n i t r o c e l l u l o s e a n d i n c o r p o r a t e t h e r e w i t h t h e
DPA,
t h e
r e s t b e i n g
worked
i n t o
t h e
m i x t u r e
t o a s s u r e
a
h e a v y d o u g h l i k e
c o n s i s t e n c y . T h i s m a t e r i a l w a s r o l l e d
intoa
‘ A
i n c h
t h i c k s h e e t which was
smooth
and
u n i f o r m .
I t
i s p a r t i a l l y c h a r a c t e r i z e d b y
t h e
f o l l o w i n g t e s t r e s u l t s :
d 42° 1 ____ _ 1 . 5 1 5 .
Vacuum s t a b i l i t y t e s t ( 5 g . f o r
4 0
h o u r s )
at
1 1 0° C.
____________________
. 2.78 ml.
g a s .
P i c a t i n n y A r s e n a l
i m p a c t
s e n s i t i v i t y
test
2 _________________________
_ 15 i n c h e s .
P i c a t i n n y
A r s e n a l
e x p l o s i o n
temperature t e s t
3 _______________
.
2 7 0 °
C.
s m o k e .
Cap s e n s i t i v i t y
t e s t
_______________
. M6
a p .
1
T h e
symbol ( 1 4 2 ° i n d i c a t e s
the r a t i o o f the density o f
the
e x p l o s i v e s h e e t a t 20° C .
t o
t h e d e n s i t y
o f
water a t 4 ° ‘ C .
2 T h e Picatinny Arsenal impact
s e n s i t i v i t y
t e s t i s d e s c r i b e d v
i n
“Standard
Laboratory
P r o c e d u r e s
f o r
S e n s i t i v i t y , B r i s a n c e
and S t a b i l i t y o f E x p l o s i v e s , ” PATR N o . 1 4 0 1 , M a r . 1 8 , 1 9 4 4 ,
r e v i s e d F e b .
2 8 ,
1 9 5 0 , W.
H.
Rlnkenbach and A .
J .
C l e a r .
3 _ T h e P i c a t i n n y A r s e n a l e x p l o s i o n t e m p e r a t u r e t e s t i s
d e
s c r i b e d
i n “ S t a n d a r d L a b o r a t o r y
P r o c e d u r e s f o r
S e n s i t i v i t y ,
Brisance
and
S t a b i l i t y
o f
E x p l o s i v e s . ”
PATR
No.
‘ 1 4 0 1 ,
Mar.
1 3 % , 1 9 4 4 , r e v i s e d - F e b .
‘ 2 8 , 1 9 5 0 , W. H .
R i n k e n b a e h a n d A ; J ’ .
ear
' > -
C o m p a r i s o n o f
t h e r e s u l t
o b t a i n e d
i n t h e v a c u u m ‘
s t a
b i l i t y t e s t o f t h i s e x a m p l e
w i t h
t h e
c o r r e s p o n d i n g
t e s t . r e '
s u l t
s h o w n
u n d e r Example
I c l e a r l y
s h o w s
t h e v a l u e o f
DPA o r s t a b i l i z a t i o n o f t h e m i x t u r e .
I Example VII
The
‘ c o m p o s i t i o n
a n d p r o c e d u r e o f t h i s e x a m p l e w e r e
i d e n t i c a l
w i t h t h o s e o f Example V n d Example
- V I
e x ~
c e p t t h a t t h e
c y c l i c
p o l y n i t r a m i n e u s e d c o n s i s t e d
o f a
m i x t u r e
c o n t a i n i n g e q u a l
a m o u n t s o f
HMX
n d R D X . ’
T h i s m i x t u r e
w a s
p r e p a r e d b y m i x i n g
4 7
p a r t s b y w e i g h t
o f t h e HIMX'of E x a m p l e I w i t h 5 3 p a r t s b y w e i g h t o f t h e
RDX
f
Example
I I . T h e
c o m p o s i t i o n o f
t h e
? e x i b l e
e x
p l o s i v e
p r e p a r e d
i n
t h i s e x a m p l e w a s
t h u s :
P a r t s
HMX __ _ _
31.5
RDX_____
__ __ 31.5
H i g h v i s c o s i t y
n i t r o c e l l u l o s e
_________________
__
8 . 0
Tributyl a c e t y l c i t r a t e _______________________ __ 28.2
Pigment (of
Example
) ____________ _ _ . ______ _
0 . 8
DPA
_ 0 . 4
8/20/2019 US3354010.pdf
http://slidepdf.com/reader/full/us3354010pdf 4/5
3 , 3 5 4 , 0 1 0
T e s t
r e s u l t s o b t a i n e d w i t h t h i s m a t e r i a l a r e :
( 1 4 2 ° ____________________________ _ 1.057.
V a c u u m s t a b i l i t y t e s t ( 5
g .
f o r 4 0 ‘
h o u r s )
at 1 1 0 ° C . ____________________ _ 2.79 ml . gas.
P i c a t i n n y A r s e n a l
i m p a c t
s e n s i t i v i t y
test
__________________________
_ 1 7
inches.
P i c a t i n n y A r e n s a l e x p l o s i o n
t e m p e r a t u r e
t e s t
__________________________
_
246° C. smoke.
De to n a t i o n velocity
______________
_
7008
m./se c .
Cap
s e n s i t i v i t y t e s t ______________ _ M6 cap .
I n t h e f o l l o w i n g
t h r e e
e x a m p l e s ( E x a m p l e s V I I I , I X ,
and X)
t h e
c y c l i c
p o l y n i t r a m i n e
u s e d
was w e t w i t h 25—
35% w a t e r . T h e w a t e r - w e t p o l y n i t r a m i n e was machine
m i x e d
w i t h t h e p l a s t i c i z e r t r i b u t y l a c e t y l c i t r a t e b e f o r e t h e
o t h e r i n g r e d i e n t s
were a d d e d . Mixing was t h e n s t o p p e d
a n d t h e
mixture
w a s
allowed
t o s t a n d f o r a few minutes
t o a l l o w t h e d i s p l a c e d water
t o
r i s e t o t h e t o p
and
be
r e
moved b y d e c a n t a t i o n .
Then
a d d i t i o n o f i n g r e d i e n t s a n d
machine-mixing
were
c o n t i n u e d .
Example V I I I
L b s .
RDX
a s
u s e d
i n Example I I b u t c o n t a i n i n g 3 0 %
w a t e r
(dry
basis) ______________________ _ 12. 6 0
Trib utyl acetylcitrate _____________________ _ 5.64
H i g h v i s c o s i t y n i t r o c e l l u l o s e , a l c o h o l - w e t
(dry
basis)
_______ 1___________________ _ 1.60
Pigment ( o f E x a m p l e I ) ___________________
__ 0.16
The
RDX
and p l a s t i c i z e r
were mixed 3
m i n u t e s
a t
1 3 0 ° F . T h e
mixer
was t h e n s t o p p e d and t i l t e d
t o
d e c a n t
t h e
w a t e r . The a l c o h o l - w e t
n i t r o c e l l u l o s e
a n d t h e p i g m e n t
were t h e n
added
and
t h e
whole
mixed
3 0 m i n u t e s w i t h
t h e
mixer h e l d a t 1 3 0 ° F . and
t h e
t o p o p e n . T h e mix was
t h e n
r o l l e d a s
d e s c r i b e d i n Example I
t o g i v e
u n i f o r m
homogeneous
s h e e t s
h a v i n g
a
v a c u um
s t a b i l i t y v a l u e o f
5 . 0 4 m l . g a s a t 1 1 0 ° C . Two
PETN-containing
a n a l o g s
o f
t h i s
m a t e r i a l ( o t h e r t h a n
t h a t
n o t e d
f o r
c o m p a r a t i v e
p u r p o s e s i n Example 1 1 ) showed v a c u um s t a b i l i t y v a l u e s
o f 1 1 + m l . wh e n
t e s t e d
a t 1 1 0 ° C . , d e m o n s t r a t i n g a s u b
s t a n t i a l l y l o w e r d e g r e e
o f
s t a b i l i t y .
Other t e s t v a l u e s :
d4“ _________________________ . _ 1 . 4 9 0 .
De to n a t i o n
velocity ____________ . 7044 m./se c .
Cap
e n s i t i v i t y
t e s t
____________ . 8 cap.
No r a c k l e s , ? a m e ,
o r
e x p l o s i o n .
F r i c t i o n
p e n d u l u m
t e s t
( s t e e l s h o e ) 1
B a l l i s t i c mortar
t e s t
v a l u e (TNT
value=1.0)
2
________________
.
1.0.
P i c a t i n n y
A r s e n a l
i m p a c t
s e n s i t i v i t y
test _______________________
_ 14 in c h e s .
1 T h e
f r i c t i o n p e n d u l u m
t e s t i s described
i n
“Picatinny Ar
s e n a l
Testing Manual,”
May
,
1 9 5 0 ,
. I . H. McIvor,
M a n u a l
7 - 1 .
2The b a l l i s t i c mortar t e s t i s described
i n
“Picatinny Ar
s e n a l
Testing Manual, May ,
1 9 5 0 ,
J .
H.
McIvor, M a n u a l
7-2.
R i ? e
bullet imp a c t
t e s t
1 _______ __ N0 re
or
explosion.
Bar drop i m p a c t t e s t
1
_________ . Do.
E l e v a t e d t em p er a t ur e t e s t 1 ____ _ No h a n g e .
Hot water
immersion
test 1 _____ _ Do.
Exudation est _______________ _ 0.09%
oss.
P i c a t i n n y
A r s e n a l
e x p l o s i o n
t e m p e r
ature
t e s t _________________ _ 2 0 8 ° C. ( d e c o m p n . ) .
1 T h e r i ? e b u l l e t impact t e s t , elevated temperature t e s t , bar
drop im p a c t t e s t , a n d hot
w ater
immersion t e s t are described
i n
M i l i t a r y S p e c i ? c a t i o n
M I L —E - 4 6 6 7 6 A ( M U )
d a t e d A p r .
1 7 ,
1 9 6 4 ,
i n paragraphs 4 . 3 . 7 , 4 . 3 . 9 , 4 . 3 . 1 1 , a n d 4 . 3 . 1 5 , r e s p e c
t i v e l y . In the elevated temperature t e s t our samples were
sub—
jected
t o s i x
weeks
at
1 6 0° F . i n l i e u o f the s ev en days
s p e c i
t i e d i n
the
ahovenoted s p e c i ? c a t i o n .
Example
IX
S e v e r a l S O - p o u n d b a t c h e s o f
? e x i b l e
e x p l o s i v e c o m p o s i
t i o n c o n t a i n i n g t h e DPA t a b i l i z e r ( s e e Example V)
w e r e
p r e p a r e d
b y t h e m i x i n g
t e c h n i q u e d e s c r i b e d i n E x a m p l e
V I I . A o r t i o n
o f t h e s e
m i x t u r e s w a s p r o c e s s e d
b y
r o l l
- 1 0
60
65
70
7 5
8
i n g
a s
d e s c r i b e d i n
t h e
a b o v e e x a m p l e s and
t h e
r e m a i n d e r
b y e x t r u s i o n . T h e
m a t e r i a l s
u s e d i n e a c h b a t c h w e r e :
L b s .
RDX
a s
u s e d i n
Example I I
b u t w a t e r - w e t
( d r y
b a s i s ) _________________________________
_
50.40
Trib utyl
acetylcitrate
______________________ _ 22. 5 6
H i g h v i s c o s i t y
n i t r o c e l l u l o s e ,
a l c o h o l
w e t
( d r y
b a s i s ) _________________________________ _
6.40
Pi gm e n t
of
Example
_____________________
__ 0.64
DPA d i s s o l v e d i n t h e a l c o h o l w e t t i n g
t h e
n i t r o
c e l l u l o s e )
______________________________
_ 0.32
T y p i c a l
t e s t
v a l u e s o b t a i n e d w i t h
t h i s
m a t e r i a l
a r e :
( 1 4 2 °
o f
r o l l e d
o n e - q u a r t e r - i n c h t h i c k
sheet __________________________ _ 1.466.
£ 1 4 2
o f extruded
Z - i n c h x 4 - i n c h
x 1 2 - i n c h
blocks _________________________ _ 1.485.
V a c u u m s t a b i l i t y t e s t
( 5
g . f o r 40
h o u r s
a t
1 1 0 °
C. _______________________
_
2.85 ml. gas.
P i c a t i n n y a r s e n a l i m p a c t s e n s i t i v i t y
test ___________________________
_ 16
i n c h e s .
P i c a t i n n y a r s e n a l e x p l o s i o n
t e m p e r a t u r e
t e s t ___________________________
_
250°
C.
smoke.
Detonation v e l o c i t y ( ( 1 4 2 0 1 . 4 6 6 ) _ _ 7011 m . / s e c .
Cap s e n s i t i v i t y t e s t ___________ _ 8 ap.
B a l l i s t i c
b o r t a r t e s t v a l u e
( T N T
value=l.0 _________________
_
1 . 0 .
Ri ? e bullet i m p a c t t e s t
_________ _ No re or explosion.
E l e v a t e d
t em p er a t ur e t e s t ______ _ No h a n g e .
Hot
water immersion test
______
_
Do.
Bar drop impact t e s t __________ __ No re or explosion.
Flame sensitivty t e s t 1 _________ _
No xplosion.
1 T h e
? a m e
s e n s i t i v i t y
t e s t
i s
d e s c r i b e d i n Speci?cation
. \ - I I I ; — E — 4 6 6 7 6 A ( M U ) , A p r . 1 7 , 1 9 6 4 ,
i n paragraph
4 . 3 . 8 .
E x t r u d e d
b l o c k s
o f t h e
? e x i b l e
e x p l o s i v e
o f
t h i s
e x
ample w e r e f o u n d
t o
w i t h s t a n d r e l a t i v e l y h i g h - v e l o c i t y im
p a c t
w i t h o u t
b r e a k a g e ,
undue d i s t o r t i o n ,
o r e x c e s s i v e
b o u n c e .
I n a d d i t i o n t o b l o c k s , 1 A - i n c h t h i c k
s h e e t s and
? l a m e n t s o n l y 1 / a i n c h i n
d i a m e t e r w e r e
p r e p a r e d r e a d i l y
b y e x t r u s i o n . B l o c k s o f
t h e
? e x i b l e e x p l o s i v e o f
t h i s i n
v e n t i o n ,
s i m i l a r t o t h o s e p r o d u c e d by
e x t r u s i o n ,
h a v e b e e n
p r o d u c e d
b y c o m p r e s s i o n
m o l d i n g .
Example X
U s i n g
t h e same
t e c h n i q u e ( o f Example V I I I ) , a
5 0 0 ‘
gram b a t c h
h a v i n g
t h e
c o m p o s i t i o n
o f
t h e
e x p l o s i v e o f
Ex
ample
VI
Was
p r e p a r e d i n
a s m a l l
sigma
b l a d e
mixer
and
r o l l e d
i n t o
a smooth
homogeneous
s h e e t .
As e x p e c t e d , t h i s
m a t e r i a l Was s u b s t a n t i a l l y i d e n t i c a l w i t h t h e m a t e r i a l o f
E x a m p l e
V I .
E x a m p l e
XI
The
c o m p o s i t i o n
o f t h e ? e x i b l e e x p l o s i v e
p r e p a r e d a c
c o r d i n g t o
t h i s example was i d e n t i c a l w i t h
t h a t o f
Ex
a m p l e
V ,
a new p r e c i p i t a t i o n
method
b e i n g e m p l o y e d
i n i t s p r e p a r a t i o n . I n a c c o r d a n c e w i t h t h i s
m e t h o d , 2 4
grams o f h i g h
v i s c o s i t y
n i t r o c e l l u l o s e was
d i s s o l v e d
i n
1 1 7 6
grams b u t y l a c e t a t e
w i t h m e c h a n i c a l
a g i t a t i o n , 1 . 2
g r a m s DPA d d e d ,
and 8 4 . 6 grams
o f t r i b u t y l
a c e t y l
c i t r a t e
t h e n s t i r r e d i n . T h i s s o l u t i o n was t h e n
added
slow
l y i n a ?ne s t r e a m t o a v i g o r o u s l y a g i t a t e d
s u s p e n s i o n
o f
1 8 9
grams
o f
t h e RDX
f
Example I I and 2 . 4
grams
o f
t h e l a m p b l a c k - c h r o m e y e l l o w , medium p i g m e n t i n
3 , 7 8 0
m l . o f d i s t i l l e d w a t e r h e l d a t 80° C . When l l t h e
n i t r o
c e l l u l o s e s o l u t i o n had b e e n
a d d e d ,
t h e
t e m p e r a t u r e
o f t h e
v i g o r o u s l y
a g i t a t e d
m i x t u r e
was
r a i s e d
g r a d u a l l y
t o
9 8 °
C .
t o
d r i v e
o f f t h e s o l v e n t . The
s u s p e n s i o n was t h e n
c o o l e d
q u i c k l y
t o
4 0 °
C .
b y p a s s i n g w a t e r a t a b o u t 1 6 °
C .
t h r o u g h t h e j a c k e t
o f
t h e v e s s e l u s e d , a n d t h e w h o l e
v a c u u m - ? l t e r e d . The g r a n u l a r p r o d u c t ,
c o n s i s t i n g
o f some
what
rounded p a r t i c l e s h a v i n g
a m a x im um
d i m e n s i o n
r a n g e
o f
a b o u t 1 , 4 , 4 i n c h t o 3 / 1 6 i n c h , was
p l a c e d
i n s h a l l o w
t r a y s
and
a i r - d r i e d
o v e r n i g h t .
I t was
t h e n o v e n - d r i e d a t
6 0 °
C . t o c o n s t a n t w e i g h t .
8/20/2019 US3354010.pdf
http://slidepdf.com/reader/full/us3354010pdf 5/5
3 , 3 5 4 , 0 1 0
9
The g r a n u l a r p r o d u c t
t h u s
p r e p a r e d
w a s
f u r t h e r p r o c
e s s e d c o n v e n t i o n a l l y b y r o l l i n g
i n t o
s h e e t s a s d e s c r i b e d i n
Example I
e x c e p t
t h a t r o l l i n g
a t
t h e s m a l l e r r o l l - g a p s e t
t i n g was
o n l y o f s u c h d u r a t i o n a s t o
o b t a i n
a p r o d u c t o f
u n i f o r m a p p e a r a n c e , t h e r e b e i n g no s o l v e n t t o e v a p o r a t e .
T h i s
m a t e r i a l
‘ w a s a l s o
formed
i n t o
b i l l e t s
b y c o m p r e s
s i o n - m o l d i n g . T h e p r o c e s s e d ? e x i b l e e x p l o s i v e p r e p a r e d
a c c o r d i n g t o
t h i s e x a m p l e
w a s s u b s t a n t i a l l y i d e n t i c a l
i n
p r o p e r t i e s w i t h t h a t o f E x a m p l e
V
i t h t h e e x c e p t i o n
t h a t
i t s v a c u u m s t a b i l i t y t e s t
v a l u e a t 1 1 0 ° C .
was 2 . 2 4
m l .
g a s .
e v o l v e d .
E x a m p l e
X I I
The c o m p o s i t i o n
o f
t h e
? e x i b l e e x p l o s i v e
p r e p a r e d a c
c o r d i n g
t o t h i s e x a m p l e was i d e n t i c a l w i t h t h a t
o f
Ex
a m p l e V I , t h e m e t h o d o f p r e p a r a t i o n o f E x a m p l e
XI
b e i n g
e m p l o y e d .
I n a c c o r d a n c e w i t h
t h e method o f
t h i s
e x a m p l e 1 2 g r a m s o f
h i g h
v i s c o s i t y n i t r o c e l l u l o s e w a s d i s
s o l v e d
i n 5 8 8
g r a m s o f
b u t y l
a c e t a t e
w i t h m e c h a n i c a l
a g i
t a t i o n ,
0 . 6
gram DPA d d e d ,
a n d
4 2 . 3 g r a m s o f t r i b u t y l
a c e t y l c i t r a t e
t h e n
s t i r r e d
i n .
T h i s
s o l u t i o n
was
t h e n
‘ a d d e d
s l o w l y
i n a ?ne
s t r e a m
t o a
v i g o r o u s l y
a g i t a t e d
s u s p e n
s i o n
o f
9 4 . 5
g r a m s o f
HMX
o f
Example
I ) a n d
1 . 2
g r a m s
o f
p i g m e n t ( a s
u s e d i n Example I ) i n 5 , 5 4 4
m l .
o f
d i s t i l l e d w a t e r
h e l d
a t 8 0 °
C .
W h en
a l l
t h e n i t r o c e l l u l o s e
s o l u t i o n
h a d b e e n a d d e d ,
t h e v i g o r o u s l y
a g i t a t e d m i x t u r e
was
h e a t e d t o 98° C . i n an open
v e s s e l
and h e l d a t t h a t
t e m p e r a t u r e u n t i l
v i r t u a l l y a l l
t h e
b u t y l a c e t a t e h a d b e e n
d r i v e n
o f f . The s u s p e n s i o n
was
t h e n c o o l e d
q u i c k l y t o
4 0 °
C .
b y
p a s s i n g
w a t e r
a t
a b o u t 1 6 °
C .
t h r o u g h t h e
j a c k e t
o f t h e v e s s e l
u s e d , a n d t h e
w h o l e v a c u u m ~ ? l t e r e d .
The g r a n u l a r p r o du c t , c o n s i s t i n g o f s o m e w h a t r o u n d e d
p a r t i c l e s h a v i n g
a m a x im um d i m e n s i o n
r a n g e
o f
a b o u t
4 3 4
i n c h
t o 3 / 1 6 i n c h ,
w a s
p l a c e d i n s h a l l o w t r a y s
a n d a i r
d r i e d
o v e r n i g h t .
I t
was
t h e n
o v e n - d r i e d a t 6 0 ° C . t o con
s t a n t
w e i g h t .
The g r a n u l a r
p r o d u c t
t h u s
p r e p a r e d was
f u r t h e r
p r o c
e s s e d
c o n v e n t i o n a l l y
i n e x a c t l y
t h e same manner a s t h e
g r a n u l a r
p r o d u c t o f
Example XI w a s
p r o c e s s e d . The
p r o c
e s s e d ? e x i b l e e x p l o s i v e
p r e p a r e d
a c c o r d i n g t o t h i s
e x
a m p l e w a s
s u b s t a n t i a l l y
i d e n t i c a l
W i t h
t h a t o f Example
V I . Some t e s t r e s u l t s
o b t a i n e d
w i t h t h i s m a t e r i a l a r e :
d 4?“ ____________________________
_
1 . 5 1 3 .
Vacuum s t a b i l i t y t e s t
( 5 g .
f o r 40 h o u r s )
a t
1 1 0 °
C. _____________________
_ 2. 89
ml. g a s .
P i c a t i n n y A r s e n a l i m p a c t s e n s i t i v i t y
t e s t ___________________________ _ 18inches.
P i c a t i n n y
A r s e n a l
e x p l o s i o n t e m p e r a t u r e
t e s t ___________________________ _ 267° C. smoke.
1 0
1 5
25
3 0
40
45
10
W h i l e t h e
p r e s e n t i n v e n t i o n h a s b e e n d e s c r i b e d
i n
d e
t a i l ,
i t
w i l l b e a p p a r e n t t o t h o s e s k i l l e d i n t h e a r t t h a t
t h e r e
a r e
many v a r i a t i o n s
p o s s i b l e w i t h o u t d e p a r t i n g from
t h e s c o p e o f
t h i s i n v e n t i o n , w h i c h i s l i m i t e d ‘
o n l y
b y
t h e
a p p e n d e d
c l a i m s .
We l a i m :
1 . A ethod f o r t h e p r e p a r a t i o n o f a s e l f - s u p p o r t i n g ,
r e s i l i e n t ,
h i g h - p o w e r e d ,
b r i s a n t , ? e x i b l e s h e e t
e x p l o s i v e
c o m p o s i t i o n
o f
m o d e r a t e c a p
s e n s i t i v i t y ,
l o w i m p a c t s e n s i
t i v i t y , a n d
g o o d t h e r m a l
s t a b i l i t y
a n d w a t e r
r e s i s t a n c e
c o m p r i s i n g
t h e
s t e p s o f
m i x i n g a b o u t 6 3 p a r t s o f a
h i g h
e x p l o s i v e
c o m p r i s i n g
d r y c y c l o t e t r a m e t h y l e n e t e t r a n i t r a m i n e
(HMX) c o n
t a i n i n g a b o u t
1 . 2 - 1 . 5 5 %
d r y c y c l o t r i m e t h y l e n e t r i n i
t r a m i n e
(RDX) a n d
a b o u t 2 8 . 2
p a r t s
t r i b u t y l a c e t y l
c i t r a t e a t a b o u t
1 3 5 °
F . t o form
a p a s t y
m a s s ,
m i x i n g t h e r e i n t o
a b o u t 8
p a r t s o f
h i g h v i s c o s i t y , a l c o
h o l - w e t
n i t r o c e l l u l o s e c o n t a i n i n g
a b o u t
1 2 . 1 t o
1 2 . 5 % n i t r o g e n a n d
0 . 8 p a r t o f a p i g m e n t c o n s i s t i n g
o f
1
p a r t
l a m p b l a c k
a n d
8
p a r t s
chrome
y e l l o w ,
medium, t o form
a
m i x t u r e ,
a d d i n g e t h a n o l t o s a i d m i x t u r e t o
form
a s t i f f d o u g h ,
m i x i n g s a i d d o u g h a t a
t e m p e r a t u r e
i n t h e n e i g h b o r ~
hood
o f
a b o u t
1 3 5 °
F . and
r o l l - m i l l i n g s a i d
mixed
dough a t a b o u t 1 3 5 ° F . t o
form
s a i d ? e x i b l e s h e e t e x p l o s i v e c o m p o s i t i o n .
2 . The
method
a s d e s c r i b e d i n c l a i m 1
w h e r e i n
s a i d
h i g h e x p l o s i v e i s d r y
RDX
o n t a i n i n g
a b o u t
25-7 3%
d r y
H MX.
3 . The method o f c l a i m 1 f u r t h e r c h a r a c t e r i z e d b y add
i n g
0 . 4 p a r t o f
d i p h e n y l a m i n e
s t a b i l i z e r
d i s s o l v e d i n t h e
a l c o h o l w i t h w h i c h t h e n i t r o c e l l u l o s e i s w e t a n d a l l o w i n g
t h e
n i t r o c e l l u l o s e - a l c o h o l - d i p h e n y l a m i n e
m i x t u r e
t o
a g e
a t
l e a s t
one
day b e f o r e u s e .
4 .
The
method
d e s c r i b e d
a s
i n
c l a i m
1
w h e r e i n
t h e
h i g h e x p l o s i v e
u s e d
c o n s i s t s o f e q u a l p a r t s HMX n d
RDX.
5 . The method o f
c l a i m 2
f u r t h e r c h a r a c t e r i z e d
b y
a d d
i n g 0 . 4
p a r t o f
d i p h e n y l a m i n e
s t a b i l i z e r
d i s s o l v e d i n t h e
a l c o h o l w i t h w h i c h
t h e
n i t r o c e l l u l o s e i s
w e t
and a l l o w i n g
t h e
n i t r o c e l l u l o s e - a l c o h o l - d i p h e n y l a m i n e
m i x t u r e t o
a g e
a t l e a s t one day b e f o r e
u s e .
R e f e r e n c e s C i t e d
UNITED STATES PATENTS
6/1 964 Wright ____________
__ 1 4 9 — — 9 2
2/1966
Murphy
___________
_ l49—18
BENJAMIN R .
PADGETT,
P r i m a r y E x a m i n e r .
3 , 1 3 8 , 5 0 1
3 , 2 3 5 , 4 2 0