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March

1 8 , 1952

J .

F .

KENNEY 2,589,703

LEAD STYPHNATE AND PROCESS OF MANUFACTURING SAME

Filed A u g . 17, 1950

lNVENTOR

JOSE/0H5

A f / V / V E Y

a Y g - i m

ATTORNEYS

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P a t e n t e d M a r .

1 8 , 1 9 5 2

2 , 5 8 9 , 7 0 3

UNITED

STATES

PATENT

OFFICE

2 , 5 8 9 , 7 0 3

LEAD

STYPHNATE

AND PROCESS

OF.

MANUFACTURING

SAME

J o s e p h F . K e n n e y , B r i d g e p o r t , C o n n . , a s s i g n o r t o .

Remington

Arms

Company,

I n c . ,

B r i d g e p o r t ,

' C o n n . , a corporation

o f

Delaware

A p p l i c a t i o n August

7 ,

1 9 5 0 , S e r i a l N o . 1 7 9 , 9 3 5

0 1 . 5 2 - 2 )

Claims.

This invention

r e l a t e s t o

normal lead-styph

nate

i n

a novel

c r y s t a l l i n e

form,

t o

the process

of

i t s

manu facture,

and

to

i t s

use as

an

e x

p l o s i v e ,

e i t h e r

by

i t s e l f o r i n admixture with

other substances c om m o n l y used i n

the

prep

a r a t i o n o f ammunition priming and d e t o n a t i n g

compositions.

Normal

e a d

styphnate

and

an e a r l y

p r o c e s s

f o r

i t s manufacture are de scribed in

the

patent t o v o n

H e r z ,

No. 1 , 4 4 3 , 3 2 8 , January

2 3 , 1 9 2 3 . The

com

p o u n d has been

e x t e n s i v e l y used

a s

an

e x p l o s i v e ,

particularly

as

an ingredient o f a m m u n i t i o n

priming

c o m p o s i t i o n s , and t h e p r o c e s s by which

i t

i s

o r d i n a r i l y

made s

d e s c r i b e d

i n

the patent

t o von

H e r z ,

No. 1 , 9 9 9 , 7 2 8 , A p r i l

3 0 ,

1 9 3 5 .

Manu

f a c t u r e has always r e q u i r e d c a r e f u l c o n t r o l ,

t o

a v o i d p r e c i p i t a t i o n o f the

product

i n e l o n g a t e d

n e e d l e - l i k e

c r y s t a l s ,

t h e f r a c t u r e

o f

which

may

cause the detonation of

a l l or a substantial

pro

portion

o f the

batch

i n

p r o c e s s . When d r y , the

s a l t

i s u n d e s i r a b l y s e n s i t i v e

t o

s t a t i c

e l e c t r i c i t y ,

and

appropriate

procedure m us t

be

f o l l o w e d

i n

i t s

h a n d l i n g .

The p r e s e n t i n v e n t i o n c o m p r i s e s t h e d i s c o v e r y

o f a new c r y s t a l l i n e f or m o f normal lead

styph

n a t e , and a

p r o c e s s

f o r

producing

t h e s a l t i n

t h i s

c r y s t a l l i n e

form. The

c r y s t a l s a r e

s t a b l e ,

r e c t a n g u l a r p a r a l l e l o p i p e d s ,

and

a r e o r d i n a r i l y

s o

nearly

c u b i c a l

that

f o r

the purpose

o f d i s t i n c

t i o n from t h e

o r d i n a r y

s a l t t h e y w i l l i n t h i s s p e c i

?cation

be

c a l l e d c u b i c

c r y s t a l s .

While normal

l e a d styphnate i n

t h e

form o f such c u b i c c r y s t a l s

i s l e s s s e n s i t i v e

t o

s t a t i c e l e c t r i c i t y ,

i t 9

i s more

s e n s i t i v e t o

impact

and

more

uniform

i n

i t s

s e n s i

t i v i t y t o i m p a c t .

The s i n g l e

?gure

o f t h e drawing shows

t h e

X-ray d i ? r a c t i o n pattern o f the

n e w normal

l e a d

s t y p h n a t e

i n

c u b i c c r y s t a l s , a n d ,

i n

j u x t a p o s e d

r e l a t i o n

t h e r e t o ,

t h e X-ray d i l f r a c t i o n p a t t e r n

o f

o r d i n a r y

normal l e a d

s t y p h n a t e p r o d u c e d

by

a process

which i s

e s s e n t i a l l y s i m i l a r

t o the

one

described

i n the aforementioned patent

t o

von

H e r z , N o . 1 , 9 9 9 , 7 2 8 .

The

procedure f o r s e c u r i n g

a

l a b o r a t o r y quan

t i t y o f c u b i c

normal l e a d styphnate

s a s f o l l o w s :

Abo ut

1 0

grams o f styphnic

a c i d

are

suspended

in 100 c c . o f

water

at

a temperature

o f 7 0 t o 7 5

C .

I t

should be

noted

that only

a

r e l a t i v e l y small

. f r a c t i on o f

the s t y p h n i c a c i d g o e s

i n t o

s o l u t i o n ,

t h e major p o r t i o n t h e r e o f remaining i n suspen

s i o n .

While

t h i s

s u s p e n s i o n

i s under

a g i t a t i o n

there i s

added thereto

about 10 c c .

o f

8-normal

p o t a s s i u m

h y d r o x i d e s o l u t i o n ,

and t h e

s t i r r i n g

i s

continued f o r

about 5 minutes. To t h i s admix

ture there i s added a s o l u t i o n

o f

about 20 grams

1 0

1 5

20

35

45

50

55

w

o f

lead n i t r a t e

i n

about 50 c c . o f

water,

the lead

n i t r a t e solution

being'added

at

such a

rate as t o

r e q u i r e

about

1 5

minutes

t i m e .

The

p r e c i p i t a t e

i s normal

l e a d

styphnate

i n c u b i c

c r y s t a l s .

The

novel s a l t

has

an

apparent

d e n s i t y

o f

1 . 5 7

grams/cc. and a l e a d content o f 43.4%. Using

a 300 m m f d . c a p a c i t o r , i t

does

not f i r e a t 3 , 0 0 0

v o l t s , w h e r e a s o r d i n a r y normal l e a d

s t y p h n a t e

g i v e s about 5 0 % ? r e s a t 7 0 0

v o l t s

and

100% ?res

a t

about 1 , 5 0 0 v o l t s .

In

admixture

with 1 0 % ground g l a s s , t h e n o v e l

s a l t

shows,

i n the u s u a l impact t e s t ,

an average

s e n s i t i v i t y o f

4 and a standard d e v i a t i o n

o f 2 ,

as com pare d

with

an average s e n s i t i v i t y of

4.5

and

a standard deviation

o f

2.3 f o r the ordinary

form.

The

d i f f e r e n c e

between

the

molecular s t r u c t u r e

o f

c u b i c

normal

lead

styphnate

and

that

o f

o r

d i n a r y normal l e a d styphnate i s s t r i k i n g l y i l l u s

t r a t e d by t h e i r X-ray

d i f f r a c t i o n

p a t t e r n s ,

r e p r o

duced i n

t h e d r a w i n g . The lower

h a l f o f

the

drawing

i d e n t i ? e d

by numeral 2 shows the famil

i a r

pattern

o f t h e normal

s a l t ,

w h i l e t h e

upper

h a l f

o f

the

drawing

designated a s I i s the pattern

o f the novel c u b i c s a l t . In the l a t t e r ,

the

l i n e s

which c h a r a c t e r i z e and

d e n t i f y

t h e o r d i n a r y s a l t

are absent, and there appears instead

a

pattern o f

l i n e s o f

d i f f e r e n t

placement, width and prom

i n e n c e ,

d e ? n i t e l y i n d i c a t i n g a d i f f e r e n t atomic

arrangement

Ammunition p r i m i n g c o m p o s i t i o n s c o n t a i n i n g

the

novel s a l t

i n

admixture with

the usual o x i

d i z e r s

and

f u e l s

show an average

s e n s i t i v i t y

o f

4.42 and a standard deviation o f 1 . 0 6 , as

com

pared

with

an

average s e n s i t i v i t y

o f 4.94 and a

standard d e v i a t i o n o f

1 . 2 0

f o r

o t h e r w i s e i d e n t i

c a l m i x t u r e s c o n t a i n i n g

o r d i n a r y l e a d

s t y p h n a t e .

I t s c a p a c i t y

f o r i g n i t i n g

o t h e r

p r i m e r i n g r e d i e n t s

and p r o p e l l e n t powders,

a s measured by

the

bar

r e l time o f a p r o j e c t i l e ,

i s

a l s o

s u p e r i o r

t o

that

o f the ordinary s a l t . The average p r o j e c t i l e

b a r r e l time when the novel

s a l t

i s used i s

2 . 9 5

m i l l i s e c o n d s , a g a i n s t

3 . 1 9

m i l l i s e c o n d s

f o r

the

o r d i n a r y

s a l t ,

a l l

o t h e r f a c t o r s b e i n g

i d e n t i c a l .

A

t y p i c a l ammunition p r i m i n g c o m p o s i t i o n

containing the

new

a l t i s

as

f o l l o w s :

T e t r a z e n e , 1%

t o

5%, p r e f e r a b l y

4 %

Cubic

normal

l e a d s t y p hn a t e ,

3 0 %

t o

5 0

% ,

p r e f

e r a b l y

38%

Lead n i t r a t e ,

20 %

t o

40%,

p r e f e r a b l y 25%

Lead s u l p h o c y a n a t e ,

5%

t o 15%,

p r e f e r a b l y 8 %

G l a s s ,

15 %

t o 30%, p r e f e r a b l y 25

The n g r e d i e n t s o f t h i s c o m p o s i t i o n

o t h e r

thanthe

n o v e l c u b i c normal l e a d

styphnate

may

be

v a r i e d

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throughout t h e realm o f t h e

t e a c h i n g s

o f

the

prior

art.

What i s

claimed

i s :

1 .

In

the manufacture o f the

normal lead

s a l t

o f s t y p h n i c

a c i d ,

t h e

method which comprises the

addition t o

a suspension of about 10 grams of

st yph n ic acid in about

100 c c .

of

water

under agi-

tation and at

about

7 0

t o

75 C . o f

about

10

c c .

o f about 8-normal potassium h y d r o x i d e , t h e

f u r

t h e r

a d d i t i o n

with continued a g i t a t i o n

o f

about

2 , 5 8 9 , 7 0 3

~ 1 0

50 c c .

o f

a

40 solution

o f

lead n i t r a t e ,

and

the

recovery

o f

the r e s u l t i n g p r e c i p i t a t e .

2 . The composition o f matter normal lead

styphnate

i n

c r y s t a l s which a r e r e c t a n g u l a r par

allelopipeds

.

3 . An

a mm u n i t i o n priming

composition

con

t a i n i n g normal l e a d

styphnate i n

c r y s t a l s which

are

rectangular

p a r a l l e l o p i p e d s .

4 .

An ammunition

priming

composition

con

t a i n i n g

normal

l e a d

styphnate

i n c r y s t a l s

which

20

4

are rectangular

p a r a l l e l o p i p e d s ,

an o x i d i z e r ,

and

a fuel.

5 . An ammunition priming composition

con

t a i n i n g

normal l e a d

styphnate i n c r y s t a l s which

are rectangular

parallelopipeds,

n o x i d i z e r , a

f u e l , and an abrasive.

JOSEPH F. KENNEY.

REFERENCES- CITED

The

following references are

o f

record

in

the

? l e o f t h i s p a t e n t :

UNITED

STATES PATENTS

Number

Name Date

1,443,328 Herz ____________ _ Jan. 23, 1923

1,889,116

Herz et al ________

_

N o v . 29,

1932

1,942,274

Brun

___________ _ Jan. 2 , 1934

1,999,728

Herz ____________ __

A pr. 30,

1935

2,137,234

Brun ___________

_

Nov. 22, 1938

2,295,104 Gar?eld

_________

__ Sept. 8 , 1942