Patented Feb.

7, 1933
1896,642

UNITED STATES PATE INT (OFFICE

ARTHUR. S. O’NEIL, OE ALTON, ILLINOIs, AssIGNOR. To WESTERN CARTRIDGE CORGI
PANY, OF EAST ALTON, ELLINOIS, A CORPORATION OF DE LAWARE
SOCESS OF EAENG NESO CELOSE POWDERS
No Drawing. Continuation of application Serial No. 589,722, filed September 21, 1922. This application
filed April 1, 1927. Serial No. 183,013.
This invention relates to explosives and final product is raw cellulose or cotton as
more particularly to nitrocellulose powders. ordinarily used in the manufacture of nitro
This application is a continuation of appli cellulose. It is not necessary to describe the
cation
1922.
Ser. No. 589,722, filed September 21, preliminary treatment, since that is well
known to those skilled in the art, consisting 55
One of the objects of this invention is to as it does of purifying
develop a process for producing the explo trating the purified cellulose the raw, cellulose, ni
sive in a simple and economical manner. and purifying
the nitrated cellulose. Further detailed de
Another object is to provide a process scription can, therefore, begin at the point
8 whereby the ballistic properties of the ex where the cellulose has been nitrated and
60
plosive can be closely controlled so as to ob purified and is ready to be pulped.
tain a finished product having the desired The pulping operation is performed as a
properties for the specific uses intended. beating operation; this is an important pro
Another object is to provide a process in cedure
which the necessity of solvents is obviated. one of astheit ismost
by means of this operation that
Another object is to provide an explosive ties, that is the important
rate of
ballistic proper 65
combustion of the
and more particularly a propellent powder finished powder, is controlled. The beating
having improved characteristics and prop operation is carried out in any of the various
erties so as to adapt the same for the spe types of beaters such as are used in the paper
20 cific uses intended. industry, examples of which are the Hol 70
Further objects will appear from the de lander, Jordan, Miller, Downingtown, etc.,
tailed description in which will be described types. One of the functions of the beating
a number of embodiments of this invention; operation is to cut the fiber to the proper
it will be understood however that the de length for felting; another important func
25 scribed embodiments are simply for illustra tion, however, is to convert a part of the
tive purposes since this invention is suscep cellulose to the hydrated condition, for cellu
tible of various other embodiments. lose is converted into hydrated cellulose due
Generally stated, in accordance with this to the mechanical action of the beater. The
invention, the nitrated cellulose is pulped to degree of hydration is controlled by the
30 a consistency so as to enable it to be felted. length of time of the beating operation and
The pulp nitrocellulose is gathered or felted by adjustment of the beater itself. The de 80
into a sheet. This sheet is then subjected to gree of hydration controls the rate of burn
wringing, drying and compressing opera ing of the finished powder and also reduces
tions so as to free the same of water and re the flame, and I have found that nitrocellu
85 duce it to the required dense state in order to lose containing as high as 13.2% of nitrogen
85
adapt it for the uses for which it is intended. can be hydrated to such a point that its burn
The apparatus employed for the carrying ing rate is no greater than that of raw cel
out of the process embodying this invention lulose. Thus by controlling the time and
may, generally stated, be the same as now adjustment of the beating operation I can
40 used in the manufacture of paper; accord
control the burningrate of the Mfinished pow 90
ingly in the description to follow the ele der to any desired degree.
ments and machines of a paper making plant But I am not limited to this method of con
will be referred to by their names as com trol as I have other means of control in this
monly used in the paper making industry. same operation. For instance, I can use a
From a process standpoint however, there mixture of nitrocellulose of different degrees 95
are certain differences in essential operation of nitration and so obtain a finished product
which must be clearly understood in order. of any desired degree of nitration. Then
to enable one skilled in the art to practice the too I can addinert material such as raw cot
50
process embodying this invention. ton to the mixture in the beater. This not
The raw material forming the basis of the only slows down the rate of burning of the 00
 2. 1,898,342.
finished powder but also adds materially, to controlling the rate of the burning of the
the mechanical strength of the finished finished powder.
Powder made in this manner will require
product. the addition of a stabilizer such as diphenyl 70
Another advantage of adding raw cotton amine; this is best added to the pulp in the
in the beating operation is that the raw cot stuff chest, although in some instances it can
ton can be hydrated more readily than the be added during some of the later operations.
nitrated cellulose so that I can take advan
From
tage of both the amount of raw cotton as a paper machine the stuff chest the pulp is taken to
well as the degree of hydration to which it is ries of screens toafter passing through a se. 75
brought for controlling my finished product. foreign material. remove any particles of
Here the fiber is felted
As mentioned above, one of the advantages and formed into a sheet while the water is ex
of adding raw cotton is that I can obtain tracted and the sheet condensed
a stronger sheet of nitrocellulose paper. quirements. The paper machineto meet re
may be 80
Nitrocellulose alone when formed into a sheet
of paper without hydrating any of the fibers either
type,
of the cylinder type, of the Fourdrinier
or it may be a combination machine.
has very little mechanical strength due to Which ever type of paper making machine
the brittleness of the fiber itself. By adding is used the fiber
raw cotton and allowing the same to hydrate sheet in the sameis manner felted and formed into a
as in the manu
during beating, this lack of strength is en facture of paper. The sheet of nitrocellu 85
tirely overcome and the fibers themselves lose as received from the wet end
appear less brittle, due to their being coated machine can be dried by passingofita over paper
a
with a film of hydrocellulose.
Another interesting as well as important regular paper machine drier. Suchcylinders
a drier
effect, traced directly to both the addition consists of a series of gear-driven
of raw cotton and to the hydration of the The wet sheet of nitro cellulose is passed over 90
heated with either exhaust or live steam.
nitrocellulose is the elimination of static. a series of such rolls as required to evaporate
This is especially apparent in the calender the
ing operation where most trouble from static beenmoisture remaining after the water has
Squeezed and wrung out in the paper 95
charges appears.
30 While have mentioned raw cotton as an making machine. Of course the sheet could
addition agent in the beating operation I do e.dried by passing it through a drying cham
not wish to limit myself to this particular The sheet of nitrocellulose as it comes from
form of cellulose as I can obtain similar
the driers is preferably calendered by pass 00
results by using cellulose in other forms such ing
as woodpulp, flax, straw, jute, etc. between the rolls of an ordinary paper
After the pulp has been beaten to the calendering
rolls, the
machine consisting of a stand of
pressure between any pair of which
proper consistency it is transferred to what can be varied to suit
is known in the paper industry as a stuff sary one or more pair conditions.
of rolls can
If neces
be steam
chest, which is a large vat or tank contain heated so as to have a hot calender action.
ing a mechanical agitating device. Its func
tion is to retain the stock as received from This is particularly advantageous when the
the beaters and to permit it to be diluted to pulp contains such deterrents as dinitrotolu
the proper consistency for felting. At this ene, waxes, etc., since the heat melts the same
and secures a more uniform distribution of 0
point this provides another impor
45 tant control of the properties of the finished
the deterrent. The calendering operation
material, for it is in the stuff chests that the offers
the
excellent opportunities for controlThe
burning rate of the finished powder.
of
various modifiers, such as deterrents or ac
celerators as well as stabilizers may be added greater the pressure employed in the calen
as required for any particular purpose. dering operation the greater is the density 115
50 Among the deterrents which can be added of the finished sheet; accordingly as the rate
in the stuff chests are starch, either raw or of burning varies inversely as the density the
gelatinized, casein, glue, nitro compounds former can be accurately controlled. -
such as dinitrotoluene, nitroguanidine, tri byThe sheet of nitrocellulose paper obtained
the process above described is now ready
cresylphosphate, camphor and waxes, such to be made into suitable form. for use as a 20
55 as paraffine, ceresine, or even such compounds propellant in either small arms or artillery.
as latex rubber. In adding deterrents such For use in pistols, rifles, and shotgun shells
as dinitrotoluene, waxes etc., which have a
comparatively low melting point, we take the sheet is best cut or punched into flakes of
suitable size and shape. This can be done
advantage of the fact that in some of the on any suitable type of cutting, machine. 25
60 later operations sufficient heat is applied to
Before cutting into shape, the sheet of
the formed sheet to melt these bodies and nitrocellulose
thus form a homogenous coating on the indi with a resulting can still be further modified
vidual fibers which make up the sheet. I properties. Thismodification
treatment
of its ballistic
consists in either
have therefore a very efficient means as well 30
65 as one which can be closely controlled for spraying with or passing through a bath
 1,896,642 3
A. of suitable solvent such as acetone, ethyl ace This will result in a progressive burning.
tate, ether, alcohol, etc. This will colloid the powder, but, in addition, the high mechanical
surface of the sheet rendering it somewhat strength of the outer layer will help support
slower burning. As the center of the sheet the comparatively weak interior of pure high
5 is not affected by the solvent but retains its nitration cotton. - (0
original fibrous condition this will be faster The few foregoing examples show the
burning than the exterior colloided surface, great possibilities of this process as worked
resulting in a more progressive burning type out on the cylinder type of paper machine.
of powder. They also indicate the larger number of pos
For large bore guns the sheet of nitrocellu sible resulting in a close con 75
lose, either calendered or uncalendered, can trol ofcombinations
be rolled into tubes or cylinders of any desired While the use of a of
the properties the finished product.
length, wall thickness and diameter of longi chine will result in a good sheet ofpaper
Fourdrinier
material,
ma
tudinal perforation. The adhesive used for
15 making the cylinder can be one that will act it does not offer the same possibilities as the
as a deterrent, such as glue, casein or gelat not cylinder machine. On the other hand, it does
inized starch, or it can be such as material limit these possibilities but makes their
application a little more awkward. It is not
as nitrocellulose in a suitable solvent. These possible to buildup
latter solutions can also contain gums such a duplex or multiple sheet
20 as kauri, copal, etc. This method of forming on an ordinary Fourdrinier machine, but
even so this can be done by means of an ad
the sheet into cylinders, makes a very flexible ditional
process for manufacturing propellants for up a slow operation. For example, I can make.
any size of artillery. burning sheet and also a faster
in accordance with the process embodying above. Theseby separate
burning one any of the methods outlined
sheets can then be
this invention, it is not only possible to pro combined
duce a sheet of nitrocellulose of a single ply, by passing the three sheets thruof athree
into a single sheet
system
plies 90
of
but it is also possible to produce a multi-ply rolls doubling machine using a suitable ad
sheet by the employment of a multi-cylinder hesive. This is a common operation in paper
type paper machine, In this way, it is pos
30 sibe to build up a multiple sheet of nitrocellu mills and is employed for such purposes as
lose; that is, a sheet made of two or more plies. making
This
double lined board.
process of forming several layers into
95
The advantage of this is at once apparent one sheet lends itself to another valuable
to anyone versed in the art of propellant ex method of making a progressive burning
plosives. For the sake of illustration
35 consider a three ply sheet. The two outer
we will powder. The two outer sheets can be made of
a comparatively
plies can be made from low nitration cotton, while the inner sheet slow burning composition, 00
say 12.6% nitrogen content while the middle sheet of nitrocellulose can be made from a
colloided with nitro
or inner layer can be made of high nitration glycerine. From this it is also apparent
cotton of, say, 13.2% nitrogen content. I that
can thus build up a sheet of powder, the outer densethis or
process can be used for making
colloided powders, using any solvent 10s
surfaces of which will have a slower rate of or colloiding agents such as acetone, nitro
burning than the interior or core. This will glycerine, ethyl acetate, ether alcohol mix
result in a truly progressive burning type of ture, etc. l
powder. I can go even farther than this, and The adhesive used can be suchS. as a solu
45 make, for instance, a five ply sheet containing
tion of gun cotton in a suitable solvent. This 8
nitrocellulose of three different degrees of solution
nitration, progressing from slower burning etc., which can carry such deterrents as D.N.T.,
in the outer layers to faster burning towards starch could are also
soluble in it. Gelatinized
be used; this would not only
the center, or vice versa, if desired.
50 In addition to controlling the rate of burn cooling effect of oftheburning
decrease the rate
starch,
but, due to the 16
would reduce
ing of the different layers by means of the the flame of the explosion, thus
degree of nitration, I can control them by wards a flameless propellant. tending Adhesion
to
the addition of deterrents or accelerators in could also be obtained by spraying with, or
the stuff chest. For example, I can take a
55 low nitration cotton, such as 12.6% nitrogen passing thru a bath of suitable solvent, such
and slow it down still more by the addition This as acetone, ethyl acetate, ether alcohol, etc. 20
of gelatinized starch or D. N.T. This will rial but would not only act as a binding mate
be used for the outer plies of my sheet. For ing of the would also modify the rate of burn
the inner layer I can take some of the same finished powder. Thus it can be
60 nitrocellulose and increase its speed of burn seen that a large number of combinations
ing by the addition of suitable compounds product with corresponding properties of the finished
can be obtained. c.
les
such as barium nitrate. As another example, Having thus described the invention what
I can use nitrocellulose containing raw cot is claimed is: k
ton and hydrated cellulose for the outer layer 1. The process of making explosives com
65 pure high nitration cotton for the inner layer. prising, converting part of the cellulose of 30
 4 1896,342.
nitrocellulose pulp to a hydrated condition
and felting or gathering the so partially con
verted pulp into a sheet.
2. The process of making explosives com
prising, beating nitrocellulose pulp so as to
cause partial hydration thereof and felting
or gathering the so partially hydrated pulp
into a sheet.
3. The process of making explosives com
10 prising, beating nitro-cellulose pulp so as to
cause partial hydration thereof, and contin
uously felting the same into a continuous
web which is thereafter continuously passed
through driers and calenders in order to pro
5 duce the finished sheet.
4. A process of making propellant powders
in which nitro-cellulose is pulped by beating,
gathered from a stuff chest and felted into a
sheet, characterized by the feature that the
20 beating is selectively carried on to an extent
sufficient to reduce the degree of nitration of
the nitro-cellulose.
5. A process of making propellant
powders in which nitro-cellulose is pulped by
25 beating, gathered from a stuff chest and felt
ed into a sheet, characterized by the feature
that the beating is selectively carried on to an
extent sufficient to partially convert the nitro
cellulose into hydro-cellulose. .
30 In testimony whereof affix my signature
this 29th day of June, 1926.
ARTHUR. S. O’NEIL.
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