Patented Nov.

30, 1943 2,335,804

UNITED STATES PATENT OFFICE . 2,335,804

.
PROPELLENT Powder,
Charles Earnest Silk, Aiton, Ill., assignor to
Western Cartridge Company, East Alten, H., k
a corporation of Delaware m
No Drawing. Application September 21, 1940,
Serial No. 357,53
8 Claims. (C. 52-13)
This invention relates to propellent powders, suitable for use in the surface-treatment of
and more particularly to progressive-burning powder grains in accordance with this invention,
Smokeless powders characterized by surface treat- . (the approximate melting points in degrees C.
ment with new and improved deterrent materials. being indicated in parentheses) are: diphenyl
It has been known in the art of propellent (73), di-p-cresyl (84), di-o-cresyl (110), di
explosives that increased projectile velocities 2,4,5 trimethyl phenyl (119°), and di-o-naphthyl
could be secured, while maintaining safe breech (155°) phthalates.
pressures in the firearm, by Surface treatment of The foregoing and other like esters may be
the powder grains with deterrents, this result be applied as the deterrent coating on single- or
ing obtained by decreasing the combustion rate of multiple-base powder grains of the desired shape
the initially burning portion of the powder grains. and size in accordance with any suitable method.
Many materials have heretofore been proposed The preformed grains of smokeless powder may
for use as smokeless powder deterrents, such as . . be composed of nitrocellulose or other gelatin
aromatic nitrohydrocarbons, dialkyl phthalates, izable nitrated carbohydrate smokeless powder
. . dialkyldiaryu reas, and a variety of waxes, fats, 5 base, for example nitrostarch, alone or in com
and resins. bination, and, if desired, may contain in addition
Despite the many proposals which have been One or more nitrated polyhydric alcohols, for
made in this art, improvements have been de example, nitroglycerin nitroglycol, and the like
sirable in several aspects, notably in providing. and/or an aromatic nitrohy Ocarbon such as
deterrent materials which may easily be applied 2) di- or trinitrotoluene. The urface-treatment
as a coating on powder grains without undesirable - may advantageously be effected as described in
agglomeration of the grains, which results in the following specific examples, in which detailed
ballistically as well as chemically stable grains,
and which act with greater efficiency.
directions are supplied in order fully to. illustrate
the invention. .
It is therefore an object of this invention to 25 In One method, the grains may be surface
provide improved progressive-burning smokeless treated while suspended by means of vigorous
powder grains. m agitation int, an excess of a non-solvent liquid.
Another object of this invention is to provide For example, the smokeless powder grains may
surface-treated smokeless powder grains having be vigorously agitated in about six times their
* a desirable combination of ignitibility, reduced 30 weight of water, (at a temperature of about 65°.
initial combustign rate, appropriate density, and C., contained in a Suitable jacketed. Wessel. The
balistic Stability. diaryl phthalate may be emulsified in a separate
. Other objects will appea from the following vessel in ten to fifteen times its weight of hot
detail description. . . . . . water containing about 0.1% (based on the
In accordance with this invention, generally 35 weight of ester) of gum arabic or other suitable
stated, the foregoing objects are accomplished by protective colloid such as starch, methyl cellulose,
employing a diaryl phthalate as the surface gelatin, or the like, and the emulsion added to
treating agent for smokeless powder grains. This the suspension of the powder grains. The tem
class of phthalate esters has been found to possess perature may be maintained at about 65°C. and
particularly advantageous properties for such use. 40 agitation continued for a suitable period, for ex
The solvent and plasticizing properties are con ample 22 hours when the deterrent coating
ducive to rapid absorption at the surface of the amounts to 5% of the weight of powder being
smokeless powder grains and the resulting prod treated. If desired, for insuring stability of the
uct is characterized by a uniform, stable, and coating, the grains may be maintained at an ele
readily ignitible surface layer. Due to the rela 45 vated temperature of 50-70° C., with or without
tively high melting point, substartially higher agitation, for an additional period up to about 24
concentrations can be tolerated in the Strface hours. The suspension is then cooled during
layer of powder grains without causing tackiness agitation, the excess liquid removed by filtration
than is the case with liquid deterrents previously or centrifuging, and the grains washed with
in use, and accordingly greater deterrent effect 50. Water. The product may then be dried, as by
may be secured. Furthermore, by reason of their treatment with warm air heated to 50° C for
extremeinsolubility in water, the novel deterrents Several days, graphited, brought to equilibrian
enhance the water. resistance of the treated with
powder grains.
the desired relative humidity, and& stored
ready for use.
Representative diaryl phthalates, which are iss In accordance with another well-known type
.
 2,885,804
of coating process, the treatment may be carried base powder coated in identical manner in ac
cordance with the first specific example described
out in a "sweetie barrel,' consisting of a rotat above, (a) with diphenyl phthalate exemplifying
able cylinder partly immersed in a temperature the new and improved deterrent substances, and
controlling bath or provided with other suitable
means for heating and cooling the contents. 5; (b) with symmetrical diethyldiphenylurea, exem
The powder grains, containing from about one plifying one of the most extensively used deter
fourth to one half their weight of water, are rents of the prior art. The base powder employed
placed within the treating cylinder, which is then consisted of gelatinized spherical grains, as de
rotated while the temperature is raised. When scribed in U. S. Patent 2,027,114, consisting of
the grains have become heated to a temperature 10 nitrocellulose, 2% incorporated dinitrotoluene
and 15% nitroglycerin, having a gravimetric
of about 70 C., the diary phthalate is added, density of 0.84 and average grain diameter of
rotation of the treating cylinder being continued. 0.019 inch. The deterrent coating amounted in
This rotation and the consequent agitation and each case to 5% by weight of the powder. The
mixing of the grains is maintained for a period resulting powders, having gravimetric densities.
of about 15 minutes after the addition of the of (a) 0.86 and (b) 0.84, were loaded and fired
deterrent has been completed. The mixture is in .30 caliber-1906 ammunition having a bullet
then cooled to room temperature by continuing Weighing 150 grains. In this ammunition, a 36.8
the rotation while cold water is circulated through grain charge of the uncoated powder produced
the temperature-controlling bath. If additional a muzzle velocity of 2470 feet per second at a
heat treatment of the grain is desired, the grains 20
pressure of 45,000 pounds per sq. in. The com
Inay be maintained Submerged under hot, Water parative test data are listed in the following
in a Suitable vessel for the required period. After
removal of the excess water by filtering or cen table:
trifuging, the product may be dried, graphited,
brought to equilibrium at the desired relative Deterrent
humidity, and stored ready for use. . r
Aryl phthalates which are characterized by (a) Diphenyl (b) Diethyl
a melting point between 60°. C. and about 100° phthalate diphenylurea
C. may be applied in accordance with the above
procedures, since the treatment of the powder 30 RESULTS OF FIRING AT NORMAL TEMPERATURE
grains can then be carried out at a convenient
temperature, somewhat above the melting point Powder charge----------------grains. 46.5 47.5
of the particular deterrent employed. However, Pressure.------------------lbs./sq. in.
Muzzle velocity--------------- ft.fsec-
43,900
2,682
45,000
2,680
aryl phthalates having melting points above 100°
C. may also be utilized in the surface treatment RESULTS OF FIRING AT-40° C.
.0f powder grains at convenient temperatures
Substantially below iO0° C. (that is, at tempera 38,200 35,100
tures at which the deterrents themselves are 5,700 9,900
Solid) either by employing then in admixtures 2,559 2,56
123 164:
which are liquid at the desired temperature, or N.
by applying the deterrent in the form of a solu The diaryl phthalate deterrent in accordance.
tion in a suitable solvent. . With this invention displayed superior results
Where a solvent is thus employed, it should particularly with respect to efficiency (a smaller
be sufficient in amount to render the deterrent charge of the powder treated therewith being
Substance liquid at the temperature of the treat required to provide the desired ballistics) and in
ment and should be sufficiently volatile SO as to the ignitibility of the coated powder (shown by
be readily removed from the powder grains dur smaller
ing the subsequent drying treatment. Prefer loweringchanges in the ballistic properties on
the firing temperature from about
ably, a solvent is employed for the deterrent 50 25 C. to -40 C.).
which is not a solvent for the smokeless powder
base, for example, aromatic hydrocarbons such grains Microscopic examination of thin sections of
as benzene or toluene, chlorinated hydrocarbons of the diphenyl-phthalate-coated powder
such as ethylene dichloride, trichloroethylene, or revealed the presence of a uniform surface layer
carbon tetrachloride, alcohols such as ethyl or 55 in which the novel deterrent was concentrated.
isopropyl, or a solvent naphtha of suitable vola Similar, study of the grains after storage of the
tility. However, it may be advantageous at times, powder at 50° C. for 30 days showed that no
in order to facilitate the coating treatment Curred.appreciable alteration of this structure had oc
and/or secure greater penetration into the pow Firing tests carried out after this period of
der grains, to add to the deterrent solution a 60 storage
volatile Solvent for the powder grains, for exam Sence ofatany 50 C. likewise substantiated the ab-.
significant change in the ballistic
ple, low boiling esters or ketones such as ethyl properties of diaryl-phthalate-coated powder.
E. isopropyl acetate, acetone, or ethyl methyl ke grains on being subjected to elevated tempera
Ole.
The amount of deterrent employed may vary 65 tures, this result representing a considerable im
provement over liquid ester deterrents such as
in accordance with the type of base powder being diethyl phthalate heretofore in use.
treated and the ballistic characteristics desired.
In general, however, an amount between A and It will be understood that the invention is not
about 5% by weight of the powder grains will to be limited to the. Specific details stated above
provide the desired results, it being understood but that variations may be made, as will be
however, that somewhat higher proportions may 70 realized by those skilled in the art, which are
contemplated within the scope of the following
be employed when necessary. -
As illustrative of the advantages which may claims.
be Segured by use of the deterrents in accord Having now described the invention, what is
ance with this invention, the following table claimed as new and is desired
Letters Patent, is: -
to be secured by
contains ballistic test data obtained with a given 75
 2,835,804 3
6. Multiple-base propellent powder grains sur
1. Propellent powder grains surface-treated face-treated
with a diaryl phthalate. with diphenyl phthalate.
2, Propellent powder grains surface-treated 7. Nitrocellulose-nitroglycerin propellent pow
with diphenyl phthalate. der grains Surface-treated with a diary phthal
3. Single-base propellent powder grains sur w ate.
face-treated with a diary phthalate. 8. Nitrocellulose-nitroglycerin propellent pow
4. Single-base propellent powder grains sur der grains surface-treated with diphenyl phthal
face-treated with diphenyl phthalate. ate.
5. Multiple-base propellent powder grains sur CHARLES EARNEST SILK.
face-treated with a diaryl phthalate. O