Year: 1897

page_text: Date of Application, 15th Jan., 1897--Accepted, 20th Mar., 1897
1, FREDERICK WILLIAM JONES, of Barwick, near Ware, in the County of
Herts, do hereby declare the nature of this invention and in what manner the
same is to be performed, to be particularly described and ascertained in and by
the following statement :-
This invention relates to improvements in the manufacture of explosives, which
are more especially intended for use with fire arms, and has reference more
particularly to smokeless or semi-smokeless powders, of the kind or class known as
dissolved or "condensed" powders, that is to say those containing nitro-cellulose
as the principal or one of the principal ingredients, aud which have been subjected
to the action of a suitable solvent or solvents to gelatinize or to dissolve them.
"
The object of the invention is to enable the densities and rates of combustion of
such powders to be regulated or varied, and also to enable a much larger proportion
of slowing or "taming" material to be employed than has hitherto been possible,
without requiring the addition of objectionable metallic nitrates.
Dissolved or condensed powders have usually the objection that the compactness
produced by dissolving nitro-cellulose causes the burning to occur only in layers
parallel to the original surface, the rate of combustion being comparatively slow,
except at high pressures. Consequently to make the powder burn in a gun barrel
very thin grains or laminæ must be employed,, or the grains must be mechanically
perforated at one or more points, so that the burning surfaces do not decrease as
the combustion progresses. Furthermore, with such explosives it is impossible to
use any large percentage of what are known as "slowing" or "taming" ingredients,
without an equally large admixture of an objectionable metallic nitrate.
quently for some fire arms such explosives cannot be used because of the high
pressures necessary for their complete combustion.
Conse-
Various attempts have been made to overcome this objection. Some propose to
use weak solvents, or a method of manufacture that makes a less completely
dissolved or gelatinized product; and others have mixed certain ingredients with
the explosive while in a plastic state, and extracted them after granulation, making
a vesicular grain; whilst others mix with the nitrocellulose base large percentages
of one or more of the more violent explosives, such as nitro-glycerine, nitro-mannite,
methyl nitrate and explosives of like nature.
Now according to my invention I prepare "dissolved" or "condensed " smokeless
powders, by any suitable method and I then submit the powder to one or both of
the following processes..
The first process is conducted in what I term the "swelling bath" which consists
of an aqueous or alcoholic solution of from 20% to 60% of a solvent for the
nitro-cellulose used such as ether, acetone, ketones, and acetic ethers of the paraffins,
and in this the granulated powder is allowed to soak, with or without agitation and
the application of heat, for one or more days. After soaking, the solvent is
extracted by washing, or by passing in steam and condensing the solvent, or, by
some similar process. This bath makes the powder swell and increase in bulk, the
amount of increase being greater, the greater the strength of the solution, the
higher the temperature or the longer the action is continued; it also affects the rate
of combustion so giving a ready means of regulating the density and combustion of
any "dissolved" nowder

page_text: If any ingredient or ingredients in the granulated powder be soluble in this bath,
the bath must first be saturated therewith or the explosive before granulation must
have incorporated with it an additional amount of such ingredient or ingredients so
that the bath leaves the desired amount in the finished powder.
The powder being freed from its solvent is then dried for use.
The second process is only applied to an admixture of the base mentioned
hereinafter, with a solid ingredient or ingredients which will melt below the
temperature of boiling water, and when melted have a solvent action on the base,
such as the di- and tri-nitro derivatives of benzene, toluene, zylene and substances
of like nature. The 66 dissolved" or " condensed" powder made from such
admixtures, is granulated in the usual way, and may or may not be treated in the
"swelling bath." It is then kept in a bath of water at a temperature above the
melting point of the aforementioned ingredient for one or more hours. The effect
of this treatment is to make the rate of combustion vary at different points in
each grain, and, as a consequence, the burning surfaces increase as the combustion
progresses, which, as will be well und erstood, enables one to produce an explosive
for fire arms giving low initial pressures. Also, it minimizes the slowing action
of the taming ingredient, thus allowing the use of a much larger percentage, and
the production of an explosive of very low heating properties, owing to the small
amount of oxygen present in it. Furthermore, the use of large percentages of
these non-volatile substances which are solvents for nitro-celluloses, lessens the
cost of production, as they require very much less volatile solvent to dissolve or
gelatinize them, when making into grain.
The dissolved or condensed powder which I treat as above may be formed from
a base of nitro-cellulose, nitro-hydrocellulose or nitro-oxy cellulose of any degree
of nitration, or from any admixture of these, with or without nitro-glycerine.
With this base I mix, if necessary, one or inore substances for regulating or
slowing the combustion, such as the nitro- and amido-derivatives of the aromatic
series of carbon compounds, picrates, nitro-naphthols, resins, graphite and such
other substances as are now commonly used for this purpose. The composition
and granulation of the powder is of course adapted for the purpose intended.
The following are however three general compositions between the limits of
which powders for every kind of fire arm can be made by my processes.
Slowing material, such as the di- and tri-nitro-
benzene, toluene, and zylene
0% to 25%
The above ingredients are either mixed together in the wet state and then dried,
or the dry nitro-cellulose is treated with its solvent containing the other ingredients
in solution.
"
For the usual preliminary "dissolving" or condensing prefer to use as a
solvent a ketone, preferably either acetone or methyl-ethyl-ketone, owing to the
ease with which they can be separated from the explosive and the purity of the

page_text: commercial product. The amount used depends on the percentage of nitro-
glycerine and slowing material in the composition, but it varies from 60 to 20 parts
by weight for every 100 parts of the original composition.
The volatile solvents being mixed with the dried composition, by any suitable
methods, the whole is left in a vapour tight vessel for some hours with or without
the application of heat until the vapours of the solvent have effected the substances
to be dissolved, when it is placed in an incorporating and mixing machine, and
kneaded or worked until the whole is gelatinized. The gelatinized mass is rolled
into sheets, or forced through dies of definite dimensions, and afterwards divided
into grains or laminæ in any suitable manner. The dimensions of the granulated
powder, will of course, vary according to the purpose for which it is made, and the
energy desired from the explosive. Thus, for military purposes a grain or lamina
would vary in thickness from 0.015 inch upwards, while for sporting rifles, shot-guns
and rim-fire cartridges the thickness would vary from 0.015 inch downwards.
These granulated products may now be treated by one of the following methods.
(1) They may be acted on in the "swelling bath," with or without the
application of heat, to decrease the density and regulate the combustion. Thus, if
a granulated powder made of pure nitro-cellulose, is heated with a 20% aqueous
solution of acetone, the powder changes colour and swells so that the density
thereof is only two-thirds of the original, and the bulk approximates more closely to
that of black powder, as a consequence of which it will fill existing cartridge cases
much better than condensed powders that have not been so treated; also its
combustion is so affected that it will burn under very low pressures, and can
therefore be used in guns where the original powder would be only partially
consumed, owing to the high pressures necessary for complete combustion.
(2) If they contain rather large percentages of slowing material, or any
nitro-glycerine, they may be acted on by the "swelling bath" only in the cold, and
the solvent freed from the explosive by washing it with cold water to avoid the
extraction of these materials. After extracting the solvent, it may be boiled in
water to fuse the slowing material, and make the rate of combustion vary at
different parts of the grain.
(3) Those granulated powders whose density must be as high as possible, and
which contain ingredients that have when fused, a solvent action on the base,
may be kept at a temperature above the melting point of the aforesaid ingredient
for a definite period, for the purpose of affecting the combustion of the parts of
each grain.
"
When so treated comparatively large percentages of "slowing or taming
ingredients can be used and an explosive of low pressure and low heating properties
can therefore be obtained.
For instance if a granulated dissolved or condensed powder containing 20% of
di- or tri-nitro-benzene, toluene or xylene be boiled in water for one or two hours,
the grains lose their gelatinous appearance and develop entirely different ballistic
properties. The fused ingredients not being sufficient to act as solvents on the
whole of each grain leave certain parts less acted on and quicker in combustion,
the partially burnt grains becoming perforated and the burning surfaces increasing
as the combustion progresses.
If any of the ingredients are to any extent soluble in water, such as
dinitrotoluene, this must be taken into account so that the correct amount is left
in the finished product.
In all cases it is desirable to submit the finished product to a washing operation
before drying.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what I
claim is :-
or
1. The method of varying the density and rate of combustion of a "dissolved"
❝ condensed smokeless or semi-smokeless powder which consists in treating

page_text: "
the same with a "swelling bath' or solvent for the nitro-cellulose therein,
substantially as and for the purpose described.
2. The method of affecting the combustion of a "dissolved or "condensed"
smokeless or semi-smokeless powder which consists in heating the same to a
temperature sufficient to liquefy one or more of those ingredients thereof which will
exert a solvent action on the remainder, substantially as described.
3. The method of varying the deusity and rate of combustion of a "dissolved"
.or "condensed "smokeless or semi-smokeless powder which consists in treating
the same with a 66
swelling bath" or solvent for the nitro-cellulose therein, and
subsequently heating the same to a temperature sufficient to liquefy one or more
of those ingredients thereof which will exert a solvent action on the remainder,
substantially as described.
"
35,
"
4. A smokeless or semi-smokeless explosive produced from a ❝ dissolved or
condensed powder rendered bulky and more rapid in its combustion at low
pressures substantially in the manner hereinbefore described and for the purpose
specified.
5. An explosive consisting of one or more of the nitro-celluloses herein nained,
with or without nitro-glycerine, mixed with 10% to 30% of the di- or tri-nitro-
derivatives of benzene or its analogues, and treated substantially as herein
described.
6. My improvements in' the manufacture of explosives substantially as herein-
before described and for the purposes set forth.
1
T
1007
HASELTINE, LAKE & Co.,
45 Southampton Buildings, London, W.C., Agents for the Applicant.