Improvements in the Manufacture of Gunpowder.
Year: 1890

page_text: Date of Application, 7th June, 1890
Complete Specification Left, 5th Mar., 1891-Accepted, 11th Apr., 1891
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Gunpowder.
1, HUBERT KOLF, of Bonn, in the Empire of Germany, Chemist, do hereby
declare the nature of this invention to be as follows:-
My invention relates to the manufacture of a smokeless or nearly smokeless
gunpowder which is especially free from danger by reason of the non-employment
of picric acid, picrates and chlorates, the use of which, or of ingredients of a similar
nature than hitherto rendered the manufacture, and also the manipulation of so
called smokeless gunpowder, dangerous.
According to my invention I obviate this objection by the use of carbon-hydrates
and plants or their waste products which possess the qualities of carbon-hydrates in
a nitrogenous condition. The materials containing carbon-hydrates are grain, malt,
malt-flour and waste from the mash, forest moss, rushes,. osiers, Iceland moss, cut-up
turnips, Saint John's bread, the roots, stems and leaves, of plants of the genus
althaea and waste of all kinds resulting from the manufacture of starch, and from
breweries and distilleries.
In carrying out my invention the hereinbefore described materials containing
carbon-hydrates are nitrated in the usual manner by treating them with nitric acid
and sulphuric acid, preferably at a temperature of between 20° to 30° C. in vessels
or vats under a pressure of from 2 to 5 atmospheres. The nitrated mass, after
having been drained and thoroughly washed in cold water to completely free it from
acid, is dried in a temperature of about 40° to 50° C. and then crushed or ground;
or the crushing or grinding can be effected while the material is in a semi-dry
condition whereby greater safety would be ensured.
For the purpose of causing regular combustion of the powder and to regulate the
point of combustion I introduce sulphur into the powdered nitrated mass, by
treating it with a sulphide of hydrogen, water containing sulphide of hydrogen,
sulpho-hydrates of sulphur-metals sulphuret of potassium, sulphide of sodium,
sulphuret of calcium or poly-sulphides. The sulphurizing materials are caused to
act on the nitrated powdered mass under a pressure of, say, about 5 atmospheres.
In about 2 hours' time the nitrated and sulphurized mass is freed from the
sulphurizing substances by carefully washing it and it is then treated with a
suitable oxygen-yielding medium (after first drying it in a temperature of from 60°
to 80° C.) by submitting it to the action of a solution containing about 5 to 20 per
cent. of nitrate of potassium, sodium or ammonium at an ordinary temperature for
about 12 hours under a pressure of, about 4 to 5 atmospheres produced, preferably
by compressed air or hydraulic power. To separate any superabundant nitrate
which has not been intimately absorbed by the mass and would therefore prevent
or destroy the homogeneity or uniformity of the product the latter is quickly
rinsed or dipped in cold water and then dried in a temperature of about 80° C.
To bring the product into compact granular or prismatic form I treat or damp or
soak it in solution containing 2% of a binitro combination of one of the before
named materials containing carbon-hydrates or of cellulose and is then by pressure
formed into grains, cakes or prisms as desired, and when dried it is ready for
packing or for use.
The advantages of the smokeless or nearly smokeless powder produced according
to my invention over that manufactured by the ordinary process are that no picric
acid, picrates, chlorates nor other explosive bodies are used in its manufacture and
consequently safety is ensured in manufacturing and manipulating it, it can be

page_text: produced at a low cost, its manufacture is simple and the product is more uniform
or homogeneous and of better consistency which causes greater evenness of
combustion.
Dated the 7th day of June 1890
G. F. REDFERN & Co.,
4, South Street, Finsbury, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Gunpowder.
I, HUBERT KOLF, of Bonn, in the Empire of Germany, Chemist, 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:-
My invention relates to the manufacture of a smokeless or nearly smokeless
gunpowder which is especially free from danger by reason of the non-employment
of picric acid, picrates and chlorates the use of which, or of ingredients of a similar
nature has hitherto rendered the manufacture, and also the manipulation of so-called
smokeless gunpowder, dangerous.
According to my invention I obviate this objection by the use of carbon-hydrates,
or plants or their waste products which possess the qualities of carbon-hydrates, in
a nitrogenous condition. The materials containing carbon-hydrates are grain, malt,
malt-flour and waste from the mash, forest-moss, rushes, osiers, Iceland-moss,
cut-up turnips, locust beans, the roots, stems and leaves of plants of the genus
althea and waste of all kinds resulting from the manufacture of starch, and from
breweries and distilleries.
In carrying out my invention the hereinbefore described materials containing
carbon-hydrates are nitrated in the usual manner by treating them with nitric acid
and sulphuric acid preferably at a temperature of between 20° to 30° C. in vessels
or vats under a pressure of from 2 to 5 atmospheres. The nitrated mass, after
having been drained and thoroughly washed in cold water to completely free it from
acid, is dried in a temperature of about 40° to 50° C. and then crushed or ground;
or the crushing or grinding can be effected while the material is in a semi-dry
condition whereby greater safety would be ensured..
For the purpose of ensuring regular combustion of the powder and to regulate
the point of combustion I introduce sulphur into the powdered nitrated mass by
treating it with a sulphide of hydrogen, water containing sulphide of hydrogen,
sulpho-hydrates of sulphur-metals, sulphuret of potassium, sulphide of sodium,
sulphuret of calcium or poly-sulphides. The sulphurizing materials are caused to
act on the nitrated powdered mass under a pressure of, say, about 5 atmospheres.
In about 2 hours time the nitrated and sulphurized mass is freed from the
sulphurizing substances by carefully washing it and it is then treated with a
suitable oxygen-yielding medium (after first drying it in a temperature of from 60°
to 80° C.) by submitting it to the action of a solution containing about 5 to 20 per cent.
of nitrate of potassium, sodium or ammonium at an ordinary temperature for about
12 hours under a pressure of about 4 to 5 atmospheres produced, preferably, by
compressed air or hydraulic power. To separate any superabundant nitrate which
has not been intimately absorbed by the mass and would therefore act prejudicially
to the consistency of the product the latter is quickly rinsed or dipped in .cold
water and then dried in a temperature of about 80°.
To bring the product into compact granular or prismatic form I treat or damp or
soak it in a solution containing 2% of a binitro-combination of one of the before
named materials containing carbon-hydrates or of cellulose and I then form it by
pressure into grains, cakes or prisms as may be desired, and when dried it is ready
for packing or for use.

page_text: It will be obvious that the solution used for the above stated purpose may also
be employed in a more or less concentrated form and can be produced in the
product obtained as before described and which already contains nitro-carbon
hydrates by simply damping it with one of the known solvents for dissolving the
nitro-carbon hydrate instead of a prepared solution. For this purpose acetic ether,
acetone or oil of camphor can be employed and the excess of liquid therefrom can
be abstracted either by a pump or by centrifugal force or by distillation, after
which the moulding or pressing may be effected.
The advantages of the smokeless or nearly smokeless powder produced according
to my invention over that manufactured by the ordinary process are that no picric
acid, picrates, chlorates nor other explosive bodies are used in its manufacture and
consequently safety is ensured in manufacturing and manipulating it, it can be
produced at a low cost, its manufacture is simple and the product is more uniform
and of better consistency which causes greater evenness of combustion.
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
1. The manufacture of smokeless or nearly smokeless gunpowder which can be
manipulated without danger, characterized by the use of nitrated carbon-hydrates
or plants such as those herein mentioned or their waste products containing carbon-
hydrates, which are,
(a) Sulphurized by treatment with a sulphide of hydrogen, sulpho-hydrates or
poly-sulphides under pressure.
(1) Impregnated with oxygen-yielding mediums by treatment with a solution
of the same under pressure.
(c) The product thus obtained is moulded by pressure with a binitro-carbon-
hydrate or a binitro-combination or with their solvents such as acetic ether,
acetone or oil of camphor into the desired form.
2. As a new article of manufacture the herein described smokeless or nearly
smokeless gunpowder consisting essentially of a carbon-hydrate or carbon-hydrate
material such as those herein mentioned which are nitrated, sulphurized and
impregnated with oxygen-yielding mediums, substantially as set forth.
Dated the 5th day of March 1901
G. F. REDFERN & Co.,
4, South Street, Finsbury, London, Agents for the Applicant.