IMPROVEMENTS IN THE MANUFACTURE OF EXPLOSIVE COMPOUNDS
Year: 1883

page_text: LETTERS PATENT to Friedrich Wilhelm Gilles, of Cöln °/Rh. Germany for
an Invention of "IMPROVEMENTS IN THE MANUFACTURE OF EXPLOSIVE
COMPOUNDS
"
PROVISIONAL SPECIFICATION left by the said Friedrich Wilhelm Gilles at
the Office of the Commissioners of Patents on the 13th April 1883.
FRIEDRICH WILHELM GILLES of Coln °/Rh, Germany,
MANUFACTURE OF EXPLOSIVE COMPOUNDS
"
"IMPROVEMENTS IN THE
This invention relates to the manufacture of explosive materials from Molasses
and residues therefrom.
In the following description the term "Molasses" is intended to include the
residues in the sugar manufacture which are obtained by the concentration and
treatment of the saccharine juices, from which residues the greater portion of the
component parts of the sugar has been removed, but which in other respects (water
not being taken into consideration) actually consist of organic non-saccharine
matters. And by the term "residues from the Molasses," on the other hand I
mean those products which are left behind as residues in the conversion of Molasses
into sugar, which products contain but a slight percentage of sugar, and likewise
(water not being considered) consist of organic non-saccharine matters.
In order to manufacture explosives from the aforesaid residues in the sugar
manufacture, these residues according to the said invention are "nitrated" that is
to say treated with a mixture of nitric and sulphuric acids. This is accomplished
in the manner hereinafter described.
In order to avoid prolixity, I shall hereinafter use only the term "Molasses," it
being understood that all that is described with reference thereto applies also to
the residues from the Molasses in the sense in which they are above defined.
Likewise, for the sake of brevity, all the nitro-compounds obtained from the
Molasses or the residues therefrom will be hereinafter referred to under the collective
designation of " Nitro-Molasses"
When a Nitro-compound is required to be obtained in a stiff compact form, then
the molasses are used without any preparatory treatment,

page_text: furnaces. The pressure occasioned by the introduction of the oxygen may vary
between 0.14 and 3 atmospheres. By withdrawing samples and analyzing the
same, it is easy to ascertain when the operation is at an end.
The molasses thus prepared are "nitrated" in a similar manner to that above
described for the raw molasses. For example I thoroughly mix the following
ingredients in about the proportions named, that is to say :—
380 grammes of Molasses
1000 grammes of concentrated Nitric Acid.
2000 gramines of concentrated Sulphuric Acid. This mixture is placed into cold
water, or water warmed to 25° c; the yellow nitro-molasses which is at once
formed is washed several times in cold water, and then with boiling water, until
all the acid is removed.
The fluid nitro-molasses thus obtained, when heated slowly, boils at between 180°
and 200°, and detonates between 220° and 250°; it can be mixed with any well
known absorbents, for instance fossil-meal
To manufacture blasting material, however, it is more practical to use saw-dust,
tan, or bran, which substances are previously soaked with a solution of nitrates of
the alkalies, preferably with nitrate of potash or sultpetre.
For this purpose for every seventy (70) parts saw-dust, tan, or bran, a con-
centrated solution of about thirty (30) parts of saltpetre in water is prepared ;
the saw-dust, tan, or bran is introduced into this solution which it absorbs, and
the water is allowed to dry up. The product thus obtained is then mixed with
the nitro-molasses in different proportions, varying according to the use to be made
of the blasting material.
The following are examples of the proportions to be used, that is to say :—
For blasting hard rocks, for every 3 parts of nitro-inolasses, 1 part of saw-dust,
tan or bran, soaked in salt petre should be employed. When the rocks to be
blasted are not so hard, the addition of saw-dust, tan or bran may be larger until
the proportion of 1 part of nitro-molasses to 1 part of saw-dust or the like, is
attained. But when the material is to be employed for blasting coals or marble,
or in places where a shattering of the material must be avoided, less nitro-molasses
should be employed, and the proportion to the saw-dust, or the like can be reduced
from 4: 5 to 1:9.
To increase the power of the explosive material as above described, cast iron or
steel filings can be added, whereby the explosive force of the product will be
materially increased. For the same purpose the following substances may be
added either singly or together, namely, chlorates or nitrates of the alkalies, ferro-
cyanide of potassium mixed with potassium chlorate (chlorate of potash), shooting
powder of any kind, mercury, fulminic acid salts, potash, or picrates.
The special manufacture of blasting cartridges with the explosive mass obtained
as above described is carried out according to any of the well known methods.
The use of saw-dust, or the like soaked in salt petre, offers this advantage, that
a very uniform absorption can be ensured, in consequence of which the explosion
takes place more suddenly and more powerfully than with the use of other
absorbents; whilst the danger of an accidental explosion is diminished, because
the above described absorbents more thoroughly cover the nitro-molasses, and
are more elastic than the fossil-meal (which is usually employed) in the compressed
state
By the explosion the absorbents unite for the most part with the gases that are
generated, and cause a more powerful explosion (a cartridge with lifty-five (55)
per cent of nitro-molasses, possesses the same explosive power as a dynamite
cartridge with seventy five (75) per cent of nitro glycerine) whilst the deleterious
gases are absorbed, a fact which is of the greatest importance especially from a
sanitary point of view in all blasting operations carried on in confined spaces,
Moreover blasting operations can be safely undertaken with explosives as herein
described at a temperature of ten degrees below zero (— 10°) without its being

page_text: necessary to warm the cartridges beforehand. Thus, with the cartridges made
with the new explosive material, blasting operations under water can be effected.
And further the manufacture as well as the transport and use of the cartridges
are much less dangerous than is the case with explosive materials heretofore
employed, and a decomposition of the explosive material is not liable to take
place.
By the addition of cast iron and steel filings the following result is obtained,
that is to say, the explosive exerts its force not only in a downward or backward
direction but also in an upward or forward as desired inasmuch as the exertion
of force in the latter direction is entirely dependent upon the proportion in which 1
the metal filings are added.

page_text: a larger proportion of carbon. In all cases the proportion of carbon to oxygen
should be in the ratio of 3 to 2.
The quantities of peroxide of lead and sulphide of carbon or oxygen to be added
are determined by the primary composition of the molasses, and cannot be given
beforehand; they should rather be ascertained through a few trials and analyses of
the molasses to be treated. For example, with raw molasses, which after
evaporation that is to say after the free water has been evaporated contains
22.5 per cent, by weight of carbon
17.5 per cent, by weight of oxygen, and
60 per cent by weight of water in chemical combination and thus shows a
higher proportion of oxygen, it is necessary to add to a kilogramme of molasses
ten (10) grammes of brown per oxide of lead and ten (10) grammes of sulphide of
carbon, in order to obtain the normal composition as above stated.
In this preparation it is preferable to mix the molasses with the peroxide of lead
and sulphide of carbon in open holders or vessels and then allow the mass which
may be either hot or cold to ferment.
The duration of this fermentation, depends upon the temperature maintained.
With a temperature of twenty live (25) degrees centigrade eight (S) to ten (10)
days are sufficient; with a temperature of from eighteen (18) to twenty (20)
degrees centigrade about fourteen (14) days; and below eighteen (18) degrees
centigrade about from eighteen (18) to twenty (20) days. If higher temperatures
are maintained much less time is required; thus with a temperature of from fifty
(50) to seventy (70) degrees centigrade, twenty (20) to twenty four (24) hours
will suffice. Higher temperatures however should not be employed.
During the fermentation, the mass must be stirred every two (2) days, or even
oftener. The process is completed when bubbles cease to form, The mass is then
allowed to stand for a short time after which the Quid matter is drawn off as
required by means of cocks. The remaining solid residue is pressed, and yields,
when washed, sulphuret of lead.
The addition of oxygen, when the proportion of carbon is too large, is performed
by means of closed holders or vessels. These vessels are provided with a
manometer, and with devices for filling and emptying them,
The oxygen is prepared by heating chlorate of potash or manganese-ore or by
decomposing water by means of an electric current, or by any other well known
method.
The oxygen is conducted into the closed vessels charged with molasses. The
said vessels must be far enough from the place where the oxygen is produced to
prevent their being heated by the generators. The pressure occasioned by the
introduction of the oxygen may vary between 0.14 and 3 atmospheres, By
withdrawing samples of the material being treated and analyzing the same, it is
easy to ascertain when the operation is completed
The molasses thus prepared are "nitrated" in a similar manner to that above
described for the raw inolasses. For example I thoroughly mix the following
ingredients in about the proportions named, that is to say ;-
380 grammes of molasses
1000 grammes of concentrated nitric acid
2000 grammes of concentrated sulphuric acid. This mixture is then placed into
cold water or water warmed to twenty five (25) degrees centigrade the yellow
nitro-molasses which is at once formed is washed several times in cold water, and
then with boiling water, until all the acid is removed.
The fluid nitro-molasses thus obtained when heated slowly, boils at between one
hundred and eighty (180) and two hundred (200) degrees centigrade, and
detonates between two hundred and twenty (220) and two hundred and fifty (250)
degrees centigrade. It can be mixed with any well known suitable absorbents, for
instance fossil meal.
To manufacture blasting material however it is more practicable to use saw-dust,

page_text: tan or bran, which substances are previously impregnated with a solution of a
nitrate of the alkalies, preferably with nitrate of potash or saltpetre.
For this purpose for every seventy (70) parts of saw-dust, tan or bran, a
concentrated solution of about thirty (30) parts of saltpetre in water is prepared.
The saw-dust, tan or bran is introduced into this solution, which it absorbs, and
the water is allowed to evaporate. The product thus obtained is mixed with the
nitro molasses in proportions, varying according to the use to be made of the
blasting material.
The following are examples of the proportions which I preferably employ for
various purposes that is to say;-For blasting hard rocks three (3) parts of nitro-
molasses to one (1) part of saw-dust, tan or bran, impregnated with saltpetre.
When the rocks to be blasted are not so hard, the addition of saw-dust, tan or bran
may be larger until the proportion of one (1) part of nitro-molasses to one (1) part
of saw-dust or the like is attained But when the material is to be employed for
blasting coal or marble, or in places where a shattering of the material must be
avoided, less nitro-molasses should be employed and the proportion to the saw-dust
or the like can be reduced from four (4) of the former to five (5) of the latter to
one (1) of the former to nine (9) of the latter.
To increase the power of the explosive material as above described cast iron or
steel filings can be added whereby the explosive force of the product will be
materially increased. For the same purpose the following substances may be
added either singly or together namely chlorates or nitrates of the alkalies,
ferrocyanide of potassium mixed with potassium chlorate (chlorate of potash)
gun-powder of any kind, mercury, fulminates, potash or picrates.
The special manufacture of blasting cartridges with the explosive mass obtained
as abovo described is carried out according to any of the well known methods.
The use of saw-dust or the like impregnated with saltpetre offers this advantage,
that a very uniform absorption can be ensured in consequence of which the
explosion takes place more suddenly and more powerfully than with the use of
other absorbents; whilst the danger of an accidental explosion is diminished
because the above described absorbents more thoroughly cover the nitro-molasses,
and are more elastic than the fossil-meal (which is usually employed) in the
compressed state,
By the explosion the absorbents unite for the most part with the gases that are
generated and cause a powerful explosion, a cartridge with fifty five (55) per cent
of nitro-molasses possessing about the same explosive power as a dynamite
cartridge with seventy five (75) per cent of nitroglycerine whilst the deleterious
gases are absorbed, a fact which is of the greatest importance especially from a
sanitary point of view, in all blasting operations carried on in confined
spaces.
Moreover blasting operations can be safely undertaken with explosives as herein
described at a temperature of twenty five (25) degrees centigrado below zero
without its being necessary to warm the cartridges before hand. Thus, with the
cartridges made with the new explosive material, blasting operations under water
can be effected. And further, the manufacture as well as the transport and use of
the cartridges is much less dangerous than is the case with explosive materials
heretofore employed and a decomposition of the explosive material is not liable to
take place.
By the addition of cast iron and steel filings the explosive exerts its force not
only in a downward or backward direction but also in an upward or forward
direction and that inasmuch as the exertion of force in the latter direction is
entirely dependent upon the proportion in which the metal filings are added.
Having thus fully described my said invention and the manner of performing
the same I wish it understood that I claim.
First. The utilization in the manufacture of explosives of the residues obtained
in the concentration and treatment of saccharino juices and by the conversion of

page_text: molasses into sugar (which residues consist of organic non saccharine matters) by
nitrating" the said residues with nitric and sulphuric acids.
Second The preparatory treatment of the said residues with brown per oxide of
lead and sulphide of carbon or oxygen.
Third Mixing explosives manufactured as herein before described with saw-dust
tan or bran previously impregnated with a solution of a nitrate of the alkalies,
such as nitrate of potash, nitrate of soda or saltpetre or with any other suitable
absorbent.
Fourth. The addition of cast iron or steel filings to the explosives obtained as
herein before described
Fifth. The combination with the explosives obtained as described of any other
explosive materials.
Sixth. The explosives obtained by the methods hereinbefore described and
consisting wholly or in part of the residues in the manufacture of sugar "nitrated”
as set forth in the first claiming clause
In witness whereof I the said Friedrich Wilhelm Gilles have hereunto set my
hand and seal this Ninth day of October in the year of our Lord One thousand
eight hundred and eighty three.