Improvements in or relating to the Manufacture of Explosives and Explosive Substances.
Year: 1897

page_text: PROVISIONAL SPECIFICATION.
Improvements in or relating to the Manufacture of Explosives
and Explosive Substances.
I, ERNEST AUGUSTE GEORGE STREET, of 95, Boulevard Beaumarchais, Paris, in
the Republic of France, Engineer, do hereby declare the nature of this invention
to be as follows:-
Being aware of the serious drawbacks met with in the manufacture, handling
and use of chlorate powders hitherto known in connection with explosives, I have
endeavoured to discover a method of obtaining stable explosives containing
chlorates, so that the ingredients, whatever be their sensitiveness to shock and
temperature, may be thoroughly mixed without danger.
The present invention relates to such explosives and to the process of their
manufacture.
Chlorate powders, like all explosives, must consist of substances providing for
combustion of the chlorates description-and of combustible substances, the
proportions being such that when explosion occurs a complete combustion takes
place (carbonic acid or carbonic oxide).
•
It is necessary moreover that the elements or ingredients constituting the
explosive should be thoroughly combined with each other.
Finally, it is necessary to render the substances to be combined harmless under
shocks and high temperatures, which may occur during the manufacture and
handling of these explosives.
I have found that in order to fulfil all these conditions, it is necessary to render
the combustible agent liquid, during the whole process of manufacture.
For this purpose I utilize the properties of certain oils to dissolve, when heated,
nitro- and azo-compounds, which I choose in preference to all other combustible
substances.
If the solubility of the nitro- or azo-compounds in these oils be small, I use other
substances which are more soluble and are formed by the combination of two
nitro-compounds or of two azo-compounds or of one nitro- and one azo-compound.
I use preferably the exact quantity of oil required to dissolve the combustible
substance chosen--the oil itself plays the part of a combustible-but this quantity
of oil must be sufficient to preserve the fluidity of the combustible mixture during
the whole process of manufacture, and this must be done in spite of the fact that
the substance will have to be suitably heated. The oily combustible mixture
surrounds each grain of chlorate the element providing for combustion-with a
shell or coating of solid or paste-like combustible, so that when, after kneading,
the mixture is cooled, there are formed crystals of nitro- or azo-compounds round
the grains of chlorate. The existence of such shell is proved by the fact that in my
explosives having for basis, say chlorate of soda, this salt, usually hygrometric,
is not influenced by atmospheric moisture.
It must also be pointed out that the oil cannot exude.
The mixture is prepared at a very high temperature, so that when it is cooled

page_text: and falls to the highest temperature occurring in summer, the crystallization, or
the paste-like state is formed. The explosive obtained in this manner is so stable
that it may be heated to 150 to 200° C., without its nature being in the least altered,
and at the same time its effect, when exploded, is very powerful, owing to the
combustible substances employed.
These advantages disappear if chlorate and the nitro- or azo-compound
combustible are simply mixed together and the mixture moistened by oil and not
dissolved in it, as has been done with cold picric acid.
It is found that oil exudes when the temperature rises, besides it will be easily
seen that, by the simple mixing, an explosive of less density is obtained than when
the material is dissolved in the oil.
Before describing the details of manufacture of these chlorates, it is necessary
to give some details about the substances I have selected as combustible agents in
my explosives.
The
ethers
NITRO-COMPOUNDS.
nitro-compounds-which must not be confused with nitrated
such as nitro-glycerine and nitrocellulose-are divided into
nitrated carbides (mononitrobenzene, mononitronaphtaline, dinitro-naphtaline,
trinitro-naphtaline, binitro-benzene etc.), nitrated phenols (trinitrophenols, picric
acid, tetra-nitro-diphenols etc.), and nitrated amines (nitro-aniline, nitrated
diphenylamine etc.). They are insoluble, or very slightly soluble, in cold and hot
mineral oils, they are little soluble in cold animal or vegetable oils, but are, on the
contrary, soluble in different proportions in the latter category of oils, if heated to
a suitable temperature.
The following examples may be given.
Crude mono-nitro-naphtaline melts at about 52°; if purified and sublimated,
its fusion point is 61°. At the ordinary temperature, from 15 to 20°, castor-oil
dissolves about 25% of mono-nitro-naphtaline, that is to say 100 parts by weight
of oil dissolve 25 parts of mononitro-naphtaline. From 65° upwards this compound
can be added in any proportion. The solubility in olive and linseed-oil is
practically the same as in castor-oil. A solution of equal parts of oil and a mono-
nitro-naphtaline solidifies when cooled.
the
Crude binitro-naphtalines, which are mixtures of binitro-naphtalines, a and ẞ,
the respective melting points being 240° and 170°, are but slightly soluble in
castor-oil. At the ordinary temperature scarcely 1% dissolves; at 100°
solubility increases and reaches about 4-5%; at 125°, the solubility becomes
about 60% whilst at the melting temperature of the nitro-compounds,
about 170 180°, the two liquids may be mixed in any proportions. The solution
solidifies when cooled.
Crude binitro-benzene melts at about 70°, and when pure at 90°. At the
ordinary temperature its solubility in castor-oil is about 4%; in olive oil
about 3%; in linseed oil about 5%. At 90°-the temperature at which binitro-
benzene is completely liquefied-20 gr. of castor oil and 20 gr. of binitro-benzene
mix perfectly, and give a clear liquid which solidifies when cooled.
Picric acid or trinitrophenol liquefies at 125°. At the ordinary temperature
linseed oil dissolves about 5% of picric acid, castor-oil about 4% and olive-oil
about 1%. At 100° castor-oil dissolves about 20% of picric acid and at about
125° 130° the temperature of fusion of picric acid-castor-oil does not dissolve
more than 50% of picric acid. If a greater quantity is added, the picric acid forms
a brown liquid layer, under the oily solution of picric acid.
Azo-COMPOUNDS.
I have found besides that azo-compounds (azo-benzol, azoxiben-
zene, amidoazobenzol, diamidoazobenzol etc.) have the same properties as
nitro-compounds; they are much more soluble in animal and vegetable oils when
heated than when cold, and mostly insoluble or but little soluble in mineral oils,

page_text: even when heated. Azobenzol and oxyazobenzol are however soluble in paraffine
and vaseline when heated. Amido-azobenzol and diamidoazobenzol are less
soluble.
COMBINATIONS OF NITRO- AND AZO-COMPOUNDS BETWEEN THEMSELVES.
.
By studying nitro- and azo-compounds, it will be found that some
of these substances are relatively little soluble in oil heated even to a high
temperature. For instance picric acid as I have said, at 125°-130° does not
dissolve in castor-oil to a greater extent than 50%. These high temperatures
cannot be used on a large scale in the manufacture of powders, as they would, in
certain special cases, be extremely dangerous. Besides, even by heating under
such conditions, it will be found impossible, for instance in the case of picric acid,
to dissolve in the oil a sufficient quantity of it.
To obviate these drawbacks, I was led to study a whole class of substances
produced by the combination of nitro- or azo-compounds between themselves, two
and two, in order to use them instead of nitro- or azo-compounds, which are little
soluble in the oils when heated. These combinations melt and become dissolved
in oils at temperatures which are much lower than that at which their components
dissolve. The incorporation of such combination substances in oil can therefore
be made without danger. It should be added that by using these binary
combinations, much more powerful explosives are obtained than when their
components, the single nitro- or azo-compounds are employed.
These binary compounds may be prepared by the method generally used in
chemistry, by combining the components molecule to molecule and in the state of
fusion.
At first the substance is melted whose temperature of fusion is the lowest, and
then the second substance is introduced into the liquid mass. By combining a
substance comparatively speaking very fusible, such for instance as mono-nitro-
naphtaline, and a substance difficult to liquefy, such for instance as picric acid,
a combination is produced the melting point and the point of solution of which are
much lower than those of picric acid.
In case that the nitro-compound is too unstable to be melted, the nitro-compounds
are dissolved one after another, beginning with the most soluble. The combination
takes place directly in the oil. All the solutions of nitro-compounds in oil can be,
besides, obtained in this manner; thus considerable quantities of combustible
substances are incorporated in oil.
Thus in one kilogramme of oil only 500 gr. of picric acid can be dissolved
at 125°, whereas if 345 gr. of mono-nitro naphtaline have been previously dissolved
in this kilogramme of oil, it will be afterwards possible to dissolve, at a temperature.
of 100°, 455 grammes of picric acid, and at 125°, 640 grammes of mono nitro
naphtaline and 860 grammes of picric acid. We will however examine hereinafter
in detail certain of these combinations as regards their melting and their solubility
in oils.
It is also easy to produce these combinations of nitro- or azo-compounds by
dissolving the component substances in any solvent: ether, alcohol, acetone,
chloroform, benzene etc. the solvent being got rid of by evaporation leaving the
combination, which can then be dissolved in oil.
The following are some details as to the manufacture and melting points and
solubility of these binary combinations, which in my opinion are destined to play
the chief part in the manufacture of chlorated explosives.
As an example, in order to obtain picro-nitro-naphthaline, one kilogramme of
mono-nitro-naphthaline is introduced into a vessel heated, by a water-bath or by
steam, to 90 or 100°, then after it has melted, 1 kg. 320 of picric acid is added,
little by little. When the solution is complete, the whole is cast in plates; the
combination is ready for use and melts at 74°.
Without heat, castor oil dissolves about 5% of this nitro-combination. At 100°
the solubility considerably increases, and castor-oil can dissolve 80% of picro-nitro-

page_text: naphthaline, which crystallises, when the solution is cooled and solidified. Being
heated to about 105-1100, 20 grammes of castor-oil can dissolve 20, 25 and even 30
grammes of picro nitro-naphthaline, these two substances become capable of being
mixed with each other. Other oils behave very much like castor-oil; linseed oil is
slightly attacked when hot.
Picro-binitro-benzene is prepared similiarly to picro-nitro-naphthaline,-one
kilogr. of binitro-benzene and 1 k. 360 of picric acid are taken, the combination
melting at 88°..
Castor-oil dissolves when cold 6 to 7% of the combination. At 100° the
solubility increases, the oil can dissolve 50% of the nitro-combination; by raising
the temperature beyond 100°, it will become possible to mix 20 gr. of castor-oil
and 20 gr. of picro-nitro benzene.
Picrates of amidoazobenzol, azobenzid, azoxybenzid, nitrodiphenylamines have
practically the same solubility in oil, as the azo-compounds used for their
preparation, picrate of diamidoazobenzol is however less soluble than diamidoazo-
benzol only.
These picroazo-compounds are prepared by dissolving, at first, the azo-compounds
in oil at the temperature of 80 to 100°, and then adding picric acid in small
portions. These solutions once prepared may be heated to a point much higher
than that at which the azo-compounds decompose when heated alone. I have
heated these solutions to 200° without observing spontaneous decomposition or
explosion.
Picramic acid can generally be substituted for picric acid.
NEW PROCESSES OF MANUFACTURING OF CHLORATE POWDER.
In order to manufacture this kind of explosive, the nitro- or azo-compound is
dissolved in the most suitable oil, heating it, if necessary to the melting point of
the nitro-compound, as long as there is no danger of decomposition of the nitro-
compound, or of explosion, during this increase of temperature.
The nitro-compound, or the azo-compound, must dissolve in such proportions
that when cooled down to the highest summer-temperatures it should crystallise,
bringing about solidification of the oily mass, or remain very pastelike in order to
prevent exudation.
If it were found that dissolving, under such circumstances, is impossible, or if
in order to bring it about, it were necessary to raise the temperature to the point
of decomposition of the nitro- or azo-compounds, then recourse may be had to a
previous preparation, by the methods indicated above, of the combination the most
soluble in oil of this nitro- or, azo-compound with another nitro or azo-compound,
then having obtained this binary compound, it would be dissolved in oil, as was the
case for very soluble nitro-compounds.
The oily solution having been prepared, it is poured out into a stirring or mixing
apparatus heated to a suitable temperature, say about 100°, in order to maintain
perfect fluidity during the whole stirring operation. Then starch, or carbon is
added and stirred till it is thoroughly absorbed or mixed with the oily solution.
Then finely pulverised alcaline chlorate or perchlorate is added little by little
the mass being constantly stirred.
The complete kneading or mixing operation, which is very short when a liquid
combustible is used, must continue till the mixture is very complete.
Then it remains only to fill the cartridges or to put up the material in the
manner desired.
Generally speaking it is found that a good explosive should contain about
10-20% of oily solution obtained as hereinbefore described.
80-65% of chlorate of an alcali
10-15% of fecula, starch or carbon
•

page_text: The latter substances may be dispensed with but in such case the explosiv
should preferably be composed as follows
20 to 30% of oily solution
80 to 70% of chlorate of an alcali.
The following are some examples which have been found to give good results:
Chlorate of potash
Oily solution of nitro naphthaline
Starch
-
-
3 kg.
400..gr.
(in equal parts)
600 gr.
800 gr.
200 gr.
Chlorate of soda
Oil solution of picro-nitro-naphthaline
(in equal parts)
750 gr.
Chlorate of soda
200 gr.
Oil solution of picro-nitro-naphthaline
-
(equal parts)
50 gr.
-
Starch
Chlorate of soda
300 gr:
70 gr.
30 gr.
400 gr.
60 gr.
Azobenzol
Castor-oil
Chlorate of potash
Picro-azo benzol
Castor oil
To the latter two mixtures may be added 20 to 40 gr. of starch.
140 gr.
2
Although perfect fluidity of the combustible nitro- or azo-compound is necessar
luring the whole operation (consequent to the previous solution) in order to obtai
good explosives, I also reserve to myself the right to manufacture detonating
mixtures by using either nitro- or azo-compounds or binary combinations forme
y nitro- and by azo-compounds, previously wetted, when hot, by animal, vegetabl
or mineral oil and afterwards mixed with an alcaline chlorate, with or withou
ydrocarbons.
As simply wetting is employed in this case, mineral oil may be used withou
inconvenience, as it is not intended to dissolve the combustible substance.
Dated this 3rd day of June 1897.
To the latter two mixtures may be added 20 to 40 gr. of starch.
Although perfect fluidity of the combustible nitro- or azo-compound is necessar
luring the whole operation (consequent to the previous solution) in order to obtai
good explosives, I also reserve to myself the right to manufacture detonating
mixtures by using either nitro- or azo-compounds or binary combinations formed
y nitro- and by azo-compounds, previously wetted, when hot, by animal, vegetable
or mineral oil and afterwards mixed with an alcaline chlorate, with or without
aydrocarbons.
As simply wetting is employed in this case, mineral oil may be used without
inconvenience, as it is not intended to dissolve the combustible substance.
Dated this 3rd day of June 1897.
BOULT & WADE.
Agents for the Applicant.
Improvements in or relating to the Manufacture of Explosives
and Explosive Substances.
I, ERNEST AUGUSTE GEORGE STREET, of 95, Boulevard Beaumarchais, Paris, in
the Republic of France, Engineer, 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:
Being aware of the serious drawbacks met with in the manufacture, handling
and use of chlorate powders hitherto known in connection with explosives, I have
endeavoured to discover a method of obtaining stable explosives containing
chlorates, so that the ingredients, whatever be their sensitiveness to shock and
temperature, may be thoroughly mixed, without danger.
The present invention relates to such explosives, and to the process of their
manufacture.
•
Chlorate powders, like all explosives, must consist of substances providing for
combustion of the chlorates description-and of combustible substances, the

page_text: proportions being such that when explosion occurs a complete combustion takes
place (carbonic acid or carbonic oxide).
It is necessary moreover that the elements or ingredients constituting the
explosive should be thoroughly combined or mixed with each other.
Finally, it is necessary to render the substances to be combined harmless under
the shocks and high temperature, which may occur during the manufacture.and
handling of these explosives. -
I have found that in order to fulfil all these conditions, it is necessary to render
the combustible agent liquid during the whole process of manufacture.
For this purpose I utilize the properties of certain oils to dissolve, when heated,
nitro- and azo-compounds which I choose in preference to all other combustible
substances.
If the solubility of the nitro- or azo-compounds in these oils be small, I use other
substances which are more soluble, and are formed by the combination of two
nitro-compounds or of two azo-compounds or of one nitro- and one azo-compound.
I use preferably the exact quantity of oil required to dissolve the combustible
substance chosen the oil itself. plays the part of a combustible-but this quantity
of oil must be sufficient to preserve the fluidity of the combustible mixture during
the whole process of manufacture, and this may be done in spite of the fact that
the substance will have to be suitably heated. The oily combustible mixture
surrounds each grain of chlorate the element providing for combustion-with a
shell or coating of solid or paste-like combustible, so that when, after kneading,
the mixture is cooled, there are formed crystals of nitro- or azo-compounds.round
the grains of chlorate. The existence of such shell is proved by the fact that in my
explosives, having for their bases, say chlorate of soda, this salt, usually hygro-
metric, is not influenced by atmospheric moisture.
It must also be pointed out that the oil cannot exude.
The mixture is prepared at a very high temperature, so that when it is cooled
and falls to the highest temperature occurring in summer, the crystallization, or
the paste-like state is obtained. The explosive, obtained in this manner, is so stable
that it may be heated to 150 to 200° C. without its nature being in the least altered,
and at the same time, its effect when exploded is very powerful, owing to the
combustible substances employed.
These advantages disappear if chlorate and the nitro- or azo-compound
combustibles are simply mixed together, and the mixture moistened by oil, and not
dissolved in it, as has been done with cold picric acid.
It is found, in such case, that oil exudes when the temperature rises, besides it
will be easily seen that by simple mixing, an explosive of less density is obtained,
than when the material is dissolved in the oil.
Before describing the details of manufacture of these chlorates, it is necessary
to give some details about the substances I have selected as combustible agents in
my explosives.
NITRO-COMPOUNDS.
The nitro-compounds which must not be confused with nitrated
ethers such as nitro-glycerine and nitro-cellulose-are divided into
nitrated carbides mononitrobenzine, mononitronaphtaline, dinitro-naphtaline,
trinitro-naphtaline, binitro-benzine etc.), nitrated phenols (trinitrophenols, picric
acid, tetra-nitro-diphenols etc.); and nitrated amines (nitro-aniline, nitrated
diphenylamine etc.). They are insoluble or very slightly soluble in cold and hot
mineral oils, they are little soluble in cold animal or vegetable oils, but are, on the
contrary, soluble in different proportions in the latter category of oils, if heated to
a suitable temperature.
The following examples may be given.
Crude mono-nitro-naphtaline melts at about 52°; if purified and sublimated,
its fusion point is 61°. At the ordinary temperature, from 15° to 20°, castor-oil
dissolves about 25% of mono-nitro-naphtaline, that is to say 100 parts by weight

page_text: of oil dissolve 25 parts of mono-nitro-naphtaline. From 65° upwards this compound
can be added in any proportion. The solubility in olive and linseed-oil is
practically the same as in castor-oil. A solution of equal parts of oil and a mono-
nitro-naphtaline solidifies when cooled.
a and B,
Crude binitro-naphtalines which are mixtures of binitro-naphtalines.
the respective melting points being 240° and 170°, are but slightly soluble in
castor-oil. At the ordinary temperature scarcely 1% dissolves; at 100° the
solubility increases and reaches about 4-5%; at 125°, the solubility becomes
about 60%, whilst at the melting temperature of nitro-compounds, about 1700-180°,
the two liquids may be mixed in any proportions. The solution solidifies when
cooled.
-
Crude binitro-benzine melts at about 70°, and when pure at 90°. At the
ordinary temperature its solubility in castor-oil is about 4%; in olive oil
about 3%; and in linseed oil about 5%. At 90° the temperature at which
binitro-benzine is completely liquefied-20 gr. of castor-oil and 20 gr. of binitro-.
benzine mix perfectly, and give a clear liquid, which solidifies when cooled.
Picric acid, or trinitrophenol, liquefies at 125°. At the ordinary temperature
linseed oil dissolves about 5% of picric acid, castor-oil about 4% and olive oil
about 1%. At 100° castor-oil dissolves about 20% of picric acid, and at about
125-130° the temperature of fusion of picric acid castor oil does not dissolve
more than 50% of picric acid. If a greater quantity is added, the picric acid forms
a brown liquid layer under the oily solution of picric acid.
AZO-COMPOUNDS.
azoxiben-
I have found, besides, that azo-compounds. (azo-benzol,
zene, and amidoazobenzol, diamidoazobenzol etc.) have the same properties
as nitro-compounds; they are much more soluble in animal and vegetable oils
when heated than when cold, and mostly insoluble or but little soluble. in mineral
oils. even when heated. Azo-benzol and oxyazobenzol are however soluble in
paraffine and vaseline when heated. Amido-azobenzol and diamidoazobenzol are
less soluble.
COMBINATIONS OF NITRO- AND AZO-COMPOUNDS BETWEEN THEMSELVES...
By studying nitro- and azo-compounds, it will be found that some
of. these substances are relatively little soluble in oil, heated even to a high
temperature. For instance picric acid as I have said, at 125-130° does not dissolve
in castor oil to a greater extent than 50% "These high temperatures cannot be
used on a large scale in the manufacture of explosive powders, as they would in
certain epecial cases be extremely dangerous. Besides even by heating under such
conditions, it will be found impossible, for instance, in the case of picric acid,
to dissolve a sufficient quantity of it in the oil.
To obviate these drawbacks I was led to study a whole class of substances"
produced by the combination of nitro- or azo-compounds between themselves, two
and two, in order to use them, instead of nitro- or azo-compounds which are little
soluble in the oils when heated. These combinations melt and become dissolved
in oils at temperatures which are much lower than that at which their components
dissolve. The incorporation of such combination substances in oil can therefore'
be made without danger. It should be added that by using these binary
combinations, much more powerful explosions are obtained than when their
components, the single nitro- or azo-compounds are employed.
These binary compounds may be prepared by the method generally used in
chemistry, by combining the components molecule to molecule, and in the state of
fusion.
-
At first the substance is melted whose temperature of fusion is the lowest, and
then the second substance is introduced into the liquid mass. By combining a
substance comparatively speaking very fusible, such for instance as mono-nitro-.
naphtaline, and a substance difficult to liquefy such for instance as picric acid,

page_text: a combination is produced the melting point and the point of solution of which
are much lower than those of picric acid.
. In case that the nitro-compound is to unstable to be melted, the nitro-compounds
are dissolved in oil, one after another, beginning with the most soluble. The
combination takes place directly on the oil. All the solutions of nitro-compounds
in oil can be obtained in this manner; and in this manner considerable quantities
of combustible substances may be incorporated in oil.
Thus in one kilogramme of oil only 500 gr. of picric acid can be dissolved
at 125°, whereas if 345 gr. of mono-nitro naphtaline have been previously dissolved
in this kilogramme of oil, it will be afterwards possible to dissolve at a temperature
of 100°, 455 grammes of picric acid, and at 125°, 640 grammes of mononitro
naphtaline and 860 grammes of picric acid. We will however examine hereinafter,
in detail, certain of these combinations as regards their fusion or melting, and
their solubility in oils.
It is also easy to produce these combinations of nitro- or azo-compounds by
dissolving the component substances in any volatile solvent; ether, alcohol, acetone,
chloroform, benzene etc. the solvent being got rid of by evaporation leaving the
combination which can then be dissolved in oil.
The following are some details as to the manufacture and melting points and
solubility of these binary combinations, which, in my opinion, are destined to play
the chief part in the manufacture of chlorate explosives.
As an example in order to obtain picro-nitro-naphthaline, one kilogramme of
mono-nitro-naphthaline is introduced into a vessel heated by a water-bath, or by
steam, to 900 or 100°, then after it has melted, 1 kilogramme 320 grammes of
picric acid is added little by little. When the solution is complete the whole is
cast in plates, and the combination is ready for use, and melts at 74°.
Without heat castor-oil dissolves about 5% of this nitro-combination, at 100°
the solubility considerably increases, and castor oil can dissolve 80% of picro-
nitro-naphthaline which crystalises, when the solution is cooled and solidified.
Being heated to about 105-110°, 20 grammes of castor-oil can dissolve 20, 23 and
even 30 grammes of picro-nitro-naphtaline, these two substances thus becoming
capable of being mixed with each other. Other oils behave very much like castor-
oil linseed oil being slightly attacked when hot.
:
Picro-binitro-benzene is prepared similarly to picro-nitro-naphthaline-1 kilogr.
of binitro-benzene and 1 kilogramme 360 grammes of picric acid are taken, the
combination melting at 88°.
Castor-oil dissolves when cold 6 to 7% of the combination. At 100 the solubility
increases, the oil can dissolve 50% of the nitro combination; by raising the
temperature beyond 100°, it will become possible to mix 20 grammes of castor oil
and 20 grammes of picro-nitro-benzene.
Picrates of amidoazobenzol, azobenzid, azoxybenzide, nitrodiphenylamines have
practically the same solubility in oil, as the azo-compounds used for their prepara-
tion; picrate of diamidoazobenzol is however less soluble than diamidoazobenzol
only.
These picroazo-compounds are prepared by dissolving first the azo-compounds
in oil at a temperature of 80° to 100°, and then adding picric acid in small portions.
These solutions once prepared may be heated to a point much higher than that at
which the azo-compounds decompose when heated alone. I have heated these
solutions to 200° without observing spontaneous decomposition or explosion.
Picramic acid can generally be substituted for picric acid.
NEW PROCESSES OF MANUFACTURING CHLORATE POWDER.
In order to manufacture this kind of explosive, the nitro- or azo-compound is
dissolved in the most suitable oil, heating it if necessary- to the melting point of
the nitro-compound as long as there is no danger of decomposition of the nitro-
compound or of oplosion during this increase
J

page_text: Although perfect fluidity of the combustible nitro- or azo-compound is necessary
during the whole operation (subsequent to the previous dissolving) in order to
obtain good explosives, I also reserve myself the right to manufacture detonating
mixtures by using either nitro- or azo-compounds or binary combinations formed
by nitro- and by azo-compounds, previously wetted, when hot, with animal, vege-
table mineral oil and afterwards mixed with an alkaline chlorate, with or without
a carbonated or hydrocarbonated substance.

page_text: As simple wetting is employed in this case, mineral oil may be used without
inconvenience, as it is not intended to dissolve the combustible substance.
Having now particularly described and ascertained the nature of this invention
and in what manner the same is to be performed, I declare that what I claim is :-
1. Process of manufacturing chlorated explosives, consisting in dissolving in
a vegetable or animal oil, with heat, a nitro or an azo compound (in such proportion
that when this oil mixture is cooled it crystallises and becomes solid or of pasty
consistency) then mixing this solution with one or more finely pulverised alkaline
chlorates or perchlorates with or without addition of a carbonated or hydrocarbon-
ated substance heat being employed to maintain the fluidity of the oily mixture
during the whole time of mixing, substantially as described.
2. The process of manufacturing chlorated explosives in which nitro or azo
compounds which are little soluble when heated in oils are employed consisting
in combining the little soluble substance (nitro- or azo-compound) with a nitro
compound, or with an azo compound, to form a combination soluble in oil when
heated, and in dissolving this binary conibination, with heat, in a vegetable or
animal oil (in such proportions that when it is cooled the oil mixture becomes by
crystallization solid or of pasty consistency) and in mixing this solution with one
or more finely pulverised alkaline chlorates or perchlorates with or without the
addition of a carbonated or hydrocarbonated substance heat being employed to
maintain the fluidity of the oily mixture during the whole operation of mixing
substantially as described.
3. In the process of manufacturing chlorated explosives the employment of
azo compounds soluble when heated in mineral oil as azo benzol, oxyazobenzol,
substantially as described.
4. The process of manufacturing chlorated explosives consisting in (a) simply
permeating with animal vegetable or mineral oil. when heated, either nitro or azo
compounds or a combination of nitro compounds or of azo-compounds or of one
nitro and one azo compound, (b) mixing the paste thus obtained with one or more
finely pulverised alkaline chlorates with or without addition of a carbonated or
hydrocarbonated substance substantially as described.
5. The explosive substances substantially as described.
6. An explosive, the combustible element of which is constituted by an azo-
compound or a combination of two nitro compounds or of two azo compounds or
of one nitro compound and of one azo compound substantially as described.
· 7. An explosive substance formed of
prepared substantially as described.
9. An explosive substance formed of chlorate of potash 3000 parts, oil solution
of nitronaphthaline (in equal part) 400 parts, starch 600 parts, prepared substan-
tially as described.
10. An explosive substance formed of chlorate of soda 800 parts, oil solution of
picronitronaphthaline (in equal parts) 200 parts, prepared substantially as
described.
11. An explosive substance formed of chlorate of soda 750 parts, oil solution of
picronitronaphthaline (in equal parts) 200 parts, starch 50 parts prepared substan-
tially as described.

page_text: 12. An explosive substance formed of chlorate of soda 300 parts, azobenzol,
70 parts castor oil 30 parts with or without the addition of starch prepared substan-
tially as described.
13. An explosive substance formed of chlorate of potash 400 parts, picroazoben-
zol 60 parts, castor oil 40 parts, with or without the addition of starch prepared
substantially as described.