Improvements in the Manufacture of Explosives.
Year: 1888

page_text: Date of Application, 31st Jan., 1888
Complete Specification Left, 24th Nov., 1888
Complete Specification Accepted, 15th Jan., 1889
Improvements in the Manufacture of Explosives.
I, ALFRED VINCENT NEWTON, of the Office for Patents, 6 Bream's Buildings,
Chancery Lane, in the County of Middlesex, Mechanical Draughtsman, do hereby
declare the nature of this invention to be as follows:-
The substance known as "Celluloid" mostly contains about two thirds of its weight
of Nitrated cotton, the explosiveness of which is well known, but owing to the combined
camphor, and the compact nature of the substance, the combustion of "Celluloid," even
granulated, is too slow to render it fit for propelling projectiles. Experiments have,
however, proved that by replacing-partly or wholly the aforesaid Camphor by Nitro-
glycerine, a kind of Celluloid is obtained which has sufficient consistency to be formed
into grains, and burns, when used in fire-arms, with the tempered velocity needed to
act as a substitute for gunpowder, over which it has the advantage of possessing
greater power, of leaving no residuum, and of being smokeless or almost smokėless.
In carrying out the invention, 150 parts by weight of Nitrated cellulose of the well-
known soluble kind, are mixed between rollers, or by aid of any other practical mixing
contrivance with 100 parts of Nitro-glycerine, wherein 10 to 12 parts of Camphor have
been previously dissolved. The dissolving action of the liquid on the soluble Nitro-
cellulose, takes place even at the ordinary temperature, but it is much quickened and
facilitated by operating at a higher temperature, not exceeding however 100°
Centigrade.
The dissolving action of the liquid is also facilitated by increasing so far its bulk,
that the Nitrated cellulose which is to be dissolved can be soaked in the liquid. For
such purpose, there is added to the Nitro-glycerine and Camphor, another liquid soluble
therein, and so volatile that it can be easily evaporated, even at the ordinary
temperature.

page_text: A liquid suitable for such purpose is Benzol, of which may be added about the weight
of the Nitrated cellulose, or generally as much, as is needed to secure the immersion of
the said Nitrated cellulose. When the added Benzol has been evaporated, or nearly so,
the mixing between rollers is carried on, until the material obtained, offers sufficient
consistency, and shows uniformity of composition. The operation very much resembles
that of making Celluloid, with this exception, that much less malaxation is needed,
since the explosive material is less hard, and since the solution of the Nitrated cellulose
therein contained, need not be so perfect as to render the material transparent.
When the aforesaid material is ready, it is rolled or pressed out into sheets or ribbons
which are easily cut up into grains by suitable machinery. The quickness of the com-
bustion in fire-arms is, as in the case of gunpowder, dependent on the size of the
grains.
The less of insoluble nitro-cellulose there is mixed up with or contained in the nitro-
cellulose used for the aforesaid purpose, and the more the dissolving power of the liquid
aforesaid is facilitated by prolonged malaxation at a raised temperature, the more
sluggish will be the combustion of the explosive material obtained.
The cellulose generally preferred for nitration is the fibre of cotton; if other fibres
are used, the quantity of the aforesaid liquid, the degree of malaxation, and the tem-
perature at which it takes place, are to be regulated by the degree of solubility of such
nitro-cellulose, and by the degree of consistency of the explosive material which suits
the object in view.
Instead of camphor, which is added to the nitro glycerine for the purpose of facili-
tating the solution of the nitrated cellulose, other excellent solvents of nitro-cellulose
equally soluble in nitro-glycerine, may be substituted for the camphor, such as acetone,
acétate of amyle, ethyle, or methyle, nitrate of ethyle or methyle, nitro benzol ; but
camphor is excellent for the purpose described.
The proportions heretofore named of nitro-cellulose, nitro glycerine and camphor,
are by no means absolute, and may be varied. Thus, for instance, the quantity of
nitro glycerine may be double that of the nitro-cellulose to be dissolved, and yet the
explosive obtained has rather more consistency than ordinary india rubber, and can be
easily cut up into grains, which keep well. On the other hand; the relative quantity
of nitro-cellulose cannot be very much increased beyond the figures above given,
without rendering the solution difficult, and impairing the homogeneity of the material.
The explosive material herein described, especially if the proportion of nitro
glycerine is predominant, can readily be mixed with or kneaded together with solid
powdered nitrates, chlorates, or explosives, such as nitrate of ammonia, nitrate of
potash, or soda, chlorate of potash, picrates, or gunpowder, which substances may be
used either with a view to economy, or for the purpose of quickening or retarding the
explosive combustion. Thus, nitrate of ammonia will tend to retard, and chlorate of
potash to quicken the explosion. In any case, the proportion of the substance to be
added is limited by the cohesiveness of the mass into which it is to be incorporated.
The nitro-cellulose can be partly replaced by nitrated starch, or nitro dextrine, which
are easily soluble in nitro glycerine, but there should be left from 10 to 20 % of
nitrated cotton, in order to give the material, which otherwise is rather too brittle,
sufficient consistency. The proportions should be so regulated that the material can
be broken up into fragments, and thus grained without becoming too brittle, even at
a low temperature.

page_text: Improvements in the Manufacture of Explosives.
1 ALFRED VINCENT NEWTON, of the Office for Patents, 6 Breams Buildings
Chancery Lane in the County of Middlesex, Mechanical Draughtsman, 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:-
The object of this invention is to combine the substances, nitro-glycerine and nitrated
cellulose, with or without nitro-starch or nitro-dextrine, or both, so as to produce an
explosive substance of a horny or semi-horny character, and capable of being reduced
to grains suitable for use as a propeller of projectiles.
My communicant, in disclosing the nature of his invention, and the manner of
carrying it out into practice, makes the following statement :-
It is well known that the substance termed "celluloid" generally contains about two
thirds of its weight of nitrated cellulose, and that it is placed among the explosives.
Owing, however, to the influence of the unexplosive camphor which it contains, and
the compact, unporous nature of celluloid, its combustion, even in a granulated state,
is too slow to render it well fitted for propelling projectiles. But by replacing almost
wholly the aforesaid camphor by nitro-glycerine, a substance somewhat resembling
celluloid in appearance is obtained, which is easily formed into grains or pellets of any
shape, and which burns, when used for fire-arms, with the tempered velocity needed to
render it a fit substitute for gunpowder, over which it has the advantages of possessing
greater power, of leaving almost no residuum, and of being smokeless or almost
sinokeless.
The incorporation of soluble nitrated cellulose with nitro-glycerine in such propor-
tions as to obtain a substance sufficiently hard and consistent to be moulded or granu-
lated, as requisite for the propelling of projectiles, can be accomplished in various
ways, which I now proceed to describe.
The limit of variation, as regards the relative proportions of the two ingredients
above named, viz. :-nitro-glycerine and soluble nitrated cellulose, which permits of
obtaining a compound consistent enough to be granulated, is very wide. But when
the proportion of nitro-glycerine exceeds two thirds of the compound, it is rather too
soft, and when, on the contrary, nitrated cellulose is in excess of two thirds, it becomes
too tough and hard to be easily granulated.
In order to facilitate the dissolving action of nitro-glycerine on soluble nitrated
cellulose, I add a suitable quantity of camphor or other solvent having the same
tendency, to facilitate the combination of the aforesaid ingredients. Such other solvents
are the acetates of methyl, ethyl, and amyl, acetone, nitrate of ethyl, acetic acid and
nitro benzol ; but the above named camphor is very suitable added in proportions of
say from 10 to 30 per cent. of the weight of the nitro-glycerine, more or less, according
as the proportion of said explosive liquid is lessened or increased, it being understood
that the greater the proportion of nitrated cellulose employed, the more camphor is
needed to facilitate the dissolving action of the nitro-glycerine.

page_text: When, in the compound above named, nitro-glycerine is predominant, it can, by the
aid of camphor as aforesaid, be incorporated with the requisite quantity of soluble
nitrated cellulose by malaxation between rollers, heated to a temperature not exceeding
100° centigrade, but which may be much lower, only the operation is then prolonged,
and a sufficiently homogeneous substance is thus obtained, which can be moulded into
sheets between rollers, and is easily cut up into grains with a knife or scissors, or any
simple machinery for quickening the operation.
The incorporation of the aforesaid nitrated cellulose with the nitroglycerine is facili-
tated by adding to the aforesaid solution of camphor in nitroglycerine, a volatile liquid
miscible in the latter, and in such quantity as will permit of the complete immersion
of the nitrated cellulose. A very suitable liquid for such purpose is benzol, of which I
add from once to twice the weight of the nitro-glycerine and nitrated cellulose com-
bined. After evaporation of the aforesaid benzol, the residue is mixed between steam
heated rollers, until the material thus obtained possesses the desired consistency, and is
of a uniform composition. It is then rolled out into sheets, and cut up into suitable
tablets or grains, or other desired forms.
The mode of operating herein described is less suitable when the proportion of
nitrated cellulose is predominant over that of nitroglycerine, inasmuch as the incorpora-
tion of the former requires more protracted manipulation, and that at a higher tempera-
ture. In such case it is convenient to increase largely the proportion of the aforesaid
facilitating solvents, taking care that they should be sufficiently volatile for evaporating
what is not intended to form part of the compound. For such purpose I add to the
nitroglycerine and camphor aforesaid, from one to six times their own weight of
an acetic ether or acetone, regulating the proportion so as to obtain a facile solution of
the nitrated cotton which I desire to incorporate. The soft or viscuous matter thus
obtained is then spread out in thin layers on plates to facilitate the evaporation of the
solvent. This is preferably effected in a closed space, with or without heat, or vacuum,
to suit the more or less volatile nature of the aforesaid solvent, for the purpose of
recovering the same.
After evaporation of the aforementioned solvent, a material remains which, on being
passed through rollers heated to say 50° centigrade, assumes a horny aspect when
cooled, but can, when heated, readily be rolled into sheets, and cut up into grains, or
be moulded into any desired shape.
In order still more fully to illustrate the modes of operating herein described, I now
proceed to name the component parts of two compounds representing about the extremè
proportions of the ingredients which may be used to secure the desired result.
In 100 parts (by parts I here and hereafter mean parts by weight) of nitro-glycerine,
I dissolve 10 parts of camphor, and add thereto 200 parts of benzol. 1 then steep
therein 50 parts of good dry soluble and pulped nitrated cotton, taking care to saturate
the same uniformly with the liquid. I next evaporate the benzol, as above explained,
and then proceed to mix the material between rollers, which I steam-heat to, say, 50
or 60° centigrade, with a view to quicken the operation. As soon as careful malaxa-
tion has reduced the material to a uniform and homogeneous state, it is rolled out into
sheets and cut up into grains, or moulded into any suitable shape, after which it is
ready for use as an explosive, which, as regards manipulation and firing, does not differ
from gunpowder.
Or, when it is desired to reduce the above proportion of nitro-glycerine to a
practical minimum, I take 100 parts of nitro-glycerine, 10 to 25 parts of camphor,
200 to 400 parts of acetate of ainyl, and steep, in the liquid thus obtained, 200 parts
of dry soluble, pulped nitrated cotton. I then mix and knead carefully until the
nitrated cellulose has become well dissolved. The soft material thus obtained, I spread
- out in thin layers, and. let.the volatile. solvent. (in the case here cited acetate of amyl),
evaporate in the open air, or in a heated room or chamber, in which latter case the
greater part of the solvent can be recovered as heretofore indicated. After complete
evaporation of the volatile solvent, the material thus obtained is rolled into sheets
between heated rollers, and cut up into suitable grains, or is moulded, as the case
may require.

page_text: The above described modes possess the disadvantage of prolonged malaxation
between rollers, which, for the purpose of quickening the operation, require to be
heated by steam or otherwise, and they also entail some waste of the solvents. These
drawbacks are, however, avoided by substituting in the compounds aforesaid, for the
major part of the soluble nitrated cotton, a nitro-cellulose of such nature as to be more
easily soluble, such as nitrated starch or nitro-dextrine, singly or mixed, or their
equivalent, such as nitrated fibre of corozzo, commonly called vegetable ivory, or
nitrated pulped wood fibre deprived of its resin. Since, however, a solid compound
consisting only of nitro-glycerine and nitro-starch or nitro-dextrine is too brittle, at
low temperature, for a granulated substance, and must needs have greater consistency,
such portion of nitrated soluble cotton must be left as is requisite to secure such
consistency and temper the brittleness of the grains.
An excellent explosive is thus obtained by dissolving 20 to 30 parts of nitrated
soluble pulped cotton in 100 parts of nitro-glycerine, and 20 parts of camphor,
adding then 100 parts of nitro-starch, containing about 12 to 12 per cent. of nitrogen,
and 200 parts of nitro-dextrine of the same tenour of nitrogen. The material is
easily formed by simply kneading it together at a temperature of, say, 60° centigrade, or
better still, by malaxation between rollers, regulating the temperature so as not to have
it too sticky.
It is, after having become homogeneous, rolled out into sheets and cut up into
grains, or moulded, as desired. By increasing the above proportion of nitrated
cotton, the consistency of the sheets or grains obtained can be proportionately
increased.
The mode of using and applying the explosive compound herein described, differs
from that of gunpowder only in so far as the charge in firearms must be regulated in
accordance with the relative powers of the explosives.
In carying out the manufacture, the nitro-glycerine and nitrated cellulose, as well
as the nitro-starch or nitro-dextrine aforesaid, must be carefully freed from adhering
acids by means of well-known processes now in use in dynamite and nitro-cellulose
factories.
From the foregoing description, it will be seen that my improved explosives, except
when nitro-dextrine or nitro-starch form part of their composition, contain mainly the
same ingredients as the substance for which Letters Patent were obtained on my
behalf, dated December 2nd 1875, No. 4179, and known as "blasting gelatine," but
differ widely from that substance in the proportions of the component parts, their
physical conditions, and their explosive character, for while blasting gelatine is a
purely detonative explosive, the substances herein described possess a comparatively
slow propelling action, and consequently belong to a different class of explosivo
agents.
Powdered nitrate such as one of the nitrates of Ammonia, Potash, Soda or Barium,
separately or collectively, or chlorates, especially that of l'otash, or perchlorates,-
especially those of Potash or Ammonia; or powdered explosives, such as picrates, are
easily incorporated by malaxation with any of the aforesaid explosive compounds, at
a temperature of, say, 60° Centigrade, when they become soft and plastic. The
quantity of such powdered salts to be added is limited by the capability of easy
practical incorporation with the aforesaid explosives and the amount of combustible
element contained therein, which forms the chemico-equivalent for complete utilization
of the oxygen contained in the aforesaid oxydising salts.
By chemico-equivalent quantities, I mean such proportions of carbon, hydrogen,
and oxygen available for explosive combustion, as will ensure the conversion of all
the hydrogen into water vapour, and all the carbon into carbonic oxide or carbonic
acid, which latter represents the final product of completest combustion. Thus, for
instance, an explosive compound very suitable for propelling projectiles, consisting of
100 parts of nitro-glycerine, 15 parts of camphor, and 100 parts of soluble nitro-cellulose,
contains almost exactly the oxygen needed for converting all the hydrogen contained
therein into water vapour, and all its carbon into carbonic oxide. But in order to
obtain complete combustion, converting said carbonic oxide into carbonic acid, it would

page_text: be necessary to incorporate with each 100 parts of the aforesaid compound, 821 parts
of nitrate or chlorate of potash, or 69% parts of nitrate of soda, or 106 parts of
nitrate of baryta, or 163 parts of nitrate of ammonia, or 96 parts of perchlorate of
ammonia.
Of course, if the quantity of oxydising nitrate or chlorate is reduced below the
aforesaid proportions, the explosive combustion will be proportionately incomplete.
Bearing in mind that 1 part of hydrogen requires, for its combustion, 8 parts of
available oxygen, and that each 6 parts of carbon require, for transformation into
carbonic oxide, 8 parts, and for forming carbouic acid, 16 parts of available oxygen,
it is easy, by the aid of chemical formulas, to calculate the proportions of oxydising
nitrates or chlorates suitable for each particular case.
As, however, the addition of the aforesaid nitrates or chlorates, with the exception
of nitrate and perchlorate of ammonia, is productive of smoke through combustion,
which smoke, for propelling powders, is objectionable, the incorporation of such
substances is only resorted to either with the object of reducing the cost price of the
aforesaid compounds, or for the purpose of quickening their explosive combustion
and enhancing their inflammability. This is not needed when the explosive compounds
herein described are to be applied for propelling bullets or projectiles from rifled guns,
but when they are to be used as substitutes for sporting powder, the confinement of
the charge is less perfect, and it is then of advantage to incorporate a small proportion
of a chlorate or nitrate, say, 10 per cent. of chlorate of potash or 30 per cent. of
nitrate of potash (more or less, as the conditions of confinement may vary), for by
this means, the ignition of the charge is facilitated, and the occurrence of "hang-fire
is effectually prevented.
"
Having now particularly described and ascertained the nature of the said
Invention, and in what manner the same is to be performed, as communicated to
ime by my Foreign Correspondent, I declare that what I claim is
-
1. The manufacturo from nitro-glycerine and soluble nitro-cellulose, of a horny or
semi-horny explosive compound, susceptible of granulation, substantially as and for
the purposes herein described.
2. In the manufacture of a compound having the explosive character above indicated,
the use of nitrated starch and nitro-dextrine (either or both), or their equivalent, in
partial substitution for the nitro-cellulose employed, as and for the purpose, above
described.
3. The combination of powdered nitrates, chlorates, or picrates, as above set forth,
with the new explosive compounds above described, composed of nitro-glycerine and
nitro-cellulose, with or without the addition of nitro-starch or nitro-dextrine.
Dated this 98th day of December 1888
NEWTON & SON,
Agents for the Applicant.