IMPROVEMENTS IN MEANS AND APPARATUS FOR THE MANUFACTURE OF AMMONIA
Year: 1879

page_text: LETTERS PATENT to William Müller, of Antwerp, in the Kingdom of Belgium,
Merchant, and Edmond Geisenberger, of Brussels, also in the Kingdom of
Belgium, Civil Engineer, for the Invention of "IMPROVEMENTS IN MEANS AND
APPARATUS FOR THE MANUFACTURE OF AMMONIA."
Sealed the 25th July 1879, and dated the 16th April 1879.
PROVISIONAL SPECIFICATION left by the said William Müller and Edmond
Geisenberger at the Office of the Commissioners of Patents on the 16th April
1879.
WILLIAM MÜLLER, of Antwerp, in the Kingdom of Belgium, Merchant, and
EDMOND GEISENBERGER, of Brussels, also in the Kingdom of Belgium, Civil
Engineer. "IMPROVEMENTS IN MEANS AND APPARATUS FOR THE MANUFACTURE
OF AMMONIA."
Our Invention relates to a new manufacturing process for the production of
ammonia, which process is based upon the following general principles:-
Firstly. Nitrates and nitrites are reducible by heat; the residue left from their
decomposition is the base which entered into their composition. The oxygen and
the nitrous products are given off as gas. When mixed with an alkaline bydrate,
and added to a body capable of combining with oxygen, such, for example, as carbon,
they may be decomposed by heat, ammonia will be given off, and the residue will
be an alkaline carbonate.
Secondly. Nitrogen or hydrogen obtained from the decomposition of products
containing them, whether separately or together, are evolved therefrom in a nascent
state, whatever be the modes employed for effecting such decomposition.
Thirdly. Nitrogen and hydrogen in presence in a nascent state unite to form
ammonia.
Fourthly. A base may form a nitrate or a nitrite in presence of the oxygenated
compounds of nitrogen under the influence or in the absence of water. The reaction
may be accelerated by heat or electricity.
Fifthly. Nitrogen and hydrogen combine under the influence of electricity. Any
body having affinity for the compound resulting therefrom accelerates the combi-
nation.
This is the case, not only with nitrogen and oxygen put in presence separately,
but also with atmospheric air, which is compound of nitrogen and oxygen, the
proportions of which may be rendered equivalent to obtain this result.

page_text: Our Invention consists in the means and apparatus hereinafter described for
carrying out practically the conditions of the above data, and producing ammonia
and ammoniacal salts or compounds on a manufacturing scale.
In a suitable retort or vessel we charge a quantity of nitrate or nitrite of baryta
or of potash, or any other nitrate or nitrite of similar character. We decompose the
said nitrate or nitrite by the action of heat, and we conduct the gaseous products of
the decomposition so as to bring them in presence of a body or bodies capable of
absorbing oxygen, or of combining with oxygen.
We select for the purpose a body, which not only is capable of combining with
or of absorbing the oxygen of the said gaseous products evolved by the decompo-
sition of the nitrate or nitrite, but which is also capable of combining with or of
absorbing the oxygen of water, thereby setting free the hydrogen of the said water
in a nascent state.
The apparatus which we prefer to use for the purpose consists of a retort mounted
in a suitable furnace, such as is generally used in the manufacture of illuminating
gas.
We charge into the said retort charcoal, coke, or other carbon, which we heat to
a red heat. The said charcoal or other carbon combines with the oxygen of the
gaseous products, and sets free the nitrogen in a nascent state.
We also conduct vapour of water upon the same absorbing or decomposing body,
(which in the present instance consists of charcoal or other carbon heated to a red
heat in a retort). The said charcoal or carbon heated to a red heat combines with
the oxygen of the vapour of water, and hydrogen is evolved in a pascent state, so
that in the same retort or vessel we have in presence nitrogen and hydrogen both
set free in a nascent state, which nitrogen and hydrogen combine and form
ammonia.
Or the gaseous products resulting from the decomposition of the nitrate or nitrite
may also be obtained directly in the form of ammonia in the retort or vessel first
described, by mixing previously with the said nitrate or nitrite an alkaline or other
hydrate, and charcoal or other carbon. By this means the ammonia will be formed
directly, and the residue will be an alkaline or other carbonate, which may be used
again as a base.
We collect the ammonia either in the form of gas or in a liquid state, by com-
pressing it sufficiently, or in the form of ammoniacal salt, or in a watery solution,
or in any form suitable for use.
The nitrate or nitrite contained in the first retort or vessel having been decom-
posed by the action of heat leaves as residue the base which entered into its
composition.
.
From this residual base we reconstitute the nitrate or nitrite as follows:-
In a suitable vessel we place the said residual base (which may be hydrated), and
we conduct upon the said base and under the influence of electricity nitrogen and
oxygen, and in some cases atmospheric air, in the proportion required to constitute
the oxygenated compound of nitrogen capable of forming a nitrate or a nitrite as
required for our process.
The nitrate or nitrite thus obtained is used in our process, as hereinbefore
described.
By this means the same base may be used over again to reconstitute the nitrate
or the nitrite after its decomposition, and it is obvious that the nitrate or the nitrite
first used in our process may be obtained by similar means. Instead of first forming
a nitrate or a nitrite for the production of ammonia, nitric acid may be obtained
directly, and be then decomposed in the same manner as the nitrate or nitrite, for
the purpose of obtaining the gaseous products herein before mentioned; the other
parts oftheoperation are carried on as hereinbefore described.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said William Müller and Edmond Geisenberger in the Great Seal Patent
Office on the 15th October 1879.
WILLIAM MÜLLER, of Antwerp, in the Kingdom of Belgium, Merchant, and
EDMOND GEISENBERGER, of Brussels, also in the Kingdom of Belgium, Civil
Engineer. "IMPROVEMENTS IN MEANS AND APPARATUS FOR THE MANUFACTURE
OF AMMONIA."
Our Invention relates to a new manufacturing process for the production of
ammonia, which process is based upon the following general principles
Firstly. Nitrates and nitrites are reducible by heat; the residue left by their
docomposition is the base which entered into their composition. The oxygen and
the nitrous products are given off as gas. When mixed with an alkaline hydrate,
and added to a body capable of combining with oxygen, such, for example, as carbon,
they may be decomposed by heat, ammonia will be given off, and the residue will
be an alkaline carbonate.
Secondly. Nitrogen or hydrogen obtained from the decomposition of products
containing them, whether separately or together, are evolved therefrom in a nascent
state, whatever be the modes employed for effecting such decomposition.
Thirdly. Nitrogen and hydrogen in presence in a nascent state unite to form
ammonia.
Fourthly. A base may form a nitrate or a nitrite in presence of the oxygenated
compounds of nitrogen under the influence or in the absence of water. The reaction
may be accelerated by heat or electricity.
Fifthly. Nitrogen and hydrogen combine under the influence of electricity; any
body having affinity for the compound resulting therefrom accelerates the combi-
nation.
This is the case not only with nitrogen and oxygen put in presence separately,
but also with atmospheric air, which is a compound of nitrogen and oxygen, the
proportions of which may be rendered equivalent to obtain this result.
Our Invention consists in the means and apparatus herein after described for
carrying out practically the conditions of the above data, and producing ammonia
and ammoniacal salts or compounds on a manufacturing scale.
In ณ suitable retort or vessel we charge a quantity of nitrate of baryta, or of
potash, or any other nitrate or nitrite of similar character. We decompose the
said nitrate or nitrite by the action of heat, and we conduct the gaseous products
of the decomposition so as to bring them in presence of a body or bodies capable
of absorbing oxygen, or of combining with oxygen.
We select for the purpose a body which not only is capable of combining with
or of absorbing the oxygen of the said gaseous products evolved by the decompo-
sition of the nitrate or nitrite, but which is also capable of combining with or of
absorbing the oxygen of water, thereby setting free the hydrogen of the said water
in a nascent state. The apparatus which we prefer to use for the purpose consists
of a retort mounted in a suitable furnace such as is generally used in the manufac-
ture of illuminating gas. We charge into the said retort charcoal, coke, or other
carbon, which we heat to a red heat. The said charcoal or other carbon combines
with the oxygen of the gaseous products, and sets free the nitrogen in a nascent
state. We also conduct vapour of water upon the same absorbing or decomposing
body (which in the present instance consists of charcoal or other carbon heated to
a red heat in a retort). The said charcoal or carbon heated to a red heat combines
with the oxygen of the vapour of water, and hydrogen is evolved in a nascent state,
so that in the same retort or vessel we have in presence nitrogen and hydrogen,
both set free in a nascent state, which nitrogen and hydrogen combine and form
ammonia; or the gaseous products resulting from the decomposition of the nitrate

page_text: or nitrite may also be obtained directly in the form of ammonia in the retort or
vessel first described by mixing previously with the said nitrate or nitrite an
alkaline or other hydrate and charcoal or other carbon. By this means the ammonia
will be formed directly, and the residue will be an alkaline or other carbonate,
which may be used again as a base. We collect the ammonia either in the form of
gas, or in a liquid state by compressing it sufficiently, or in the form of ammoniacal
salt, or in a watery solution, or in any form suitable for use.
The nitrate or nitrite contained in the first retort or vessel having been decom-
posed by the action of heat leaves as residue the base which entered into its
composition. From this residual base we reconstitute the nitrate or nitrite as
follows:-
In a suitable vessel we place the said residual base (which may be hydrated) and
we conduct upon the said base, and under the influence of electricity, nitrogen and
oxygen, and in some cases atmospheric air in the proportion required to constitute
the oxygenated compound of nitrogen capable of forming a nitrate or nitrite as
required for our process.
The nitrate or nitrite thus obtained is used in our process as hereinbefore
described.
By this means the same base may be used over again to reconstitute the nitrate
or the nitrite after its decomposition, and it is obvious that the nitrate or the nitrite
first used in our process may be obtained by similar means.
Instead of first forming a nitrate or a nitrite for the production of ammonia,
nitric acid or a compound of nitrogen, more or less oxygenated, may be obtained
directly, and be then decomposed in the same manner as the vapours produced
from the nitrate or nitrite for the purpose of obtaining the gaseous products herein
before mentioned. The other parts of the operation are carried on as herein before
described.
Having thus explained the nature of our said Invention, we will proceed to
describe, with reference to the accompanying Drawings, the manner in which the
same is to be performed.
Figure 1 represents in longitudinal section an apparatus for the manufacture of
ammonia constructed and arranged according to our Invention. a represents a
retort or vessel made of cast iron or other suitable material mounted in a furnace b
heated from the fire place b'. In the top of the vessel a is an opening a', through
which the said vessel is charged and discharged. The said opening a is closed by
a removeable cover held in position by a stopper a² which closes the opening to the
furnace b. The vessel a is connected by pipes c, c, c, with a retort d containing
wood, charcoal, coke, or other carbon, and mounted in the furnace e. The said
retort d, which may be made of cast iron or other suitable material, is connected by
means of a pipe f with a reservoir 9 made of wood lined with lead or of another
suitable material, in which reservoir g is contained at g¹ sulphuric acid, water, or
any other suitable body capable of absorbing ammonia or combining with ammonia.
The reservoir g is provided with a pipe h, which at its other end opens into the
fire place e' of the furnace e. The vessel a contains nitrate or nitrite of baryta, or
another nitrate or nitrite suitable for our process. The said vessel a having been
heated the nitrate or the nitrite it contains is decomposed, and nitrous vapours are
evolved therefrom and pass through the pipes c, c', c³, into the retort d containing
carbon heated to a red heat.
As the nitrous vapours pass into the retort d vapour of water from a suitable
generator is also caused to enter the said retort through the pipes i and c². The
said nitrous and aqueous vapours are decomposed in the retort d. The oxygen is
fixed by the carbon, forming oxide of carbon, whilst the nitrogen and the hydrogen
evolved in a nascent state unite and form ammonia, which ammonia passes with
the oxide of carbon into the reservoir g, where it is absorbed by or combines with
the sulphuric acid, water, or other body therein, whilst the oxide of carbon passes
through the pipe h to underneath the fire place el of the furnace e, or it may be
collected for use.

page_text: In forming a nitrate or a nitrite for our process, or in reconstituting the nitrate
or the nitrite which has been decomposed in the vessel a by the above described
distilling operation, we prefer to use apparatus of the character represented in
Figure 2, which apparatus consists of a vessel k made of stone or other suitable
material, provided with handles and closed by a cover of the same material k³,
which is fitted tightly upon the vessel k by means of a hydraulic joint at k². The
said cover is provided with tubes 1, 1', through which the pipes m, m³, pass into
the apparatus. Through one of the said pipes atmospheric air is caused to enter
the vessel k, and through the other pipe oxygen; derived from any suitable source,
is conducted into the said vessel. n, n, are two tubes, through which two electric
wires o, o¹, in connection with a suitable source of electricity pass into the appa-
ratus; p is a peep hole covered over with glass, through which the interior of the
vessel may be viewed; q is the baryta or other base contained in the vessel k.
Atmospheric air and oxygen are caused to enter onto the base g through the
pipes m, m³, and under the influence of electricity acting through the wires o, o',
the nitrogen of the air combines with the oxygen and unites with the base so as to
form a nitrate or nitrite of the said base. By this means the nitrate or nitrite
which had been decomposed in the retort a may be renewed or reconstituted, and
the operation may be continued with only such intervals as are caused by the
removal of the residuum, and its being replaced by reconstituted nitrates or
nitrites.
Amongst the bodies fulfilling the necessary conditions which we prefer to select
for forming the nitrates or nitrites we may mention, firstly, potash, soda, baryta,
lime, manganese, iron, lead, but it will be understood that we do not confine our-
selves to these bodies, as others having the same properties may be advantageously
used in our process; secondly, amongst the bodies which fulfil the requisite con-
ditions for combining with the oxygen of the nitrogenated compounds, and of the
vapour of water, we prefer to select charcoal or iron, as being more easy to obtain
and use, but we do not confine ourselves to them, and we claim the right of using
all bodies capable of being regenerated under the influence of heat alone, or of a
body having more affinity than them for the oxygen they have absorbed.
As an example we may site iron which at a red heat absorbs oxygen, forming
oxide of iron. If then it be required to regenerate the iron, all that is necessary is
to subject the said oxide of iron to the reducing action of oxide of carbon. We
may also mention mercury which absorbs or reabsorbs oxygen at a temperature of
350 and 450 degrees centigrade, or 662 and 842 degrees Fahrenheit respectively.
Figure 3 represents a modification of the apparatus represented in Figures
1 and 2. In this modification the vessel a and furnace b, Figure 1, are dispensed
with, and in their place is substituted a vessel K, Figure 3, similar in every respect
to the stone vessel herein before described and represented in Figure 2, except that
for the pipe m' is substituted a pipe c¹ connecting the said vessel K with the retort
d which as well as the reservoir g and parts connected therewith are similar to
those represented in Figure 1, and being marked with the same letters of reference
we do not consider further description of them necessary. Through the pipo m,
Figure 3, nitrogen and oxygen previously mixed together, or atmospheric air, or
atmospheric air prepared for the purpose is caused to enter the vessel K, and by
the action of electricity conveyed through the wires o, o'; the said atmospheric air
or prepared atmospheric air or mixture of nitrogen and oxygen is transformed into
vapours of oxide of nitrogen, which vapours pass through the pipe C¹ into the
retort d, and the process is then continued in the retort d and reservoir g, as
herein before described with reference to Figure 1.
Having now described the nature of our said Invention, and the manner of
carrying the same into effect, we wish it to be understood that we do not confine
ourselves to the precise details hereinbefore described and illustrated in the
accompanying Drawing, as the same may be varied without departing from the
nature of our said Invention; thus the vessel a, the retort d, and the vessel k may
be made of any other suitable shape and arrangement, and the vessel a and retort d

page_text: may be heated by other means than those represented and described. Also, the
reconstitution of the nitrate or nitrite employed may be effected directly in the
vessel a, Figure 1, after its distillation, and when the base remains as a residue by
arranging the said vessel so as to allow a mixture of nitrogen and oxygen gases or
air to enter it, and causing electricity to act upon it so as to form with the base
the required nitrate or nitrite.
But we claim as our Invention,―
Firstly. The combination of the means and processes herein before described for
the purpose of producing ammonia on a manufacturing scale.
Secondly. The combination of apparatus for the manufacture of ammonia, sub-
stantially as herein before described and illustrated in Figure 1 and in Figure 3
of the accompanying Drawings respectively.
Thirdly. The means of effecting practically the constitution or the reconstitution
of nitrates or nitrites used in the manufacture of ammonia according to our process,
and the construction and arrangement of apparatus for effecting such constitution
or reconstitution of nitrates or nitrites, substantially as herein before described and
illustrated in Figure 2 of the accompanying Drawing.
In witness whereof, we, the said William Müller and Edmond Geisenberger,
have hereunto set our hands and seals, this Thirteenth day of October, in
the year of our Lord One thousand eight hundred and seventy nine.