Process of and Apparatus for Manufacturing Ammonia.
Year: 1887

page_text: Date of Application, 11th Oct., 1887
Specification Accepted, 11th Nov., 1887
COMPLETE SPECIFICATION.
A Process of and Apparatus for Manufacturing Ammonia.
I, BENJAMIN JOSEPH BARNARD MILLS carrying on business under the firm or style
of Harris and Mills of 23 Southampton Buildings, in the County of Middlesex, Patent
Agent, do hereby declare the nature of this invention, a communication to me
from abroad by Thomas B. Fogarty, of the City of Brooklyn, County of Kings, and
State of New York, in the United States of America, and in what manner the same
is to be performed, to be particularly described and ascertained in and by the
following statement, reference being had to the accompanying drawings, forming a
part of this specification
:―
The object of my invention is to obtain ammonia by a simple and economical
process from atmospheric nitrogen and the hydrogen of decomposed steam.
It is well understood that ammonia cannot be practically produced upon a large
scale by the direct synthesis of its elements; but it is at the same time well known
that there is no practical obstacle in the way of the artificial production of cyanogen,
and that this having been produced, as an intermediate step, its conversion into
ammonia is an easy matter.
It is well known also that it is extremely difficult to effect the combination of
nitrogen and carbon-the elements of cyanogen and to form free cyanogen gas, even
at a high temperature. If, however, an alkali or alkaline earth, or indeed, any
substance capable of combining with cyanogen, or of producing a substance capable
of combining with it be present, cyanogen is readily produced from its elements and
combined with the alkali to form therewith a cyanide or cyanate which, in turn,
may be decomposed by steam with the production of ammonia, oxides of carbon,
and hydrogen gas.
Taking advantage of this disposition of incandescent nitrogen and carbon to
combine in the presence of an alkali, submit a suitably prepared mixture of
carbon and alkali to the action of nitrogenous gas in a close furnace or retort, and,
simultaneously with such gas, or mixed therewith, I also introduce into my retort a
ሐ

page_text: suitable volume of steam, preferably super-heated, whereby the cyanides resulting
from the combination of the nascent cyanogen with the alkali, may as fast as formed,
be decomposed by the steam with the production of ammonia, oxides of carbon, and
hydrogen gas; the alkali returning to its original state or entering into fresh
combinations.
The nitrogen used may be derived from any suitable source, but I prefer to obtain
it from the nitrogenous gas produced by the partial combustion of coal, coke, or any
other suitable form of carbon in a closed furnace or cupola.
I shall now proceed to describe my invention so fully and clearly that any person
skilled in the art of making ammonia may be able to understand and practice the
same, and for this purpose I shall divide or classify it into two heads or parts,
consisting, first, in obtaining nitrogen either pure or as contained in nitrogenous fuel
gas, and second, in converting such nitrogen into ammonia by causing it to combine
with hydrogen.
In carrying out the first part of my invention I prefer to make a nitrogenous fuel
gas by forcing air, either alone or mixed with steam, through a suitable cupola,
furnace or retort suitably filled or charged with coal, or coke, or other suitable
carbonaceous fuel in a state of combustion or incandescence.
My second stop consists in the conversion, either in whole or in part, of the nitrogen
of the nitrogenous gas into ammonia, and consists in causing the gas to pass through
a suitably constructed cupola, furnace or retort wherein it meets with suitably
adjusted currents or moving volumes of suitably mixed carbon and alkali, preferably
in a pulverized or finely divided state, and steam-preferably super-heated; and
wherein the mixed volume of nitrogenous gas, alkalized carbon and steam is subjected
to a high or incandescent temperature, under the influence of which the alkalized carbon
combines with the nitrogen of the gas to form alkaline cyanides which are, in turn,
decomposed by the steam with the production of ammonia, oxides of carbon and
hydrogen gas, while the combined alkali returns to its original state or enters into
fresh combinations.
The annexed drawings illustrate and are a part of this specification.
In Figure 1 which shows, in elevation, the general arrangement and form of my
apparatus
A is a steam boiler of any suitable construction, B a cupola or furnace for
producing nitrogenous gas, C a furnace for the conversion of the nitrogen of the
nitrogenous gas into ammonia; D, a washer wherein the solid matter escaping from C
is separated from the gas, and É a condenser wherein the gas, now largely im-
pregnated with ammonia, is cooled preparatory to the separation and collection of the
ammonia.
In Figure 2, which is a vertical section of C, and D, Figure 1.
F is a vertical cupola or retort, provided at top with a suitable hopper G, suitably
provided with a suitable feeding screw H for feeding the alkalized carbon into the
retort F, which is filled with suitable shelves or bafflers by means of which the
downward passage of the alkalized carbon through the retorts is retarded. I is
the outlet from the retort F and is sealed in the liquid contained in the hydraulic
main J. D is a washer in which the gas is freed from such dust as may adhere to it,
and whence the gas passes through the outlet K to the condenser E, where it is
cooled preparatory to the contained ammonia being separated and collected by any of
the usual processes.
L is the inlet for the admission of nitrogenous gas to a super-heater M, whence it
enters the retort F at N.
O is an inlet for the admission of steam to a super-heater P, whence it enters the
retort F, at R.
S is a furnace, of any suitable construction for heating the cupola F.
Figures 3 and 4 are sections of Figure 2, on the lines X and Y respectively.

page_text: DIODE OF OPERATION.
The mode of operation is as follows :-I first force air alone or air and steam mixed
through a suitably constructed cupola or furnace B containing incandescent coal,
coke, or charcoal, or any suitable form of carbon in a state of incandescence, and
thereby produce a fuel gas containing a large per cent. of nitrogen. I now cause my
nitrogenous gas to pass through the pipe L into a suitably constructed super-heater M,
wherein it is raised to a high or incandescent temperature. From the super-heater M
my gas passes into a suitably constructed retort F, which is maintained at a high or
incandescent temperature by the furnace S; and wherein it meets with a suitably
adjusted volume of steam, preferably super-heated by means of the super heater P.
The mixed volume of gas and steam now encounters a suitably adjusted volume of
pulverized carbon and alkali which is fed into the retort continuously by means of the
screw H from the hopper G, whereupon the mixed volume of gas, steam and
pulverized material pass downward, through the retort wherein it is raised to and
maintained at a uniformly high temperature, the consequence of which is that the
nitrogen of the gas unites with the carbon and alkali to form cyanides and cyanates
therewith and these, in turn, are immediately decomposed by the steam present
producing ammonia, oxides of carbon and hydrogen gas; while the alkali is set free
and returns to its original state or enters into fresh combinations. I am careful that
the volume of steam used may be largely in excess of that required for the mere
decomposition of the cyanides and the resulting production of ammonia, because I am
thus enabled, through the decomposition of the steam by the pulverized carbon, to
increase both the volume and quality of my resulting gases to any desired extent,
and, with the additional advantage of furnishing to any desired extent, either in the
form of fuel gas or of undecomposed steam or gaseous envelope sufficient for the
protection and preservation of my ammonia. which might, otherwise, be destroyed by
contact with the heated surfaces of the interior of the retort.
My gaseous product and undecomposed solid matter now escape from the retort
through the outlet I and pass into a suitable hydraulic main J wherein they become
partially separated, the heavier portion of the solid matter remaining in J, while the
gaseous mixture passes onward through the washer D, wherein the Hoating particles
of dust which still adhere to it are washed out, and whence it escapes into the
condenser, or other suitable cooling apparatus E, wherein it is cooled and prepared to
have the contained ammonia separated from the other gases by means of scrubbers or
other suitable appliances. The solid matter which collects in the hydraulic main and
washer may be removed by the screw Q.
It is evident that the super-heaters M and P may be dispensed with, as the gaseous
and pulverulent volume descending through the retort would, under ordinary
circumstances, soon become raised to a high temperature by the beat of the retort
itself, but, the effect of this would be to throw so much more work upon the retort
the effectiveness of which would be diminished to a corresponding extent, and,
consequently, it is most desirable that the gas and steam would be both raised to as
high a temperature as practicable before entering the retort.
It is also evident that the gas and steam may, without disadvantage, be mixed
before being super-heated.
I do not bind myself to the exact process or succession of processes, or to the
exact form of apparatus described, for it is evident that they may be varied
indefinitely.
Having now particularly described and ascertained the nature of my said invention
and in what manner the same is to be performed I declare that what I claim is :-
1. The process herein described of producing ammonia, consisting substantially as
follows; first, injecting air alone, or air and steam mixed, into and through
incandescent carbon contained in a suitable furnace, causing the oxygen of the air; or,
of the combined volume of air and steam to combine with the carbon and to produce

page_text: carbon gases and free nitrogen; second, causing the crude nitrogenous gas so
produced to mix with a suitable volume of steam, and the mixed volume of gas and
steam to meet with a moving or falling volume of carbon and alkali reduced to a
pulverized or finely divided state, commingling and mixing intimately with such
carbon and alkali and causing the nitrogen of the gaseous mixture to combine with
them producing cyanogen which is, in turn, decomposed by the steam present
producing ammonia, hydrogen gas, and oxides of carbon, substantially as described.
2. In a process for producing ammonia, the process of causing nitrogenous
generator gas to meet and mix with a suitably adjusted volume of steam, and the
mixed volume of gas and steam so formed to meet with a moving or falling volume of
carbon and alkali reduced to a pulverized or finely divided state, raising the entire
volume, both gaseous and solid, to a high or incandescent temperature, causing the
nitrogen of the gas to combine with the carbon and alkali and to produce cyanogen
and decomposing this by means of the steam present with the production of ammonia,
hydrogen gas, and oxides of carbon, substantially as described.
3. In a process for producing ammonia from the nitrogen of nitrogenous gas by
causing such nitrogen to combine with carbon and alkali and to produce cyanogen
and alkaline cyanides, which, in turn, are decomposed by steam, producing ammonia,
hydrogen gas, and oxides of carbon, the process of super-heating the steam and gas
previously to their introduction to the retort in which the ammonia is produced,
substantially as described.
4. In a process for producing ammonia from the nitrogen of nitrogenous gas by
causing such nitrogen to combine with carbon and alkali, and to produce cyanogen
and alkaline cyanides and for decomposing the cyanogen and cyanides, so produced,
by steam, producing ammonia, hydrogen gas, and oxides of carbon; the process of
producing the cyanogen in an atmosphere of nitrogenous gas and steam mixed, and
afterward decomposing the cyanogen so produced by the steam contained in the
mixture, substantially as described.
5. In a process for producing ammonia from the nitrogen of nitrogenous gas by
causing such nitrogen to combine with carbon and alkali; and to produce cyanogen
and alkaline cyanides, and for decomposing these by steam, producing ammonia,
hydrogen gas, and oxides of carbon; the process of preserving the ammonia by
means of an excess of steam, substantially as described.
6. In an apparatus for producing ammonia, the combination of the retort F, with
the super-heaters M and P, constructed and operated substantially as described.
7. In an apparatus for producing ammonia, the combination of the feeding
apparatus G, with the retort F and super-beaters M and P, constructed and operated
substantially as described.
8. In an apparatus for producing ammonia, the combination of the retort F, with
the hydraulic main J, suitably provided with the extracting screw Q, constructed and
operated substantially as described.
9. In an apparatus for producing ammonia, a hydraulic main J, suitably provided
with an extracting screw Q, constructed and operated, substantially as described.
Dated this 11th day of October 1887
B. J. B. MILLS.
By Harris & Mills,
23, Southampton Buildings,
Agents.