Improvements in the Method of and Apparatus for Manufacturing Cyanides, Ammonia, and Fuel Gas.
Year: 1893

page_text: Date of Application, 4th July, 1893-Accepted, 25th Nov., 1893
COMPLETE SPECIFICATION.
Improvements in the Method of and Apparatus for Manufacturing
Cyanides, Ammonia, and Fuel Gas.
A communication from ESEK COWEN, of 15, Wall Street, in the City, County, and
State of New York, United States of America, Attorney at Law.
I, ALFRED JULIUS BOULT of 323 High Holborn in the County of Middlesex,
Chartered Patent Agent, 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 produce with rapidity and at a comparatively
small expense such combinations of nitrogen as are available for use in agriculture
and in the industrial arts or which are capable of being so rendered by some simple
secondary process; and simultaneously with such combinations to produce fuel
gases capable of being utilized for domestic or industrial purposes, and to this end
my correspondent avails himself of the synthetical and dissociative influence of a high
temperature in the manner hereinafter fully set forth and preferably by means of
an improved apparatus illustrated in the accompanying drawings, in which
Figure is a vertical elevation of said apparatus ;
Figure 2 is a vertical sectional elevation, enlarged, showing the furnace, retort
and washer;
Figures 3, 4 and 5 are transverse sections respectively, upon the lines a b c
Figure 2.
Figures 67 and 8 are views showing another form of apparatus specially intended
to obtain combined nitrogen.
The most valuable forms of combined nitrogen are cyanogen and its salts, and
ammonia, and for this reason my correspondent has devised a method and means
whereby to obtain these products cheaply and rapidly.
While use can be made of various forms of apparatus in carrying out this
improved process, that illustrated in the drawing is preferred, in which A represents
a steam generator which may be of any suitable construction; B a gas generator
of any suitable construction; C a furnace for the production of cyanides; L a tank
and K a washer.
The generator or steam boiler A is of any suitable construction and has a
capacity equal to the production of the amount of steam required.
Steam from the boiler A passes through an injector a by means of which or of
any other suitable form of pump, jet aspirator or exhauster, a suitable volume of
steam and air is forced or drawn through an incandescent volume of carbonaceous
or hydro-carbonaceous fuel contained in a generator B, the oxygen of the steam
and air combining with the incandescent carbon of the fuel to produce carbonic
oxide and carbonic acid, while the hydrogen and nitrogen are set free, and the
general result being combustible gas containing a large volume of nitrogen.
A suitable generator gas may be also produced by similarly passing air, unmixed
with steam, through the incandescent fuel in the generator B, forming a generator
or producer gas, of which the well-known Siemens' producer gas is an excellent
type. In this case, the boiler A may be dispensed with.
Through the combination of its oxygen with the carbon of the incandescent fuel
in the generator B as just described, the nitrogen of the air is thus rendered
practically free from oxygen and is reduced to a condition suitable for the production
of cyanides a large volume of fuel gas being simultaneously produced.
The details of construction of the furnace G, are best shown in Figures 2 and 5,
which illustrate said furnace as consisting generally of an elevated stack of fire
brick or other refractory material. Said stack has a feed opening 3, at the upper

page_text: end and is expanded below the latter to receive the retort M also of suitable
refractory material, the chamber W between the retort and the stack communicating.
with a fire-place D the lower end of the retort communicating with the top of the
tank L, containing a suitable supply of water and an outlet opening 4, affording a
.communication between the tank Land the washer K which may be of any approved
construction, but as shown is provided with a series of alternating plates forming a
circuitous passage. The gaseous matter passes from the washer K to the pipe 6
and the wash-water passes into the washer through the pipe e. At the top of the
stack and preferably at such an elevation above the retort as not to be detrimentally
affected by the heat of the latter, is arranged a hopper F having a feeder G shown
in the form of a revolving screw, but which may be of any other suitable con-
struction and a distributor H in the form of a revolving disc but which may be of
any other suitable construction and which receives the matter fed from the
hopper by the screw and distributes, it equally through the opening 3 into the
retort. This distributor, though advantageous is not absolutely necessary. Where
the hopper, feeder and distributor may be exposed to any excessive heat, they are
made of suitable refractory material. The pipe 7 extending from the generator B
communicates at the upper end with two branches 89 leading to two super-
heaters P P at the upper part of the stack, a valve R₁ in a casing R serving to
direct the gases alternately to one superheater or the other, said gases after passing
through either superheater flowing through a port S1 into the inlet opening 3 and
passing thence to the retort. Ports TT communicating with a circumferential
chamber O around the top of the retort permit the gases from the chamber W to
pass alternately to the superheaters P P accordingly as said ports are controlled
by valves 10 10 and other ports U U controlled by valves 12, 12 afford communi-
cation between the superheaters and the chimney E. In the stack and around the
inner chamber W is a chamber or series of chambers N with which communicates
one or more pipes 13, leading from a reservoir, or other source of supply of air or
combustible gas or of both. These superheaters may, under some circumstances,
be dispensed with. Assuming that the stack has been heated to a sufficient
temperature, by the products of combustion, from the fire-place D, and that one of
the superheaters P or P' has also been heated by said gases which have just been
directed into the other superheater communication is opened between the generator B
and the heated superheater, the gases from the generator B are caused to flow
through the heated superheater and out through the opening s¹ into the feed-
opening 3 and there meeting the material falling from the feeder pass downward
therewith through the retort M.
These gases will, usually, practically consist of a mixture of hydrogen oxides of
carbon, and nitrogen, the last named being in the proportion of about 60% and
will probably vary in composition within certain limits according to the temperature
and process of distillation or source and material from which they are obtained.
Simultaneously with the introduction of the superheated generator gases into the
retort M as just described, there is introduced through the pipe J into the feed-
opening 3 a suitable volume of hydrocarbon gas or vapour or a mixture of both,
which mixes with the generator gas passing through the retort. The hydrocarbon
gases or vapours thus introduced or, as usually happens, a mixture thereof, may be
derived from any suitable source, and may or may not be accompanied by or mixed
with other gases and vapours.
Also, by means of the feeder G, there is fed into the retort from the hopper Fa
suitably adjusted volume of pulverized alkali or alkaline earth, which passes down-
ward through the retort in a state of intimate mixture with, and in the company of
the generator and hydrocarbon gases. My correspondent does not, however,
confine himself to the process of introducing the alkali into the retort in a
pulverized state, for under certain conditions it may be advantageously introduced
in the form of vapour, in which case the hopper may be dispensed with and a pipe
for the introduction of the vapour may be substituted. In passing through the
externally heated retort M the hydro-carbon gases and vapours thus introduced

page_text: produced may pass to the tank L, where part of them will be decomposed,
producing ammonia and fuel gases, the remainder being converted by means of
suitable iron salts or oxides in ferro-cyanides which are utilized in any well
known way.
When ammonia is the product chiefly sought for, the cyanides may be decomposed
before passing into the tank L, by means of a regulated volume of steam admitted
at a point above the bottom of the retort to a pipe shown in dotted lines. This
will decompose the cyanides producing ammonia and its carbonates and fuel gas.
The production of the cyanides raises the temperature at the lower part of the
retort without any detrimental effect, as far as regards the cyanides themselves, but
causing loss and inconvenience when the production of ammonia is desired, the high
temperature decomposing the nascent, ammonia into its elements. To avoid this
I feed from the hopper F such an excess of carbon as will decompose a similar
excess of steam producing a volume of water gas that will absorb or take up
the heat sufficiently to reduce the temperature of the resulting gases to a degree
suitable for the production and preservation of ammonia.
A Figures 6, 7 and 8 is a furnace for the production of cyanides and fuel gases.
This furnace is suitably connected with a gas generator B and encloses a suitable
constructed retort C, which is externally heated by means of a volume of flame
passing through the surrounding flue or fire-chamber D. The retort is also shown
as suitably provided with a hopper E and feeding mechanism F. G shows a
suitably located pipe or other suitable duct, by means of which a suitable hydro-
carbon either solid, liquid, or gaseous, is introduced into the fluc H. L are
refractory bafflers or shelves, for the purpose of retarding the fall of pulverized
material when such is used, through the retort and M is a tank containing water
for collecting or decomposing the cyanides.
By the combustion of carbonaceous fuel of any sort, whether solid, liquid or
gaseous, in a suitably adjusted volume of air or of air and steam mixed, there is
produced in a furnace B (constructed suitably to the character of the fuel used) a
volume of generator or producer gas; and, by means of a secondary volume of air
supplied through a flue 1, or its equivalent, part of the generator or producer gas
is burned in the combustion flues or chambers J, and by means thereof the retort C
is raised to a high temperature.
As soon as the retort C has reached a working heat, I suck, draw or force, by
means of a suitable fan, blower aspirator, exhauster, or other suitable apparatus,
a suitably adjusted volume of the generator gas produced in B, up through the
flue H, and thence down through the retort C, and through or over the water in
the tank M, whence the gas is drawn through suitable washers or scrubbers or other
suitably constructed apparatus, whereby the cyanides and other nitrogenous com-
pounds produced, may be collected. For the purpose of illustration a blower X
is shown for impelling the gas.
My correspondent now, by means of the hopper E, and the feeder F, feed a
suitable volume of an alkali or of a suitable compound or admixture thereof into
the retort C, through, which it falls and wherein it is brought into intimate contact
and admixture with the generator gas passing through the retort.
My correspondent usually prefers to use the alkali in the form of a powder, but
it is sometimes preferable to introduce it into the retort in a vaporized condition.
Also when it is introduced into the retort in a pulverized condition, and is inclined
to be rendered pasty by the heat or from any other cause to clog the feeder, there
is frequently an advantage in mixing with it some inert, infusible substance such as
pulverized carbon, whereby the pastiness of the alkali may be compensated for and
corrected. The carbon used will not be lost, for it may be caused to decompose
a volume of steam, preferably superheated, admitted into the lower part of the
retort, and may thus be caused to produce a large volume of fuel gas.
Also by means of the pipe G a suitable volume of hydrocarbonaceous matter is
introduced into, the flue H. This hydro-carbon may be in either the solid, liquid,
gaseous or vaporous condition, in any of which cases, it will be decomposed by the

page_text: heat, the volatile portion of its solid or liquid matter into gases and vapours, and
its gaseous and vaporous constituents into simpler products, so that, in any case,
its constituent volatile matter will be certain to reach the retort in the form of gas
or vapour. When a liquid, gaseous or vaporous hydro-carbon is used, it may be
caused to flow through the pipe G, by simple gravity or pressure; but, when the
hydrocarbon is used in a solid form, it will be necessary to force it through by
means of some suitable mechanism.
The mixed generator and hydro-carbon gases are now caused to enter the retort C,
but as it is most desirable that they should be practically free from free oxygen and
carbonic acid under the influence of the high temperature, such oxygen as may be
present in the generator gas is caused to combine with the hydrocarbons, and its
carbonic acid also, to be reduced by them with the production of carbonic oxide
and free hydrogen.
The mixed gases and vapours introduced into the retort C, are there subjected
to a high temperature, and the contained hydro-carbons finally become "cracked"
or reduced to simpler compounds, and, under sufficient exposure to the high
temperature, become finally resolved into nascent carbon and hydrogen, and, there
are thus produced compound and simple bodies which are possessed of strong
chemical affinities, and which combine readily with free nitrogen in the presence of
an alkali, and under the influence of a high temperature, while some notably
nascent hydrogen and acetylene, are endowed with such strong affinities that they
are capable of combining directly with nitrogen, thus:
42 (ascent) + 12 A
Around these metamorphoses revolves an endless train of intermediate, analogous,
and secondary reactions, all of which tend and gravitate to, and rest upon the
common basis of the intense chemical energy and strong affinities of acetylene and
nascent carbon and hydrogen, and the same holds good, but in a much less degree,
of olefiant gas..
Among the above reactions may be included the analogous results obtained by
the use of the other alkalies, such as potassium, calcium barium, magnesium and
strontium; and of their carbonates, oxides, and hydrates, all of which are avail-
able, in a greater or less degree for the purposes of this invention.
The cyanides produced are received in the tank M, where they may be treated
by any of the usual processes. When the chief object is to produce ammonia, the
cyanides may be decomposed before falling into M, by means of a suitably regulated
volume of steam, preferably superheated, admitted to the retort at such a height
above the water as to ensure their decomposition before reaching it.
When pulverized carbon is introduced into the retort through the hopper E,
steam sufficient for its gasification should be admitted over and above that required
for the decomposition of the cyanides and the production of ammonia.
Having now particularly described and ascertained the nature of this invention
as communicated to me by my foreign correspondent, and in what manner the same
is to be performed, without limiting myself to the precise processes or succession
of processes, actions and reactions described, or to the exact form and arrangement
of apparatus shown, I declare that what claim is :-
1. In the production of cyanides causing acetylene and nascent carbon to combine
with nitrogen by bringing the same into the presence of finely divided alkali within
a heated retort or chamber the nitrogen being previously superheated substantially
as set forth.
2. In the production of cyanides and ammonia passing through a highly heated

page_text: retort a gas containing oxides of carbon free hydrogen and nitrogen together with
hydrocarbon gas and an alkali or the vapour thereof thereby producing alkaline
cyanides together with ammonia and free gas as hereinbefore set forth together
with the sub-processes described.
3. The within described improvement in producing ammonia or the simple hydro-
carbons by hydrogenation and securing acetylene by highly heating hydrocarbon
gases and vapours and adding fuel gas to the nascent acetylene substantially as
set forth.
4. The method of producing a fuel gas by burning carbonaceous matter supplying
air or steam thereto and introducing bydrocarbon and bringing the gases into the
presence of a heated alkali, substantially as set forth.
5. In the production of cyanides, ammonia and fuel gases, supplying the heating
retort with the excess of carbon and subsequently decomposing by steam for the
purposes set forth.
6. The within described apparatus, consisting of a retort combustion chamber
and gas supplying devices together with the superheaters feeders and distributors
substantially as set forth.
7. A mixing and decomposing furnace or chamber with generating furnace and
ammonia retort substantially as set forth.
Dated this 4th day of July 1893.
W. P. THOMPSON & BOULT,
Agents for the Applicant.