IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE OF AMMONIA AND HYDRO-CARBON GASES
Year: 1883

page_text: LETTERS PATENT to William Robert Lake, of the firm of Haseltine, Lake.
& Co, Patent Agents, Southampton Buildings, London. for an Invention of
"IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE OF AMMONIA AND
HYDRO-CARBON GASES " communicated to him from abroad by Thomas Burke
PROVISIONAL SPECIFICATION left by the said William Robert Lake at
the Office of the Commissioners of Patents on the 13th November 1883.
WILLIAM ROBERT LAKE, of the firm of Haseltine, Lake, and Co, Patent Agents
Southampton Buildings, London, IMPROVEMENTS IN AND RELATING TO THE,
[A communication to him
from abroad by Thomas Burke Fogarty, of Brooklyn, New York, United States of
America.]
«
MANUFACTURE OF AMMONIA AND HYDRO-CARBON GASES
">
This invention relates to the production of ammonia and the manufacture of gas
and comprises improvements upon the process' described in the specification of
former Letters Patent granted to me and dated February 28th A D 1882 N° 978.
The chief object of the present invention is the production upon a large scale of
ammonia from atmospheric nitrogen, by a cheap and simple process, and its novelty
mainly consists in converting the atmospheric nitrogen, discharged with the hydro-
carbon gases and other products of furnace combustion, into ammoniacal gas,
removing the ammonia from the said gases, and then passing the remaining
nitrogenous gas, deprived of carbonic oxide and carbonic acid, into retorts containing
bituminous coal, mixed with an alkali or alkaline earths, while undergoing the.
process of destructive distillation for the generation of illuminating and heating
gas, or either of them, if desired, as hereinafter fully described.
The several parts or subprocesses making up the complete process and the order
in which they are preferably employed may be conveniently described or classified
as follows, that is to say:-
1 The manufacture of a cheap, nitrogenous non-illuminant heating gas. II. The
superheating in a suitably constructed apparatus of the said nitrogenous gas,

page_text: thereby removing any undecomposed steam therefrom or removing such steam by
condensing it previous to superheating the gas, or in any suitable manner.
III. The introduction of the said superheated gas, so freed from steam or moisture,
into a suitably constructed furnace, cupola, or retort, wherein it is met by a falling
shower or volume of a mixture of carbon and alkali reduced to a finely divided or
pulverulent state, which mixture is thereby raised to the high temperature of the
gas itself, the nitrogen therein being thus caused to combine with the carbon and
alkali and to form therewith cyanogen or compounds or derivatives thereof.
IV. The decomposition of the cyanogen, its compounds or derivatives by means of
steam, producing thereby ammoniacal and non-illuminant combustible gases. V. The
separation first of the ammonia from the said gases and then the carbonic oxide
therefrom and also any carbonic acid that may be generated, and then passing the
remaining nitrogenous gas, consisting mainly of hydrogen and some free nitrogen
into suitably constructed retorts containing bituminous coal, appropriately mixed
with a suitable alkali or alkaline earth, undergoing destructive distillation, the
result being large additional volumes of ammoniacal and other gases; VI. The
treatment of the coke produced in the said process of distillation, with water in a
close chamber, for the purpose of decomposing the cyanides and other compounds
of cyanogen therein contained, and thereby obtaining a further additional yield of
ammonia.
VII Mixing the ammonia thus generated, and the combustible gases and steam
which are invariably produced with it, with the volumes of illuminating and other
gases escaping from the retorts and subjecting this mixture of gases to any of the
improved processes of condensation, scrubbing and other means of purification
usually adopted, whereby the ammonia is collected and separated from the coal
gas proper, and may be treated in any approved manner to obtain it in solid form,
if desired.
It is evident that although the first four-sub-processes or steps above mentioned
constitute a complete process of making ammoniacal and non-illuminant combustible
gases, and may be used as an independent process by stopping the operation at
such point and recovering the ammonia in solid form, if desired, by any approved
method, yet, as preliminary steps in one continuous process, they furnish
ammoniacal and non-illuminant combustible gases which, when treated as, above
described, furnish a nitrogenous gas which can be as readily combined with
bituminous coal and alkali in process of destructive distillation for the production
of illuminating gas, where desired, as can atmospheric air or any nitrogenous gas
derived from any source, with the greater advantage, however, of thereby
generating largely, increased volumes of coal gas and at the same time a large
additional volume of ammonia, as hereinafter fully explained.
For the purpose of making more clearly understood the precise manner in which
the manufacture of ammonia may be advantageously combined with the
production of illuminating gas through the destructive distillation of bituminous
coal, it is necessary to advert to some conditions of the coal-gas manufacture which
have not hitherto met with the attention to which their importance entitles them.
In the manufacture of coal-gas, as usually conducted, bituminous coal is charged
into suitable retorts set in suitable ovens or furnaces and heated by an external
fire to a high temperature thus subjecting the coal to destructive distillation, the
products of such distillation being illuminating gas more or less contaminated by
impurities, ammoniacal liquor and tar.
As soon as the process of distillation is completed, the incandescent coke is
withdrawn from the retorts, and that portion of it which is not required for
immediate use as fuel is cooled or quenched in the open air by means of water
and thrown aside until needed for use as fuel. It has been ascertained, however,
from chemical examination of this coke and of the gases evolved from it during
the process of being cooled by water, as described, that it contains large quantities 5
of cyanides and that the escaping vapors and gases are highly charged with
ammonia capable of being collected and utilized as a by-product.

page_text: It is also well established that the ammonia produced by the destructive distilla-
tion of bituminous coal, and also that obtained during the cooling process from the
cyanides in the coke, is not originally contained in the coal itself but only the
elements required for its production, and that it is by the combination of these
elements within the retorts that the ammonia and other products of cyanogen
which are obtained, are formed.
It is likewise known that the illuminating power of coal gas is mainly due to
the rich hydro-carbon vapors which are evolved from the coal during the earlier,
periods of distillation, and, that a large percentage of these vapors becomes"
condensed or converted into tar in consequence of the gases which are being
evolved, not containing non-illuminant gases, such as hydrogen and light carburetted
hydrogen, sufficient to dissolve and retain in suspension the large volume of rich
illuminating vapors evolved at this period of the distillation; so that a great loss
of rich illuminating material takes place through the want of a suitable diluent
capable of absorbing and retaining them in suspension.
>
For these reasons, in localities where there are gas-works, it is of great advantage:
to combine the manufacture of ammonia from atmospheric nitrogen with that of
coal gas, for, thereby not only may the yield of ammonia be enormously increased,
but at the same time a still greater increase of rich illuminating gas is produced,
for, the large volumes of non-illuminant gases generated in the preliminary ammonia
process, if introduced into the coal-gas retorts at a suitable period of the distillation
and in suitable quantity, furnish exactly what is needed at that time, an excellent
diluent capable of absorbing and retaining in solution the rich hydro carbon vapors
which would otherwise go to form tar, and at the same time, containing as they do
a very large percentage of nitrogen, they furnish material which uniting with the
carbon and alkali in the retorts, produces cyanogen and cyanides readily convertible:
into ammonia.
4
=
1
While, therefore, for the purposes of this invention it is not essential to have
recourse to the non-illuminant gas produced in the preliminary ammonia process,
for, any generator gas free from steam and sufficiently free from carbonic oxide and
carbonic acid may be used, yet the non-illuminant gases produced in the preliminary
ammonia process, suitably purified as described, will be found much superior to
ordinary generator gas for the purpose of a diluent, on account of the percentage of
nitrogen therein having been largely reduced by the preliminary ammonia process. :
The coke remaining in the retorts at the end of the distillation will contain a
large percentage of alkaline cyanides which may be converted into ammonia, for:
which purpose, instead of withdrawing it from the retorts, and cooling, or quenching
it with water in the open air, as is commonly done, immediately after withdrawing
it from the retorts it is introduced into a suitably constructed vessel or chamber,
or a series of such, wherein it is cooled or quenched by means of steam, or preferably,
by throwing upon it a regulated jet or spray of water.
There is an objection to the use of steam for quenching the cyanized coke
because, to be effective, it must necessarily be introduced at the bottom of the
chamber, and if this be done, the ammonia produced will be forced to pass
upward through the superincumbent mass of incandescent coke and will be thereby!
decomposed, whereas by using, instead of steam, a jet or spray of water, thrown
upon the top of the mass of incandescent coke, it is cooled from the top downward
so that the ammonia produced will always ascend through a medium having a
temperature lower than that at which it was formed and will therefore be in no
danger of being destroyed, as would happen if steam were used.
1
3.
The coke produced in the ordinary process of making coal gas may be advan-:
tageously treated with steam or preferably a jet of water in close chambers, as just
described, with the result of producing an increased yield of ammonia through the
decomposition of the contained cyanides as above described. It is, however, at
all times advantageous to further increase the yield of ammonia by supplying
additional volumes of nitrogen from the atmosphere, or other sources, and alkali, as
already described

page_text: According to the said invention a generator is suitably charged with coal, coke,
charcoal, or some other suitable form of carbonaceous fuel; and, the fuel having
been ignited it is allowed to burn until it becomes incandescent. A chimney valve
is now closed, and, by means of a suitable jet, pump, or aspirator, suitably adjusted
volumes of air and steam are forced into the closed ash-pit. As soon as the stream
of mingled steam and air comes in contact with the incandescent fuel in the
generator it is forced upward through the mass, and forms what is known as a
generator gas; the hydrogen and nitrogen of the steam and air, for the most part,
passing off unchanged, while their oxygen combines with the carbon of the coal or
other fuel to form carbonic oxide and carbonic acid in proportions which vary
according to the relative proportions of steam and air, the temperature of the
furnace, and the greater or less depth of the mass of incandescent fuel.
A Siemens' superheater is connected to the gas superheater by a pipe and the
superheated or incandescent gas from the former is met in the combustion chamber
of the gas superheater by a current of air, preferably superheated, forced in through
an aperture. By this means the gas superheater and ammonia furnace are both
raised to a proper temperature. The necessary flow of gas is established through
two openings, the latter being closed after the gas-superheater and ammonia furnace
have attained the proper temperature. The opening at the base of the gas-
superheater may be connected to the Siemens superheater or to one of a pair of
such superheaters, so that the heated gases of combustion can at the proper times
be returned, through a suitable valve, back to one of said pair, so arranged as to
alternately discharge into the combustion chamber of one gas super-heater of a pair
of such super heaters. One Siemens superheater and one gas superheater will
thus be maintained in full operation, while the other one of each of said pairs is
revived.
A Siemens regenerator furnace, the gas superheater, and the ammonia furnace
having been thus previously heated, the generator gas is introduced into the
gas-superheater, through an inlet whence it passes upward through the mass of
incandescent bricks contained in the superheater, by means of which it is raised
to an intensely high temperature.
From the superheater the generator gas (now highly incandescent) passing
through a flue into the ammonia furnace where it meets with a volume of carbon
and alkali which is fed continuously into the furnace and at any desired rate
of speed by means of a hopper and valve, or damper or other suitable feeding
apparatus
As the successful operation of the apparatus depends in a very great measure
upon the area of carbonaceous material presented to the action of the gas and
upon a close contact of the solid materials used it is of great importance that the
carbon and alkali should be introduced into the furnace in a finely pulverized or
comminuted state and also in a state of intimate mixture with each other.
f
The highly incandescent generator gas now raises the carbon and alkali to
its own high temperature and, mixed with the falling mass, passes downward
through the furnace, its course being hindered and broken by bafflers or obstruc-
tions placed in the furnace at frequent intervals. The nitrogen in the gas now
combines with the carbon and alkali to form cyanogen and alkaline cyanides, and
these, mixed with the uncombined carbon and alkali and free gases, continue to pass
downward through the furnace until they meet with a jet of steam admitted
through the pipe. The effect of the admission of this steam is such that the
temperature of the descending mass of mixed gases and solids is reduced to, and is
maintained at, any lower point designed, and, at the same time the contained
cyanides are decomposed by the steam being converted into ammonia; while the
solid matter falls to the bottom of the furnace, where it is received in a pan
containing water, or in some other suitable receptacle, whence it may be removed
through an opening suitably sealed by the water in the said pan. The ammoniacal
and other gaseous products escape from the furnace through an outlet and are

page_text: thence conducted to suitable condensers and scrubbers where they are cooled, and
the contained ammonia separated and collected, either in the form of a carbonate or
by the use of any suitable reagent.
The nitrogenous gas thus deprived as far as possible of ammonia carbonic oxide,
carbonic acid, and watery vapor, is led in any suitable pipe to the entrance of the
retort and then treated as hereinafter described.
It will be seen that in the operation just described there is absolute control not
only of the temperature at which the cyanides are formed but also of that at which
they are decomposed. For the formation of the cyanides there is admitted through
the said flue a uniform volume of intensely heated gas and from the feeding
apparatus a regulated volume of mixed carbon and alkali at a low temperature, the
consequence of which is that a stated and uniform equilibrium of temperature will
be maintained in the furnace. In like manner there is supplied through a pipe for
the purpose of decomposing the cyanides formed in the furnace, and which are
descending through it at an uniform rate of speed and in an uniform volume, a
regulated volume of steam of uniform pressure and temperature. The consequence
of this is that here again an equilibrium of temperature will be established, which
can be maintained at any desired point by increasing or diminishing the supply of
steam, easily obtained or maintained at proper temperature for the purpose. The
ability to thus control the temperature at which the cyanides are decomposed and
the ammonia produced is of the highest importance on account of the liability of
ammonia to decomposition by exposure to an elevated temperature.
As it is of the utmost importance that the generator gas should be introduced
into the ammonia furnace in as dry a state as possible, it is very often advantageous
to cause it to pass through a suitable condenser previously to its introduction to the
superheater, for, whatever undecomposed steam it contains will by this means be
almost entirely removed before introducing it to the superheater, where any
undecomposed steam still remaining in it will be taken up and decomposed by the
carbonic oxide of the gas itself, the oxygen of the steam combining with the
carbonic oxide to form carbonic acid, its hydrogen being set free.
For the purpose of making the operation continuous, instead of intermittent, it
is necessary to use two or more sets of Siemens regenerator furnaces (as is usual
in a well known process of making steel), and the same number of gas superheaters.
Should it be desired to combine the process of obtaining ammonia from
nitrogenous gas, obtained through any other than the preliminary ammonia
process, or derived from any other source, with the production of coal-gas through
the destructive distillation of bituminous coal, such nitrogenous gas (but preferably
that subjected to the preliminary ammonia process) however produced, and freed
from steam or watery vapor and carbonic oxide, (at least to a practical extent,) is
introduced in a regulated quantity through an inlet into the lower chamber of a
retort suitably provided with a perforated false bottom and charged in the usual
manner with bituminous coal suitably mixed or impregnated with lime, soda,
potash, or barium, or some other suitable alkali or alkaline earth, and wherein such
alkalized coal is undergoing destructive distillation for the production-if desired―
of illuminating gas.
The nitrogenous gas is now caused to pass through the perforated bottom of the
retort and the superincumbent mass of coal, and to permeate such coal in every
direction, the consequence of which is that the nitrogen in the gas will combine;
with the carbon and alkali, producing cyanogen and compounds thereof.
Part of the cyanogen thus produced, especially in the earlier period of the
distillation, is decomposed by the watery vapor in the retort, while by far the
greater portion remains in the coke as a solid cyanide. The gaseous products of
the retort pass out of the pipe and are collected in any suitable holder or holders,
after separation of the aminonia, and such purification as is commonly practiced in'
condensers, scrubbers and the like of ordinary construction.
The coke produced, or at least so much of it as is not immediately transferred to

page_text: the furnace as fuel, is passed with as little exposure to the air as possible, into a
decomposing or cooling chamber which is immediately closed by a cover.
By means of a water-pipe a regulated jet or spray of water is now thrown upon
the incandescent mass of coke in the cooling chamber. Some of the water is
decomposed by the incandescent carbon but the surface of the mass of coke soon
becomes cooled to a point at which it is no longer capable of decomposing the
water, or rather the steam produced from it. As the coke cools the steam
produced takes hold of, and decomposes, the cyanides contained in the coke, every
stratum of which from the top downwards becomes successively cooled and reduced
to a temperature suited to the production of ammonia. The steam is in turn
decomposed by the cyanides present, its hydrogen continuing with the nitrogen of
the cyanides to form ammonia, while its oxygen unites with this carbon to produce
carbonic oxide and carbonic acid, and their alkali is set free or enters into fresh
combinations. The ammoniacal and other gases produced escape from an outlet,
and, after separation of the ammonia and purification, go to swell the volume of
the illuminating gases already collected from the retort in any suitable gas-holders,
such as are commonly used in gas works.
It will be readily perceived that in the conversion within the cooling chamber of
the cyanides in the coke into aminonia, the cooling process proceeds from the top
downward through the mass of coke, which, if the operation be carefully conducted,
will be cooled at the top to so low a temperature, as to be incapable even of
producing steam; while its centre may be at a temperature suitable for the
production of ammonia, and its bottom may still be in a highly incandescent state
and fully capable of decomposing steam and producing combustible gases. A self-
evident advantage of this is, that, as the ammoniacal gas is evolved, it passes from
the lower through the upper strata of coke, which are sure to be at a temperature
much to low to decompose or injure it.
When the decomposition of the coke contained in the decomposing chamber is
completed it is removed.
It is evident that a seperate chamber may be used for each retort, or that one
chamber may be made to decompose the coke from an entire bench, or even from
several benches of retorts
As it is desirable to maintain the gas at as high a standard of illuminating power
as possible, care must be taken not to introduce the nitrogenous gas into the retort
until the destructive distillation of the coal therein has reached the point at which
the rich hydro-carbon vapors and gases begin to come off in quantities in excess of
the absorbent power of the non-illuminant gases produced, such as hydrogen and
carburetted hydrogen, which generally occurs about half or three quarters of an
hour after charging; and again, the supply of nitrogenous gas should be gradually
reduced when the production of the rich vapors begins to fall off, graduating the
reduction as these disappear, but it is well to continue to supply a small quantity
of the said gas to the end of the distillation, as the charge is then in the best
condition for the production of cyanides.
As has been already stated, any gas rich in nitrogen may be used for the purposes
of this invention but a generator gas is preferable which has been partly deprived.
of its nitrogen in passing through an ammonia furnace because by being partly
deprived of its nitrogen in the first operation the gas is already partly prepared for
use as a diluent for the rich bydro-carbon vapors produced by the destructive
distillation of the coal in the retort.
It is also very desirable that the nitrogenous gas if used should, as far as possible,
be free from watery vapor, carbonic acid, and carbonic oxide, as the first would be
very destructive of the cyanides; the presence of the second fatal to the illuminating
power of the gas; while the last is acknowledged to be a virulent poison which
once mixed with coal gas cannot be removed from it without serious loss
The necessity of excluding carbonic acid gas in any considerable quantity from
the mass of carbon and alkali in the cource of destructive distillation is therefore

page_text: apparent, for, if so present, it will be converted into carbonic oxide by taking up
another equivalent of carbon from the carbon vapor in the retort.
In feeding the pulverulent carbon and alkali into the ammonia furnace, it will
be understood that the reaction between the said materials and the superheated
generator gas introduced into said furnace can only be in fixed chemical proportions
or equivalents. The quantities fed in should therefore in practice approximate the
true combining proportions in order to avoid the accumulation of unchanged
material in the bottom of the furnace. The same kind of coal or carbon, and
alkali, similar to those named as suitable for use in the retort may be used in the
ammonia furnace.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said William Robert Lake in the Patent Office on the 13th May
1884.
"
WILLIAM ROBERT Lake, of the firm of Haseltine, Lake, and Co, Patent Agents,
Southampton Buildings London. "IMPROVEMENTS IN AND RELATING TO THE
MANUFACTURE OF AMMONIA AND HYDROCARBON GASES A communication to me
from abroad by Thomas Burke Fogarty, of Brooklyn, New York, United States of
America.
This invention relates to the production of ammonia and the manufacture of gas,
and comprises improvements in the process described in the specification of former
Letters Patent granted to me and dated February 28th A D 1882 N° 978.
The chief object of the present invention is the production, upon a large scale, of
ammonia from atmospheric nitrogen, by a cheap and simple process, and its
novelty mainly consists in converting the atmospheric nitrogen, discharged with
the hydrocarbon gases and other products of furnace combustion, into ammoniacal
gas, removing the ammonia from the said gases, and then passing the remaining
nitrogeneous gas, deprived of carbonic oxide and carbonic acid, into retorts
containing bituminous coal, mixed with an alkali or alkaline earths, while
undergoing the process of destructive distillation for the generation of illuminating
and heating gas, or either of them, if desired, as hereinafter fully described.
The several parts or sub-processes making up the complete process and the order
in which they are preferably employed may be conveniently described or classified
as follows, that is to say :-
I. The manufacture of a cheap, nitrogeneous, non-illuminant heating gas.
II. The superheating in a suitably constructed apparatus of the said nitrogeneous
gas thereby removing any undecomposed steam therefrom, or removing such steam
by condensing it previous to superheating the gas, or in any suitable manner.
III. The introduction of the said superheated gas, so freed from steam or moisture,
into a suitably constructed furnace, cupola, or retort, wherein it is met by a
falling shower or volume of a mixture of carbon and alkali reduced to a finely
divided or pulverulent state, which mixture is thereby raised to the high
temperature of the gas itself, the nitrogen therein being thus caused to combine
with the carbon and alkali and to form therewith cyanogen or compounds or
derivatives thereof. IV. The decomposition of the cyanogen, its compounds or
derivatives by means of steam, producing thereby ammoniacal and non-illuminant
combustible gases.
V. The separation first of the ammonia from the said gases
and then the carbonic oxide therefrom and also any carbonic acid that may be
generated; and then passing the remaining nitrogeneous gas, consisting mainly of
hydrogen and some free nitrogen into suitably constructed retorts containing
bituminous coal, appropriately mixed with a suitable alkali or alkaline earth;
undergoing destructive distillation, the result being large additional volumes of
ammoniacle and other gases. VI. The treatment of the coke produced in said process
of distillation, with water in a close chamber, for the purpose of decomposing the
cyanides and other compounds of cyanogen therein contained, and thereby
obtaining a further additional yield of ammonia. VII. Mixing ammonia thus
generated and the combustible gases and steam which are invariably produced
with it, with the volumes of illuminating and other gases escaping from the retorts
and subjecting this mixture of gases to any of the approved processes of
condensation, scrubbing and other means of purification usually adopted whereby
the ammonia is collected and separated from the coal gas proper, and may be
treated in any approved manner to obtain it in solid form, if desired.

page_text: It is evident that although the first four sub-processes or steps above mentioned
constitute a complete process of making ammoniacal and non-illuminant combustible
gases, and may be used as an independent process by stopping the operation at
such point and recovering the ammonia in solid form, if desired, by any approved
method; yet, as preliminary steps in one continuous process, they furnish
ammoniacal and non-illuminant combustible gases, which when treated as above
described, furnish a nitrogeneous gas which can be as readily combined with
bituminous coal and alkali in process of destructive distillation for the production
of illuminating gas, where desired, as can atmospheric air or any nitrogeneous gas
derived from any source, with the greater advantage, however, of thereby generating
largely increased volumes of coal gas and at the same time a large additional
volume of ammonia, as hereinafter fully explained.
For the purpose of making more clearly understood the precise manner in which
the manufacture of ammonia may be advantageously combined with the production
of illuminating gas through the destructive distillation of bituminous coal, it is
necessary to advert to some conditions of the coal-gas manufacture which have not
hitherto met with the attention to which their importance entitles them.
In the manufacture of coal gas, as usually conducted, bituminous coal is charged
into suitable retorts set in suitable ovens or furnaces and heated by an external
fire to a high temperature, thus subjecting the coal to destructive distillation, the
products of such distillation being illuminating gas more or less contaminated by
impurities, ammoniacal liquor and tar
As soon as the process of distillation is completed the incandescent coke is
withdrawn from the retorts and that portion of it which is not required for
immediate use as fuel is cooled or quenched in the open air by means of water and
thrown aside until needed for use as fuel. It has been ascertained, however, from
chemical examinations of this coke and of the gases evolved from it during the
process of being cooled by water, as described, that it contains large quantities of
cyanides and that the escaping vapors and gases are highly charged with ammonia
capable of being collected and utilized as a by-product.
It is also well established that the ammonia produced by the destructive
distillation of bituminous coal, and also that obtained during the cooling process
from the cyanides in the coke, is not originally contained in the coal itself but
only the elements required for its production and that it is by the combination of
these elements within the retorts that the ammonia and other products of cyanogen
which are obtained, are formed.
It is likewise known that the illuminating power of coal gas is mainly due to
the rich hydro-carbon vapors which are evolved from the coal during the earlier
periods of distillation, and, that a large percentage of these vapors becomes
condensed or converted into tar in consequence of the gases which are being
evolved not containing non-illuminant gases, such as hydrogen and light carburetted
hydrogen, sufficient to dissolve and retain in suspension the large volume of rich
illuminating vapors evolved at this period of the distillation; so that a great loss
of rich, illuminating material takes place through the want of suitable diluent
capable of absorbing and retaining them in suspension
For these reasons in localities where there are gas-works, it is of great advantage,
to combine the manufacture of ammonia from atmospheric nitrogen with that of
coal gas, for, thereby not only may the yield of ammonia be enormously increased,
but at the same time a still greater increase of rich illuminating gas is produced;
for, the large volumes of non-illuminant gases generated in the preliminary
ammonia process, if introduced into the coal gas retorts at a suitable period of the
distillation and in suitable quantity, furnish exactly what is needed at that time,
an excellent diluent capable of absorbing and retaining in solution the rich hydro-
carbon-vapors which would otherwise go-to form tar, and at the same time,
containing as they do a very large percentage of nitrogen, they furnish material.
which uniting with the carbon and alkali in the retorts produces cyanogen and
cyanides readily convertible into ammonia. -

page_text: While, therefore, for the purposes of this Invention it is not essential to have
recourse to the non-illuminant gas produced in the preliminary ammonia process,
for, any generator gas free from steam and sufficiently free from carbonic oxide
and carbonic acid may be used, yet the non-illuminant gases produced in the
preliminary ammonia process, suitably purified as described, will be found much
superior to ordinary generator gas for the purpose of a diluent, on account of the
percentage of nitrogen therein having been largely reduced by the preliminary
ammonia process.
The coke remaining in the retorts at the end of the distillation will contain a
large percentage of alkaline cyanides which may be converted into ammonia, for
which purpose, instead of withdrawing it from the retorts, and cooling, or
quenching it with water in the open air, as is commonly done, immediately after
withdrawing it from the retorts, it is introduced into a suitably constructed vessel
or chamber, or series of such, wherein it is cooled or quenched by means of steam
or preferably, by throwing upon it a regulated jet or spray of water.
There is an objection to the use of steam for quenching the cyanized coke
because, to be effective, it must necessarily be introduced at the bottom of the
chamber, and if this be done, the ammonia produced will be forced to pass upward
through the superincumbent mass of incandescent coke and will be thereby
decomposed, whereas by using, instead of steam, a jet or spray of water, thrown
upon the top of the mass of incandescent coke, it is cooled from the top downward
so that the ammonia produced will always ascend through a medium having a
temperature lower than that at which it was formed and will therefore be in no
danger of being destroyed as would happen if steam were used.
The coke produced in the ordinary process of making coal gas may be advan-
tageously treated with steam or preferably a jet of water in close chambers, as just
described, with the result of producing an increased yield of ammonia through the
decomposition of the contained cyanides as above described. It is however, at
all times advantageous to further increase the yield of ammonia by supplying
additional volumes of nitrogen from the atmosphere, or other sources, and alkali as
already described
In the accompanying drawing
Figure 1 is a sectional elevation of apparatus for the preliminary generation of
ammonia and
Figure 2 is a sectional view of apparatus for the further generation of ammonia
together with the generation of ordinary bituminous coal-gas
In Figure 1. A indicates a gas generator having a suitable hopper B, an outlet C,
a chimney valve D a furnace door E, a steam pipe F, and an air pipe G.
H indicates the furnace, I the superheater, and J the chimney of an ordinary
Siemen's regenerator furnace
K indicates a gas super-heater suitably connected with an ammonia furnace M,
and the Siemen's superheater I.
In Figure 2. O indicates a gas retort set in an ordinary furnace heated by the
fire P and having the perforated shelf or bottom Q, and provided with the inlet R,
outlet S, and door or cover D²
T, indicates a cooling and decomposing chamber suitably provided with the
cover U, outlet V, water-pipe W, steam-pipe X, and door Y.
The operation of the apparatus is as follows that is to say, The generator A is
suitably charged with coal, coke, charcoal, or other suitable carbonaceous fuel, and
the fuel having being ignited is allowed to burn until it becomes incandescent.
The chimney valve D is now closed, and, by means of a suitable jet, pump, or
aspirator, suitable volumes of air and steam are forced into the closed ash-pit as
shown, by the pipes F and G. As soon as the stream of mingled steam and air
comes in contact with the incandescent fuel in the generator it is forced upward
through the mass, and forms what is known as a generator gas; the hydrogen and
nitrogen of the steam and air, for the most part, passing off unchanged, while their
oxygen combines with the carbon of the coal or other fuel to form carbonic oxide>

page_text: and carbonic acid in proportions which vary according to the relative proportions
of steam and air, the temperature of the furnace, and the greater or less depth of
the mass of incandescent fuel.
The Siemen's superheater I. is connected to the gas superheater K by the pipe L,
and the superheated or incandescent gas from the former is met in the combustion
chamber of the gas superheater K by a current of air, preferably superheated, forced
in through the aperture 1. By this means the gas superheater K and ammonia
furnace M are both raised to a proper temperature. The necessary flow of gas is
established through the openings N and h³, the latter being closed after the gas
super-heater K and furnace M have attained the proper temperature. The opening
at the base of the gas super-heater K, may be connected to the Siemen's
superheater I, or to one of a pair of such superheaters, so that the heated gases of
combustion can at the proper times be returned, through a suitable valve, back
to one of the said pair so arranged as to alternately discharge into the combustion
chamber of one gas-super-heater K. One Siemens super-heater I and one gas
super-beater K will thus be maintained in full operation, while the other end of
each of the said pairs is being revived.
The Siemens regenerator furnace, the gas-super-heater K, and the ammonia
furnace M having been thus previously heated, the generator gas is introduced into
the gas-super-heater K, through the inlet a, whence it passes upward through the
mass of incandescent bricks contained in the super-heater, by which means it is
raised to an intensely high temperature
From the super heater K the generator gas (now highly incandescent), passes
through the flue N into the ammonia furnace M, where it meets with a volume of
carbon and alkali which is fed continuously into the furnace M and at any desired
rate of speed by means of the hopper 6 and the valve or damper C, or other
suitable feeding apparatus.
As the successful operation of the apparatus depends in a very great measure
upon the area of carbonaceous material presented to the action of the gas and upon
a close contact of the solid materials used it is of great importance that the carbon
and alkali should be introduced into the furnace in a finely pulverized or
comminuted state and also in a state of intimate mixture with each other
The highly incandescent generator gas now raises the carbon and alkali to its
own high temperature and, mixed with the falling mass, passes downward through
the furnace, its course being hindered and broken by bafflers or obstructions &
placed in the furnace at frequent intervals. The nitrogen in the gas now combines
with the carbon and alkali to form cyanogen and alkaline cyanides, and these,
mixed with the uncombined carbon and alkali and free gases, continue to pass
downward through the furnace until they meet with a jet of steam admitted
through the pipe e. The effect of the admission of this steam is such that the
temperature of the descending mass of mixed gases and solids is reduced to and is
maintained at any lower point desired, and, at the same time the contained cyanides
are decomposed by the steam, being converted into ammonia, while the solid matter
falls to the bottom of the furnace, where it is received in a pan f containing water,
or in some other suitable receptacle whence it may be removed through the
opening g. suitably sealed by the water in the said pan f. The ammoniacal and
other gaseous products escape from the furnace through the outlet h, and are thence
conducted to suitable condensers and scrubbers where they cooled, and the contained
ammonia separated and collected, either in the form of a carbonate or by the use of
any suitable reagent.
The nitrogeneous gas thus deprived as far as possible of ammonia carbonic oxide,
carbonic acid and watery vapor, is led in any suitable pipe to the entrance R of
the retort-0, and then treated as hereinafter described
It will be seen that in the operation just described there is absolute control not
only of the temperature at which the cyanides are formed but also of that at
which they are decomposed. For the formation of the cyanides there is admitted
through the flue N, an uniform volume of intensely heated gas, and from the
•
.

page_text: feeding apparatus b a regulated volume of mixed carbon and alkali at a low
temperature, the consequence of which is that a stated and uniform equilibrium
of temperature will be maintained in the furnace. In like manner there is supplied
through the pipe e, for the purpose of decomposing the cyanides formed in the
furnace, and which are descending through it at an uniform rate of speed and in
an uniform volume, a regulated volume of steam of uniform pressure and
temperature. The consequence of this is that here again an equilibrium of
temperature will be established, which can be maintained at any desired point by
increasing or diminishing the supply of steam, easily obtained or maintained, at
proper temperature for the purpose. The ability to thus control the temperature
at which the cyanides are decomposed and the ammonia produced is of the highest
importance on account of the liability of ammonia to decomposition by exposure to
an elevated temperature.
As it is of the utmost importance that the generator gas should be introduced
into the ammonia furnace M in as dry a state as possible, it is very often
advantageous to cause it to pass through a suitable condenser previous to its
introduction to the superheater K, for, whatever undecomposed steam it contains
will by this means be almost entirely removed before introducing it to the super
heater K where any undecomposed steam still remaining in it will be taken up and
decomposed by the carbonic oxide of the gas itself, the oxygen of the steam
combining with the carbonic oxide to form carbonic acid, its hydrogen being set
free.
For the purpose of making the operation continuous, instead of intermittent, it is
necessary to use two or more sets of Siemens regenerator furnaces, (as is usual in a
well known process of making steel), and the same number of gas superheaters K.
Should it be desired to combine the process of obtaining ammonia from
mitrogeneous gas, obtained through any other than preliminary ammonia process,
herein before described or derived from any other source, with the production of
coal-gas through the destructive distillation of bituminous coal, such nitrogeneous gas
(but preferably that subjected to the said preliminary ammonia process) however
produced, and freed from steam or watery vapor and carbonic oxide, (at least to a
practical extent) is introduced in a regulated quantity through the inlet R into the
lower chamber o of a retort O, suitably provided with a perforated false bottom Q,
and charged in the usual manner with bituminous coal suitably mixed or
impregnated with lime, soda, potash, or barium, or some other suitable alkali or
alkaline earth, and wherein such alkalized coal is undergoing destructive
distillation for the production-if desired of illuminating gas.
The nitrogeneous gas is now caused to pass through the perforated bottom of the
retort and the superincumbent mass of coal, and to permeate such coal in every
direction, the consequence of which is that the nitrogen in the gas will combine
with the carbon and alkali producing cyanogen and compounds thereof.
Part of the cyanogen thus produced, especially in the earlier period of, the
distillation, is decomposed by the watery vapor in the retort, while by far the
greater portion remains in the coke as a solid cyanide. The gaseous products of
the retort pass out of the pipe S, and are collected in any suitable holder or holders,
after separation of the ammonia, and such purification as is commonly practised in
condensers, scrubbers and the like of ordinary construction.
The coke produced, or at least so much of it as is not immediately transferred to
the furnace as fuel, is passed, with as little exposure to the air as possible into the
decomposing or cooling chamber T, which is immediately closed by the cover U.
By means of the water-pipe W, a regulated jet or spray of water is now thrown
upon the incandescent mass of coke in the chamber T. Some of the water is
decomposed by the incandescent carbon, but the surface of the mass of coke soon
becomes cooled to a point at which it is no longer capable of decomposing the water
or rather the steam produced from it. As the coke cools the steam produced takes
hold of and decomposes the cyanides contained in the coke, every stratum of which
from the top downward becomes successively cooled and reduced to a temperature

page_text: suited to the production of ammonia. The steam is in turn decomposed by the
cyanides present, its hydrogen continuing with the nitrogen of the cyanides to form
ammonia, while its oxygen unites with this carbon to produce carbonic oxide and
carbonic acid, and their alkali is set free or enters into fresh combinations. The
ammoniacal and other gases produced escape from the outlet V, and, after separation
of the ammonia and purification, go to swell the volume of the illuminating gases -
already collected from the retort O in any suitable gas holders, such as are commonly
used in gas works.
It will be readily perceived that in the conversion, within the chamber T, of the
cyanides in the coke into ammonia, the cooling process proceeds from the top
downward through the mass of coke, which, if the operation be carefully conducted,
will be cooled at the top to so low a temperature, as to be incapable even of
producing steam; while its centre may be at a temperature suitable for the
production of ammonia, and its bottom may still be in a highly incandescent state
and fully capable of decomposing steam and producing combustible gases.
self-evident advantage of this is, that as the ammoniacal gas is evolved it passes from
the lower through the upper strata of coke which are sure to be at a temperature
much too low to decompose or injure it.
A
When the decomposition of the coke contained in the decomposing chamber T is
completed, it is removed through the door Y.
It is evident that a separate chamber may be used for each retort, or that one
chamber may be made to decompose the coke from an entire bench, or even from-
several benches of retorts.
As it is desirable to maintain the gas at as high a standard of illuminating
power as possible, care must be taken not to introduce the nitrogeneous gas into the
retort until the destructive distillation of the coal therein has reached the point at
which the rich hydrocarbon vapors and gases begin to come off in quantities in
excess of the absorbent power of the non-illuminant gases produced, such as
bydrogen and carburetted hydrogen, which generally occurs about half or three
quarters of an hour after charging; and again, the supply of nitrogeneous gas should
be gradually reduced when the production of the rich vapors begins to fall off,
graduating the reduction as these disappear, but it is well to continue to supply a
small quantity of the said gas to the end of the distillation, as the charge is then
in the best condition for the production of cyanides.
As has been already stated, any gas rich in nitrogen may be used for the purposes
of this invention but a generator gas is preferable which has been partly deprived.
of its nitrogen in passing through an ammonia furnace such as the furnace M,
Figure 1, already described, because by being partly deprived of its nitrogen in the
first operation the gas is already partly prepared for use as a diluent for the rich
hydro-carbon vapors produced by the destructive distillation of the coal in the
retort O.
It is also very desirable that the nitrogeneous gas if used should, as far as possible
be free from water vapor, carbonic acid, and carbonic oxide, as the first would be
very destructive of the cyanides; the presence of the second fatal to the illuminating
power of the gas; while the last is acknowledged to be a virulent poison which
once mixed with coal gas cannot be removed from it without serious loss.
The necessity of excluding carbonic acid gas in any considerable quantity from
the mass of carbon and alkali in the course of destructive distillation is therefore
apparent, for, if so present, it will be converted into carbonic oxide by taking up
another equivalent of carbon from the carbon vapor in the retort.
In feeding the pulverulent carbon and alkali into the ammonia furnace, it will be
understood that the reaction between. the said materials and the superheated
generator gas introduced into said furnace can only be in fixed chemical proportions
or equivalents. The quantities fed in should therefore in practise approximate the
true combining proportions in order to avoid the accumulation of unchanged
material in the bottom of the furnace. The same kind of coal or carbon, and

page_text: alkali, similar to those named as suitable for use in the retort O, may be used in
the ammonia furnace M.
Having thus fully described the said invention as communicated to me by my
foreign correspondent and the manner of performing the same I wish it understood
that I claim
First The process herein before described of converting nitrogen into ammonia,
consisting in first feeding pulverized carbon and alkali into a current of highly
heated or incandescent nitrogeneous gas within a suitable chamber, thereby
producing cyanogen and alkaline cyanides; then converting said products into
ammonia by means of steam and separating the said ammonia from the remaining
gases; then separating therefrom carbonic oxide and carbonic acid, leaving non-
illuminant nitrogeneous gas; and then passing the said nitrogeneous gas through
heated retorts containing carbon and alkali in course of destructive distillation,
thereby producing more cyanogen and cyanides, for another and large yield of
ammonia, and an increased yield of hydro carbon gases, all substantially as, and for
the purposes, described.
Second In the process herein before described, feeding pulverized carbon and an
alkali into a current or moving volume of incandescent or highly heated nitrogeneous
gas, within a suitable chamber, thereby producing cyanogen and alkali cyanides;
and then decomposing the cyanogen and cyanides so formed by means of steam,
whereby they are converted into ammonia and the temperature at which the
ammonia is formed controlled by the steam which affects said decomposition,
substantially as described.
Third. In the process hereinbefore described, passing nitrogeneous gas through a
mixture of bituminous coal and an alkali, or alkaline earth, while subjected to
destructive distillation in a retort or similar vessel, thereby causing the nitrogen
contained in the said gas to combine with the said carbon and alkali and form
cyanogen and alkaline cyanides, and its non illuminant constituents to serve as
diluents to the rich hydro carbon gases and vapors distilled from said coal and to
absorb and retain them in suspension, substantially as described.
Fourth In the process berein described, passing nitrogeneous gas through
a mixture of bituminous coal and an alkali or alkaline earth, while subjected to
destructive distillation in a retort or similar vessel, thereby causing the nitrogen of
the said gas to combine with the said carbon and alkali and form cyanogen and
alkaline cyanides; and then decomposing the cyanogen and cyanides so formed in
a separate vessel, substantially as, and for the purposes, described.
In witness whereof I the said William Robert Lake have hereunto set my
hand and seal this twelfth day of May in the year of Our Lord one thousand
eight hundred and eighty four.
IXM BORT TAIZE