A Method of and Apparatus for the Continuous Manufacture of Ammonia from Nitrogenous Coke
Year: 1896

page_text: Date of Application, 22nd Dec., 1896
[Communicated from abroad by CARL PIEPER of Berlin in the Empire of Germany
Engineer.]
"A Method of and Apparatus for the Continuous Manufacture of
Ammonia from Nitrogenous Coke."
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
45 Southampton Buildings, in the County of Middlesex, do hereby declare the
nature of this invention to be as follows:-
In a method which has become known of treating nitrogenous substances the
principal part of the nitrogen is transformed into ammonia, by carrying on in
the same retort in which the drying and smouldering of the nitrogenous raw
material takes place, a so called steaming process which consists substantially in
treating the nitrogenous coke freed from all bye-products with superheated steam.
This method of treatment has defects which it is the object of the present
improvement to obviate.
The defects are that in the fractional treatment of the raw material in the
same receptacle (retort) a very considerable reduction of the raw material takes
place in the retort first by the drying and then by the smouldering of the
material, so that on the admission of superheated steam (during the last stage
of the process), which acts upon the coke free from other gasifiable products, the
quantity of the steam is out of proportion to the quantity of the coke to be
treated by it. In addition to this the fresh steam admitted acts in its pure state
only upon a portion of the surface of the nitrogenous coke and even there becomes
mixed with the products of decomposition of the so-called steaming process, thus
the one proposed power of reaction on the largest portion of the surface of the
nitrogenous coke is diminished or entirely lost. In the known process.not only
the coke containing nitrogen but also the coke which is free from nitrogen, that
is to say the total quantity of the coke, has to be kept heated in the retort, a
circumstance which has an injurious influence upon the decomposing material
(steam) and the material to be decomposed (nitrogenous coke) and also
the products of decomposition themselves. This operation diminishes
the yield to be obtained and is the cause of the so-called steaming process of the
known method taking too much time and the process itself being thus rendered
expensive.
By my improvement I obviate these defects as follows, that is to say, I subject
in a special apparatus adapted to be regulated, only so much nitrogenous coke
to the action of the steam (which is definite in quantity and temperature) as can
be decomposed by intimate contact, in order that the final products, that is to
say on the one hand coke alone, and on the other hand ammonia, carbonic acid

page_text: and hydrogen may be obtained in pure mixture and in a perfect state quantitatively
and qualitatively.
The heating chamber for the treatment of the nitrogenous raw material is
furnished with a nozzle for the admission of the superheated steam, and a recep-
tacle in which the nitrogenous coke is raised by a feeding screw or other con-
veyor. The raw material treated on its surface passes with the steam over a
bridge, a part of which may be inclined and enters the precipitating chamber
for the coke free from nitrogen, such chamber extending downwards in the
shape of a funnel. From this chamber the gaseous products obtained in the
process escape through an outlet near the top and the coke which is free from
nitrogen is removed at the bottom of the chamber by a screw conveyor or other
suitable means.
The whole process takes place also in this case with the requisite protection
against any access of air. The conveyor feeding screw transports the raw material
from a chamber continually filled with coke and shut off from the air, and
in like manner the delivery conveyor screw transports the coke free from nitrogen,
if desired continually, to a chamber secured against any access of air. The gases
formed in the precipitating chamber pass through receivers filled with liquid for
obtaining or purifying the gaseous final products.
Such a heating apparatus is placed in a furnace wherein its walls are suitably
heated from the outside, particularly the casing through which the feeding con-
veyor transports the raw material, the bridge and the walls of the precipitating
chamber, the latter to a less degree.
The nozzle through which the superheated steam enters may be constructed
to suitably reduce the velocity of the steam which enters. If desired I may also
employ a conveyor above the bridge, in order that the raw material may never
ol struct the channel. It is expedient to employ such an arrangement in cases
where a very short duration of the contact between the steam and the raw material
is sufficient in order to extract a comparatively small quantity of nitrogen con-
tained in the coke. On the other hand I may place suitable obstructions in the
channel with a view to increasing the duration of contact. The delivery conveyor
screw may be made in two parts and the end nearest the inlet may be of greater
diameter or be caused to turn at a greater speed, and be adapted to operate inde-
pendently of the other part which serves only for transporting purposes and is
provided with a screw or vanes. Such an arrangement has for its object to move
the material dropping over the bridge into the precipitating chamber, either
intermittently or continuously, and to bring the same again in contact with a
fresh superheated steam jet admitted into the chamber by a second nozzle or
pipe. In such a case I prefer to introduce the second steam jet at an appropriate
angle or to distribute the same in a suitable manner by a shield (or a cone) or
the like.
By treating the raw material as it is caused to pass upward in a casing by the
feeding conveyor, I gain advantages as regards the regulation of the working
process. I may however, if desired, effect the admission of the raw material
to the decomposing chamber from above, from one side or even from the front.
Moreover the feed of the coke may of course be effected at the same time by
several screws or other conveyors placed side by side, and a number of steam
nozzles, may be used in this case, which arrangement has only for its object to
enable a greater quantity of material to be treated without the necessity of em-
ploying several funnel shaped precipitating chambers.
Dated this 22nd day of December 1806
HASELTINE, LAKE & Co.
45 Southampton Buildings, London, W.C. Agents for the Applicant.

page_text: "A Method of and Apparatus for the Continuous Manufacture of
Ammonia from Nitrogenous Coke."
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
45 Southampton Buildings, in the County of Middlesex, 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: -
According to a known method of treating nitrogeneous substances the main
portion of the nitrogen is transformed into ammonia by carrying on in the same
retort in which the nitrogeneous raw material is subjected to a drying and
smouldering process, a so-called steaming process, the characteristic feature of
which consists in the fact that the nitrogeneous coke, freed from all byre-products,
is treated with superheated steam.
The nitrogeneous coke herein referred to is an intermediate product obtained
after a process of dry distillation to which the material is subjected for the pur-
pose of driving off from the raw material all gaseous substances in order to
obtain coke proper.
The above mentioned method of operation has certain defects, which it is the
object of the present invention to obviate.
These defects are due to the fact that-in carrying out the fractional treatment
of the raw material in one and the same vessel (retort)-a very considerable
reduction of volume of the raw material is caused in the retort in the first
instance owing to the drying process and subsequently owing to the smouldering
process to which the raw material is subjected, so that, when (during the last
stage of the process) the superheated steam is admitted which is caused to act
upon the coke freed from other gasifiable products, the volume of steam is out
of proportion to the volume of coke subjected to the action of said steam.
further to be noted that the freshly admitted steam will in its pure state act
only upon a portion of the surface of the nitrogeneous coke and there combine
with the products of decomposition resulting from the so-called steaming process,
whereby consequently the only intended reactive power upon the greater portion
of the surface of the nitrogenous coke is either reduced or entirely lost.
It is
Moreover according to the known method, not only the nitrogenous coke but
also the non-nitrogenous exhausted coke that is to say the whole amount of coke
stored in the retort must be kept heated, a fact which causes the decomposing
agent or material (steam) and the material to be decomposed (carburetted nitrogen)
as well as the products of decomposition themselves to be disadvantageously acted
upon. It is owing to this fact that the desired yield is reduced, so that in
applying the so-called steaming process when carrying out the known method,
too long time is required and that the operation itself is rendered considerably
more expensive.
According to the present invention these defects are obviated in such a manner
that in the interior of a special apparatus adapted to be regulated, only such a
quantity of nitrogenous coke is exposed at a time to the action of steam of a
given volume and temperature, as can be decomposed by intimate contact, so
as to completely preserve the final products as regards quantity and quality that
is to say, coke on the one hand, and ammonia, carbonic acid and hydrogen in a
pure mixture on the other hand.
The object of my said invention therefore is to effectively get rid of the exhausted
coke in order to prevent the decomposition of the superheated steam on such coke
and the consequent loss of the power of reaction of the steam upon
the nitrogen
contained in the coke to be acted upon.

page_text: In order that the method of carrying the invention into practice may be clearly
understood I have illustrated the same in the accompanying drawings in which,
Figure 1 is a longitudinal section of the heating chamber for the treatment of
nitrogenous raw material,
Figure 2 is a cross section of the same on the line x, y,
Figure 3 is a longitudinal section of a modified form of the said heating
chamber, and
Figure 4 is a cross section thereof on the line v, 20.
Referring to Figures 1 and 2, D is the nozzle for the admission of superheated
steam; E is a chute or chamber in which the nitrogenous coke is raised by a
suitable elevating device such as for instance a screw S; b is a bridge, over
which the raw material to be acted upon passes along together with the steam;
and is an inclined portion of the bridge designed to remove the residue coke
quicker than on the bridge b; G is a dust and precipitation-chamber for the non-
nitrogenous coke, which chamber as shewn in cross-section Figure 2, is preferably
made hopper shaped and tapering in a downward direction. From this chamber Ğ
the gaseous products obtained by the process are discharged through H whilst
the non-nitrogenous coke is discharged at the bottom of the chamber G by means
of a screw conveyor T, or otherwise.
The whole process takes place with complete exclusion of air. The screw S
conveys the raw material from an air-tight chamber constantly filled with coke,
whilst on the other hand, the screw T transports the exhausted non-nitrogenous
coke, either continuously or intermittently into another air-tight chamber. The
gases, discharged through H pass through receivers filled with liquid, which
feceivers or scrubbers serve for obtaining salts or purifying the gaseous final
products.
A heating apparatus of this kind is located in a furnace, in which its walls
are suitably heated externally, more especially the body, through which the
screw S conveys the raw material, also the bridge and the walls of the
chamber G, the latter, however to a smaller degree. If advantageous I may
introduce a second jet of steam into the apparatus through a suitable noxxle 1
arranged in the wall of the chamber G, so as to thoroughly act a second time
upon the coke not fully exhausted of its nitrogen. If required, I may also employ
a conveyor above the bridge, in order that the raw material may never obstruct
the channel. It is expedient to employ such means in cases where a very short
or exceptionally long duration of the contact between the steam and the raw
material is required in order to extract the whole of the nitrogen contained in
the coke.
A partly modified form of apparatus is shewn in Figures 3 and 4. In this
apparatus the nitrogenous coke is fed from the chamber E into the decomposi-
tion chamber F by means of the screw conveyor S. It then passes down the
incline'b of the bridge where it is acted upon by the current of superheated steam
coming through the nozzle 1) and passing in a direction opposite to that in
which the nitrogenous coke is fed. The exhausted coke then falls to the bottom
of the precipitation chamber G from whence it is conveyed into an air-tight
chamber by means of the conveyor T as described with reference to Figures 1
an 2.
From the foregoing it will be seen that in the form of apparatus shown in
Figures 1 and 2 the steam passes over the coke in the same direction in which
the said coke is travelling whereas in Figures 3 and 4 it passes in the opposite
direction to that in which the nitrogenous material is fed so that the coke, after
having been subjected to the action of the steam, does not come in contact with
steam or with the gaseous products of the process which latter are carried over
the dust collecting chamber I to the discharge conduit H, in the same manner as
described with reference to Figures 1 and 2.
The fact that I cause the raw material to be raised by a screw S in the interior
of a body or chamber of the kind represented in Figure 1 of the drawing has its '

page_text: advantages as regards the practicability of the adjustment. The raw material
may, however, also be supplied to the decomposition chamber F from one side or
even from the front. The coke may, of course, also be simultaneously supplied
through the medium of several adjacent screws or other conveying media, and
several steam admission nozzles may be employed, a modification which solely
serves to allow of larger quantities of material being treated, without the hopper
shaped space G requiring to be materially altered.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, as communicated
to me by my foreign correspondent, I declare that what I claim is:-
1. The hereindescribed process for the treatment of nitrogenous substances for
extracting ammonia therefrom, the characteristic feature of which is that the
raw material, after having undergone the smouldering process, is exposed to a
jet or jets of superheated steam in such quantities that the fresh steam acts
essentially only upon fresh coke, containing nitrogen.
2. An apparatus for carrying the above described process in to practice, in
which the nitrogeneous material is traversed by the current of the superheated
steam which latter together with the gaseous products created passes through a
dust collecting chamber into a scrubber or purifier while the exhausted nitro-
genous material is precipitated in the dust-collecting chamber and is removed
therefrom by a conveyor substantially as described with reference to Figures 1
and 2 of the drawings.
3. An apparatus for treating nitrogenous substances for the extraction of
ammonia therefrom, consisting of an inlet pipe for the introduction of the super-
heated steam into the apparatus, a chute or chamber provided with elevating
screw for introducing the raw material into the decomposition chamber, a bridge
in the said chamber on which the raw material is subjected to the action of the
stram and a precipitating chamber for receiving the dust and the exhausted
material from said bridge and over which the steam together with the gaseous
prcducts from the raw material passes on its way to the collecting or purifying
chamber, the said precipitating chamber having by preference a screw conveyor
arranged at its bottom for the purpose of removing the said exhausted material,
substantially as set forth.
4. A partly modified form of apparatus for treating nitrogenous material for
the extraction of ammonia therefrom in which the feed chute is arranged to
introduce the raw material from the top onto an inclined bridge, a steam nozzle
opposite the said bridge so arranged that the steam passes in an opposite direction
to the raw material from the chute, a precipitating chamber and discharge screw
for the exhausted material below the feed chute and steam nozzle, a dust col-
lecting chamber and an outlet for the gaseous products substantially as set forth
with reference to Figures 3 and 4 of the drawings.
D: 001 d. of Cantambo 1907
HASELTINE, LAKE & Co.
45 Southampton Buildings, London, W.C. Agents for the Applicant.