Improvements in and relating to the Manufacture of Ammonia and By-products.
Year: 1894

page_text: Date of Application, 16th Nov., 1894
Complete Specification Left, 23rd Aug., 1895-Accepted, 28th Sept., 1895
[Communicated from abroad by CARL PIEPER, of 3 Hindersinstrasse, Berlin,
N.W. 40, Civil Engineer, and CHRISTIAN FELLNER, of 8 Seilerstrasse,
Frankfort-on-the-Main, Civil Engineer, both in the. Empire of Germany.]
Improvements in and relating to the Manufacture of Ammonia
and By-products.
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:-
My invention relates to the manufacture of ammonia from nitrogenous organic
materials, especially from peat, and has for its object to obtain substantially
the entire quantity of nitrogen in the form of ammonia while leaving behind as
far as practicable the carbon contained therein and obtaining gases of great caloric
value.
I avail myself of the well-known facts that nitrogenous substances, when treated
with water-vapour under the action of an elevated temperature, will develop
ammonia, and that, on subsequently coking such substances in a suitable manner,
almost their entire amount of nitrogen remaining will be found in the coke, and,
my invention consists in effecting the treatment of the coke under such conditions
as will always ensure more heat being absorbed than generated in the apparatus
by the process, there being thus no tendency towards an increase of temperature in
the apparatus.
This mode of operation is based upon the discovery which I have made, that
from peat and similar nitrogenous material, nitrogen can be amply developed at a
temperature remaining below that at which water-vapour is decomposed by carbon,
so that the temperature at which such a decomposition takes place is always
sufficient for obtaining all the nitrogen in the form of ammonia. Owing to the
consequences of this discovery, the manufacture of ammonia especially from peat,
if properly carried out, possesses great industrial value.
According to my said invention the coke obtained by smouldering or roasting
the nitrogenous organic material, for instance peat, is treated with water-vapour
appropriately superheated, while excluding all access of air, in an apparatus that
acts similarly to a retort, the process being carried on at such a temperature as is
necessary for effecting the decomposition of the carbon. By reason of the
disengagement of hydrogen more heat is absorbed than is produced by the oxidation
of the carbon, and I endeavour to maintain the difference as great as possible by
causing the oxidation of the carbon to form carbonic oxide by the introduction of
only an appropriate quantity of water-vapour. The addition of heat which becomes
necessary in order to keep the temperature of the apparatus at a suitable height
for the continuance of the reaction between the water-vapour and carbon, is
effected by heating the contents of the apparatus from the outside through the
walls of the apparatus.
I am in this way enabled to continually control and regulate the temperature sp
that there will be no heat applied which is injurious to the ammonia produced by.
the process, and I create no danger of explosion from the presence of gases at a
high tension and avoid the formation of oxyhydrogen gas "knallgas” as well as

page_text: the production of a large quantity of gas of but comparatively little caloric value.
The process will absorb but little more carbon than is required for the reaction,
and I obtain this carbon back in the form of gas having high caloric value, it being
only mixed with hydrogen, while the remainder of the carbon is left in the solid
form as a material adaptable for the manufacture of fuel blocks.
Dated this 16th day of November 1894.
HASELTINE, LAKE & Co.,
45 Southampton Buildings, London, W.C., Agents for the Applicant.
Improvements in and relating to the Manufacture of Ammonia
and By-products.
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 :-
The object of my invention may shortly be described as a method of obtaining
practically all the nitrogen contained in nitrogenous substances, such as peat, in
the form of ammonia, along with the most valuable by-products in one continuous
process from the same distilling apparatus, recovering at the end the coke of the
raw-material used.
It has heretofore been attempted to obtain ammonia from nitrogenous materials
by first extracting the volatile products thereof and then treating the coke-residues
with air, or a mixture of air and steam, in order to gain the nitrogen contained in
the coke.
Another process consisted in "burning" (decomposing) the whole of the
nitrogenous material in superheated steam, neglecting thereby the direct pro-
duction of valuable by-products and losing also a considerable amount of the
ammonia obtainable.
These methods necessitate the employment of temperatures so high as to destroy
a great part of the products that can be gained, and they have therefore proved
unfit to be turned to account for manufacturing or commercial purposes.
The task of my new invention has been:
First, to avoid temperatures capable of decomposing the ammonia, and
Secondly, to obtain in one continuous operation not only the ammonia and gases
valuable as heat generators, but also the tar, coke and other useful component
elements of the raw-material.
The process which I use, has three stages, i.e. drying, distilling and vapourizing,
and I so conduct the whole process that the generation of heat within the apparatus
(vessel or retort), is avoided. The well-known distilling process is included in the
cycle of operations, because by means of it up to about 30% of the nitrogen
contained in the raw-material may be extracted together with other volatile matter,
such as tar, methyl-alcohol, acetone, acetates etc. At the end of the distilling
process there remains practically nothing but coke in the apparatus. This coke
contains the greater part of the nitrogen.
In producing nitrogen from this coke, no air must be admitted, as the temperature
at which the carbon of the raw-material would be burned, is so high, that it would
decompose ammonia. I also make special use of the fact that in decomposing
water (during the vapourizing process) one ninth of its weight is separated in the
form of hydrogen, by which means heat is absorbed at the rate of, say, 34000 units
per kilogramme of hydrogen. Again the oxygen set free by the decomposition of
the water, serves to burn carbon to carbouic acid. This carbon represents about

page_text: thrice the weight of the freed hydrogen and its oxidation evolves approximately
25000 units of heat. In this way a cooling effect is produced within the apparatus,
which must be counteracted by appropriately admitting heat from the outside, if the
operation is to be kept up.
As the decomposition of the water, by the carbon, takes place at a temperature
which is not sufficient to decompose the ammonia, the temperature of the apparatus
(vessel or retort) may be maintained at a correspondingly low degree, without
jeopardizing the final result.
In the case of peat coke, for example, the proper working conditions are met
with at an incipient-red heat of a cast iron vessel or retort.
I will now describe my invention as applied more particularly to peat or turf.
The air-dried peat is broken up into pieces and placed in a retort which may be
revolving. The retort is heated from the outside to drive off the moisture still
retained by the peat. The heat within the retort, will not rise much beyond
100° Centigrade so long as water evaporates from the raw-material. The finish of
the drying process may be observed either by the rising of the temperature at the
outlet from the retort, or by the fact, that the gas, which escapes from a test-valve
or cock, becomes inflammable.
The heating of the retort is now continued in order to gain all the products of
distillation.
The distilling process is completed, as far as it is required to be for the purposes
of the invention, when the main bulk of the tar has been extracted, a stage which
may be ascertained by analyzing the gas from time to time. For the purposes of
ordinary practice, the discontinuance of the production of inflammable gas is a
sufficiently reliable sign, that such stage has been reached.
I now proceed to heat the apparatus, from the outside, more vigorously during
the vapourizing process and admit steam, appropriately superheated, into the retort
in which practically nothing but coke is contained. The steam as it comes into
contact with the coke decomposes into oxygen and hydrogen. The oxygen, by
combining with carbon, yields carbonic acid, while part of the hydrogen combines
with the nascent nitrogen (resulting from the decomposition of the coke which
contains it) into ammonia. The remainder of the hydrogen and the ammonia
obtained, is let into sulphuric or other suitable acid, which will retain the
ammonia, whilst the hydrogen separates and may be utilized as fuel for heating
the retort.
The proper temperature at which the vapourizing process is carried on, is secured
by regulating the heat applied to the outside of the retort, or by the quantity or
temperature of superheated steam introduced therein.
After the separation of the nitrogen from the coke, the process is complete;
the remaining coke is discharged from the vessel or retort, and a fresh charge
of material is introduced, to undergo the same cycle of operations as before.
The discharged coke is suitable for the manufacture of fuel in blocks such as
briquettes.'
66
Practical experiments have shown that the same method is well applicable to
other bodies containing nitrogen, with only such alterations as the varying
by-products in each case may require.
I am aware that in known methods of manufacture, ammonia, tar and gaseous
by-products have been obtained the latter being of comparatively little calorific
value. I do not therefore claim generally the production of such substances by the
distillation of nitrogenous materials, but I declare that I claim :-
1. The hereindescribed process of obtaining in one continuous operation from
nitrogenous substances especially turf and peat (1) the products of distillation
(2) ammonia (3) gases of considerable calorific value (4) coke, such process
being specially characterized by the entire exclusion of air and the prevention of
the generation of heat within the vessel containing the materials operated upon.
2. In a process for obtaining ammonia from nitrogenous substances especially

page_text: turf and peat, excluding the air entirely during the application of the steam to the
heated materials and conducting such operation at a low temperature and so that
no heat is generated within the vessel containing the substances operated upon,
substantially as described.
3. In processes such as are claimed in the two preceding claims regulating the
temperature during the vapourizing operation by varying the quantity or
temperature of the steam admitted, substantially as described.
Dated this 22nd day of August 1895.
HASELTINE, LAKE & Co.,
45 Southampton Buildings, London, W.C., Agents for the Applicant.