A Process and Apparatus for the Manufacture of Ammonia.
Year: 1890

page_text: Date of Application, 9th May, 1890
Complete Specification Left, 7th Feb., 1891-Accepted, 9th May, 1891
PROVISIONAL SPECIFICATION.
A Process and Apparatus for the Manufacture of Ammonia.
We, HENRY BAUDOUIN and PIERRE FERDINAND ESCARPIT both of No. 23
Boulevard de Strasbourg, Paris, France do hereby declare the nature of this
invention to be as follows:-
This invention relates to the manufacture of ammonia by subjecting a mixture of
nitrate of soda and a hydrocarbon such as naphthaline to decomposition by heat.
At a temperature of about 600° C. the oxygen of the nitric acid and the carbon
of the hydrocarbon form carbon dioxide which combines with the soda forming
carbonate of soda, while the nitrogen of the nitric acid and the hydrogen of the
hydrocarbon combine forming ammonia.
The reaction is effected in an inclined retort within which is a travelling chain
scraping the bottom. The thorough mixture of nitrate of soda and hydrocarbon
is introduced by a branch pipe at the upper end of the retort the ammonia gas
ascends by a branch pipe extending upwards from the lower end, and the carbonate
of soda descends by a branch pipe extending downwards from the lower end. The
ammonia gas is collected on lime which takes up the water and carbon dioxide not
absorbed by the soda.
Dated this 9th day of May 1890.
ABEL & IMRAY,
Agents for the Applicants.
COMPLETE SPECIFICATION.
A Process and Apparatus for the Manufacture of Ammonia.
We, HENRY BAUDOUIN, and PIERRE FERDINAND ESCARPIT, of 23 Boulevard
de Strasbourg, Paris in the Republic of France, Manufacturing Chemists 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 subject of this invention is an improved process of manufacture of ammonia,
based upon the principle that carbon and nascent hydrogen if brought into contact
with nitrate of soda at a suitable temperature, decompose and generate ammonia
from the resulting carbonate of soda and carbonic acid.
To attain this result, a mixture of nitrate and of any suitable hydrocarbon is
decomposed in a closed vessel at a temperature of from 800 to 900° Centigrade.
Any desirable hydrocarbon such as found in the trade may be employed for the
purpose say naphthaline, tar, heavy oils and the like; also coal which being
distilled at a given temperature will give off nascent hydro-carbons capable of
bringing about the desired re-action some of which may be described as follows:-
With the coal may be mixed 100 kilogrammes of nitrate of soda and 125 kilo-
grammes of a suitable hydrocarbon (the weight indicated ris.-125 kil. is the
average, which however may vary according to its richness in bydrogen). At a
given temperature the coal is decomposed into carbon and hydrogen, which latter
acts upon the nitrate of soda, and in its turn decomposes it. making ammonia with
the nitrogen, while liberating the oxygen and oxide of sodium.
In this re-action owing to an excess of carbonic acid, there forms carbonate of
ammonia and an important condition is that the coal used should be perfectly dry.

page_text: The result of this operation is 18 kilogrammes of ammonin gas or 95 kilog, of
liquid ammonia at 22" 175 kilog, of crystallised carbonate of soda (known in the
trade as sola crystals) at 33° Deeroizilles; 19 or 20 per cent, of oxide of sodium
(Na, 0); 50 kilog, of coke, and a quantity of heavy oils which quantity varios
between 5-7 kilog.
When naphthaline is used (in a retort-shaped apparatus brought to nascent red-
heat, about 600°) a mixture is made of 100 kilog. of nitrate of son and 45 kilog.
of naplahaline. Naphthaline (CH) at this temperature decomposes into carbon
and hydrogen which latter acting in its unscent state upon the nitrate is in its turn
decomposed, thus Na O, Az O̟, the hydrogen by absorbing the nitrogen, generating
ammonia and a small amount of water, while the earlon acts upon the Oxygen
the nitrate and converts it into carbonic acid, which latter combines with the
liberated soda, greedily absorbing such carbonic acid and thus producing carbonate
of soda.
1
of
The water is also decomposed at this temperature (1, 0) into hydrogen and
oxygen which latter in its turn supplies carbonic acid for the production of
carbonate of ammonia.
To free the ammonia from the carbonic neid it contains the gas is collected in
an ordinary washing apparatus where it is treated with lime. In this manner
100 kilog. of nitrate of soda will yield 90 kilogs, of ammonia at 22°, 185 kilog, of
crystals of sola (NaO), CO₂) plus 10 equivalents of water.
Suitable apparatus for carrying out these dillerent decompositions in practice, is
shown in the accompanying drawings though it will of course be understood that
the same results may be obtained by other apparatus of a similar description.
The apparatus consists of a cast-iron still or retort A arranged in an inclined
position to facilitate the descent of the carbonate of soda and internally provided
with a pitch chain adapted to prevent obstruction.
The still or retort is preferably about two metres long and has an internal
diameter of about 40 centimetre-, It is provided with a valve and with a receiver
for the carbonate of soda.
The feeding apparatus II consists of a metal hopper of a capacity of about
1000 kilog. After being filled the hopper I is closed and it is internally provided
with a screw or conveyor somewhat similar to that used in coffee-mills which is
operated by suitable machinery to regulate the supply of the material to be
converted into ammouin.
B is a structure of masonry. Ca furnace about 70 centimetres long and
30 centimetres wide. D D are the end-plates or covers of the retort or still.
EE are the pulleys or wheels whereby the pitch-chain is moved the front wheel
being mounted on a shaft passing through the wall of the retort and the masonry,
and carrying on its projecting end another pulley for the reception of the driving
strap or equivalent: suitable packing preferably asbestos is applied to the joints to
prevent escape of gas.
E is a dome or chamber of an internal diameter of preferably about 20 centi-
metres and having walls say 20 mm. thick surmounted by a plug or valve luted to it by
means of clay or the equivalent.
Gis a pipe or shoot commecting the hopper H containing the mixture to be
treated with the retort.
His the hopper of a capacity of preferably about 1000 kilog.
I is the orifice
for the introduction of the material and is the shaft whereon the helical
conveying arrangement is mounted by which the uniform descent of the mixture to
be treated is ensured.
Jis a metal reservoir for the reception of the carbonate of soda and coke.
K is a cylinder for receiving the heavy oils and substances capable of condensation.
Lis the washing apparatus." M the outlet for the ammonin-gas. N is a gange.
O is a preferably cast-iron pipe. P is the furnace chimney, and R is the discharge
cock.

page_text: Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed, we declare that what
we claim is :—
1. The production of ammonia based upon the reduction of nitrates of soda by
means of hydrocarbons carbonate of soda being obtained as a bye-product.
2. The apparatus substantially as herein described whereby the process of
reduction theoretically set forth above is carried out in practice.
3. In apparatus for the production of ammonia from nitrate of soda the
combination with a retort and pitch chain and wheels within it of a hopper having
a conveyor or agitator within it and a shoot connecting the hopper to the retort a
carbonate of soda and coke reservoir a vessel for receiving the heavy oil and
substances capable of condensation and a gas washing apparatus substantially as
herein described.
Dated this Sixth day of February 1891.
W. P. THOMPSON & BOULT,
Agents for the Applicants.