Improvements in the Process for Treating Gas Liquor and other Ammoniacal Liquors.
Year: 1887

page_text: Date of Application, 3rd Aug., 1887
Complete Left, 26th Apr., 1888
Complete Accepted, 1st June, 1888
Improvements in the Process for Treating Gas Liquor and other
Ammoniacal Liquors.
I, ERNST GRAHN of 28 Mainzer Chaussee, Coblentz, Prussia, in the Empire of
Germany, Civil Engineer do hereby declare the nature of this invention to be as
follows:-
The methods hitherto in use of manufacturing ammonia compounds, consist in
separating the ammonia, which in a free condition or in the form of volatile salts is
contained in the liquors to be worked, by heating and vaporizing a part of the liquor,
in then leading away the ammonia which is mixed with steam, and in condensing the
same thereupon by suitable absorbents. According to the process hereinafter
described the ammonia or the volatile ammoniacal salts are turned out by means of
a current of air or gas whilst heating or not the liquor at the same time, and the
air charged with ammoniacal vapours is set free from its contents of ammonia by
suitable absorbents.
In passing a finely divided current of gas (air or smoke gases and the like) through
the ammonia containing liquor, the volatile ammonia compounds pass by diffusion
into the gas, and a complete separation of the ammonia without a partial vaporization
of the solution is thereby obtained. The current of air charged with ammonia or
volatile ammoniacal salts is placed in contact according to the ammonia compounds to
be produced, with solid, liquid or gaseous absorbents.
By using a current of air or gas to conduct the ammonia from the liquor to be
worked into the absorbent, not only the separation of the ammonia is facilitated and
more completely than by the method heretofore in use of boiling, but also the
stoppages produced by the condensation of the volatile ammoniacal salts and the
separation of the condensing water, by which a part of the ammonia which has been
distilled off is either conducted again into the distilling vessel or introduced into
the absorbent, are thereby avoided.
In the new process the air charged with ammoniacal vapors may directly be
introduced into the absorbing apparatus and according to the absorbent, which is used,
solid and dry ammonia-compounds or any other solutions and mixtures may directly
be obtained.

page_text: In order to explain the new method by an example; I will describe the process by
which gas liquor is worked, according to my invention, into phosphate of ammonia or
ammonia-phosphate of calcium or into artificial nitrogenous manure.
The gas liquor which is to be worked, flows into the upper part of a vessel which
in a similar manner as the ordinary column-apparatus used in the distillation of gas
liquor or in the rectification of spirit, is divided by a certain number of intermediate
bottoms into several compartments, over which the liquid flows down. Into the
lowest compartiment of the vessel, in which the liquid driven off is gathered, a finely
divided current of air is thrown in, which may be heated to a more or less high
degree by steam (for instance by means of a steam jet blowing engine). The current
of air taking up the ammonia from the liquor flows upward through the several
compartments of the column, and is thereby being continually distributed afresh into
the liquor which flows down. In this way the current of air is cooled more and more
whilst losing thereby its water vapor and becomes enriched in ammoniacal vapors
owing to its contact with more and more concentrated solutions. The upper part of
the column apparatus, into which the gas liquor flows in a continuous stream, acts
therefore as a cooler and condenser.
1. The liquid freed from ammonia escapes continuously from the lower part of the
apparatus.
2. In order to free the ammonia which is bound to fixed salts lime milk is added
to the solution before the latter flows out of the apparatus.
The dimensions of the apparatus and the number of the compartments arranged
one above the other and over which the ammoniacal liquor flows down and continually
comes afresh in contact with the air, are dependent upon the ammoniacal standard
of the liquid.
The intimate contact of the air and the liquor may also be effected by causing
the latter to flow downward in vessels filled with coke or other material, while a
current of air is blown from below upward.
The quantity of the air blown into the vessels and the heating of the liquor are
so calculated that on one side the water flowing off is completely freed from ammonia,
and that on the other side, the escaping current of gas which is charged with
ammoniacal vapors has nearly the temperature of the entering gas-liquor. In
. particular cases the complete cooling of the current of gas may be effected by a special
condenser.
To produce ammoniacal salts, the current of gas charged with ammoniacal vapors
may be placed in direct contact with the usual absorbents.
In order to produce directly artificial ammonia-manure, the current of gas
containing the ammonia is introduced into vessels, which are similar to the purifying
boxes of gas works. The absorbent, having for its purpose to enrich in nitrogen,
such as superphosphate, double phosphate, dissolved guano, is spread in these boxes
over hurdles. In passing through the acid absorbent, spread in layers of moderate
height, the whole of ammonia is separated from the current of gas and a dry
nitrogenous manure is directly obtained.
The advantages of the above described method consist therefore on the one hand
in the easier and more complete separation of the ammonia from liquors by means of
a current of gas without partially distilling the liquor, that is to say in the saving
of combustibles, and on the other hand of the possibility of directly producing dry
nitrogenous manures.
The production of sulphate of ammonia is therefore avoided and the sulphuric
acid, the presence of which is prejudicial in the manufacture of artificial manure,
is thereby prevented and the ammonia directly obtained in the form of phosphate of
ammonia and in chemical mixture with the manure.
D
T
.
e
1000
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool,
Agents for the Applicant.

page_text: Ammoniacal Liquors.
I, ERNST GRAHN, of 28 Mainzer Chaussee, Coblentz, Prussia, in the Empire of
Germany, Civil Engineer, 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 methods hitherto in use of manufacturing ammonia compounds, consist in
separating the ammonia, which in a free condition or in the form of volatile salts is
contained in the liquors to be worked, by heating and vaporizing a part of the liquor,
in leading then away the ammonia which is mixed with steam, and in condensing the
same thereupon by suitable absorbents. According to the process hereinafter
described, the ammonia or the volatile ammoniacal salts are turned out by means of a
current of air or gas whilst heating or not, the liquor at the same time, and the air
charged with ammoniacal vapors is set free from its contents of ammonia by suitable
absorbents.
In passing a finely divided current of gas (air or smoke-gases and the like)
through the ammonia containing liquor the volatile ammonia compounds pass by
diffusion into the gas and a complete separation of the ammonia without a partial
vaporization of the solution is thereby obtained. The current of air charged with
ammonia or volatile ammoniacal salts is placed in contact according to the ammonia
compounds to be produced, with solid liquid or gaseous absorbents.
By using a current of air or gas to conduct the ammonia from the liquor to be
worked into the absorbent, not only the separation of the ammonia is facilitated and
more completely than by the method heretofore in use, of boiling, but also the
stoppages produced by the condensation of the volatile ammoniacal salts and the
separation of the condensing water, by which a part of the ammonia, which has been
distilled off, is either conducted again into the distilling vessel or introduced into
the absorbent, are hereby avoided.
In the new process, the air charged with ammoniacal vapors may directly be
introduced into the absorbing apparatus, and according to the absorbent, which is
used, solid and dry ammonia compounds or any other solutions and mixtures may
directly be obtained.
In order to explain the new method by an example, I will describe the process by
which gas liquor is worked, according to my invention into phosphate of ammonia or
ammonia-phosphate of calcium, or into artificial nitrogenous manure.
The gas liquor, which is to be worked, flows into the upper part of a vessel, which
in a similar manner as the ordinary column-apparatus used in the distillation of gas-liquor,
or in the rectification of spirit, is divided by a certain number of intermediate bottoms
into several compartments, over which the liquid flows down. Into the lowest compart-
ment of the vessel, in which the liquid driven off is gathered, a finely divided current of air
is thrown in, which may be heated to a more or less high degree by steam (for instance
by means of a steam jet blowing engine). The current of air taking up the ammonia

page_text: from the liquor flows upward through the several compartments of the column, and is
thereby being continually distributed afresh into the liquor, which flows down. In this
way the current of air is cooled more and more, whilst losing thereby its water vapor,
and becomes enriched in ammoniacal vapors owing to its contact with more and more
concentrated solutions. The upper part of the column apparatus, into which the
gas liquor flows in a continuous stream, acts therefore as a cooler and condenser.
1. The liquid freed from ammonia escapes continuously from the lower part of the
apparatus.
2. In order to free the ammonia, which is bound to fixed salts, lime-milk is added
to the solution before the latter flows out of the apparatus.
The dimensions of the apparatus and the number of the compartments arranged one
above the other and over which the ammoniacal liquor flows down, and continually
comes afresh in contact with the air, are dependent upon the ammoniacal standard
of the liquid.
The intimate contact of the air and the liquor may also be effected by causing the
latter to flow downward in vessels filled with coke or other material, while a current
of air is blown from below upward.
The quantity of the air blown into the vessels and the heating of the liquor are so
calculated, that on one side the water flowing off is completely freed from ammonia, and
that on the other side, the escaping current of gas which is charged with ammoniacal
vapors, has nearly the temperature of the entering gas liquor. In particular cases the
completo cooling of the current of gas may be effected by a special condenser.
To produce ammoniacal salts, the current of gas charged with ammoniacal vapors
may be placed in direct contact with the usual absorbents.
In order to produce directly artificial ammonia-manure, the current of gas containing
ammonia as introduced into vessels, which are similar to the purifying boxes of gas
works. The absorbent having for its purpose to enrich in nitrogen, such as super-
phosphate, double phospate, dissolved guano, is spread in these boxes over hurdles.
In passing through the acid absorbent spread in layers of moderate height, the whole
of ammonia is separated from the current of gas and a dry nitrogenous manure is
directly obtained.
The advantages of the above described method, consist, therefore, on the one hand,
in the easier and more complete separation of the ammonia from liquors, by means
of a current of gas without partially distilling the liquor, that is to say, in the saving
of combustibles, and on the other hand, of the possibility of directly producing dry
nitrogenous manures.
The production of sulphate of ammonia is therefore avoided, and the sulphuric acid,
the presence of which is prejudicial in the manufacture of artificial manure, is thereby
prevented, and the ammonia directly obtained in the form of phosphate of aminonia,
and in chemical mixture with the manure.
Having now particularly described and ascertained the nature of my said Inven-
tion and in what manner the same is to be performed, I declare that what I
claim is:-
The treatment of gas liquor and other ammoniacal liquors with a current of gas
(air smoke etc.) in order to separate ammonia or volatile ammonia compounds
for the purpose of directly manufacturing nitrogenous manures, substantially as set
forth.
WM. P. THOMPSON & Co.,
6, Lord Street, Liverpool,
Filing Agents for the Applicant.