IMPROVEMENTS IN THE MANUFACTURE OF SULPHATE OF AMMONIA, AND IN APPARATUS THEREFOR."
Year: 1878

page_text: LETTERS PATENT to Roger William Wallace, of Mark Lane, in the County of
Middlesex, for the Invention of "IMPROVEMENTS IN THE MANUFACTURE OF
SULPHATE OF AMMONIA, AND IN APPARATUS THEREFOR."
PROVISIONAL SPECIFICATION left by the said Roger William Wallace at the
Office of the Commissioners of Patents on the 19th September 1878.
ROGER WILLIAM WALLACE, of Mark Lane, in the County of Middlesex. "IM-
PROVEMENTS IN THE MANUFACTURE OF SULPHATE OF AMMONIA, AND IN APPARATUS
THEREFOR."
0
This Invention relates to improvements in the manufacture of sulphate of
ammonia, and in apparatus therefor, by means of which improvements à smaller
plant and less fuel are required, while at the same time a larger proportion of
the said sulphate is obtained from the crude ainmoniacal liquor. than by any
process heretofore practised, and at the same time the sulphuretted hydrogen
evolved during the process is utilized for the same, and then disposed of without
difficulty.
In carrying the said Invention into practice I provide a tank, which is preferably
placed below the surface of the earth, this tank serving to contain the crude
ammoniacial liquor which is pumped up to a tower through a suitable pipe, the said
liquor passing in its course through a series of sulphuretted hydrogen condensers,
by which it is heated to a certain temperature. As this liquor descends within the
said tower steam at a high pressure is admitted at the bottom by a pipe leading
from steam boilers forming part of the apparatus, thereby causing the crude liquor
to give off nearly the whole of the free aminonia gas, which consists of carbonate
and sulphide of ammonia, which then passes off to saturators through a suitable
pipe. The remaining liquor is then carried by means of a pipe provided at the
lower part of the tower to one or more blowers or tanks, to which steam is admitted
by a branch pipe leading from another pipe connected with the boilers. From these
Duine G21

page_text: tanks this liquor is blown into the ordinary steam boilers through a connecting
pipe, where the remainder of the free ammonia above described is eliminated, from
which boilers the gas liquor is afterwards blown off through another pipe to a tank
containing lime, which is agitated by means of a perforated pipe connected with the
said steam boilers, the fixed ammonia or sulpho-cyanide of ammonia left in the
liquor is here eliminated, and is taken back to the tower through a pipe provided
for the purpose, which pipe also serves as an overflow pipe to prevent the tower
from becoming too full, if there should be any obstruction in the pipe at 'the bottom
thereof, when, as before described, it is taken away to a saturator or saturators, in
which by being combined with sulphuric acid it becomes sulphate of ammonia.
The sulphuretted hydrogen generated in the said saturators is passed through
the aforesaid condensers, which are constructed of wrought iron, and are provided
with a number of small tubes arranged vertically. Within the surrounding space
there is a continual flow of the crude ammoniacal liquor passing from the crude
liquor tank to the tower. This liquor condenses, and at the same time, is heated
by the sulphuretted hydrogen passing through the vertical tubes from whence the
uncondensed sulphuretted hydrogen is conveyed to the boiler furnaces to be burnt,
or being ignited in a fire clay retort to the acid chambers, where it is utilized for
the formation of sulphuric acid. The spent lime in the agitating tank is blown off
through pipes to a series of precipitating tanks.
I construct the tower of square cast or wrought iron plates, but preferably of
cast iron, and I provide within the same a series of angle iron bars arranged in
tiers, each tier crossing the other alternately at right angles. Previous to the
descent of the liquor down the tower it enters a wrought-iron tumbling box
having a division in the centre, thus forming two compartments; this box oscillates
upon an axle having its bearings in the side plates at the top of the tower; one
edge or side of this box rests upon the angle iron bars at such an angle that the
other part will be in a position to receive the entering liquor until when sufficient
thereof has entered it will descend by the weight of the liquor, and fall over to the
opposite side, discharging the liquor when the other side of the box thus comes into
position to receive the entering liquor, and when full enough will fall over on the
other side; this motion takes place alternately from side to side, thus distributing
the liquor equally over the entire area of the top tier of angle bars, thereby causing
the liquor to drip evenly through each opening between the bars to the bottom of
the still.
It will be understood that I may employ a series comprising any number of the
apparatuses above described as may be desirable, according to circumstances.
According to another part of my said Invention for the manufacture of sulphate
of ammonia I dispense with a considerable portion of the apparatus above described,
and proceed as follows, that is to say :-
I place within the tank containing the crude ammoniacal liquor a pipe, which is
connected with an air pump, or with a gas exhauster worked by a steam engine, or
in any other suitable manner. This air pump or exhauster exhausts the air from
the tank, and the liquor evaporates, giving off the free ammonia gas, which is led
by a suitable pipe direct to the saturator, where it is treated in the usual manner.
If necessary the liquor may be heated by steam passing through a coiled pipe or
otherwise to ensure the evaporation of the ammonia.
The fixed ammonia is then
eliminated, agitating with lime in the usual manner.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said Roger William Wallace in the Great Seal Patent Office on the 19th
March 1879.
ROGER WILLIAM WALLACE, of Mark Lane, in the County of Middlesex. "Iм-
PROVEMENTS IN THE MANUFACTURE OF SULPHATE OF AMMONIA, AND IN APPARATUS
THEREFOR."
This Invention relates to improvements in the manufacture of sulphate of
ammonia, and in apparatus therefor, by means of which improvements a smaller
plant and less fuel will be required, while a larger proportion of the said sulphate
can be obtained from the crude ammoniacal liquor than by any process heretofore
practised, and no water will be required, moreover, the residual liquor being highly
concentrated permits the cyanides and other products therein to be very con-
veniently eliminated.
For carrying the said Invention into practice I provide apparatus as shewn in
the accompanying Drawings, in which,
Figure 1 is a plan, and,
Figure 2, a side elevation of the said apparatus.
Figure 3 is an elevation partly in section, and drawn to an enlarged scale of a
portion of the same.
Figure 4 is a plan, and,
Figure 5, a side elevation partly in longitudinal section, illustrating a modified
construction of the said apparatus.
The same letters indicate similar parts throughout the Drawings.
The apparatus shewn in Figures 1, 2, 3, has a tank a, which is preferably placed
below the surface of the earth; this tank serves to contain the crude ammoniacal
liquor, which is pumped up to a tower b through a suitable pipe b', the liquor
passing in its course through a series of sulphuretted hydrogen condensers ċ by
which it is heated. As this liquor descends within the said tower b vapor generated
at a high pressure from the same is admitted at the bottom of the tower by a
pipe 62 leading from boilers e forming part of the said apparatus, thereby causing
the crude liquor to give off nearly the whole of its free ammonia gas (which consists
of carbonate and sulphide of ammonia), and it then passes off to saturators &
through a suitable pipe d'. The remaining liquor is then carried by means of a
pipe d provided at the lower part of the tower b to one or more forcing boilers or
tanks *, to which steam is admitted by a branch pipe d³ leading from the pipe baª
connected with the said boilers e; from these tanks d* this liquor is blown into the
boilers e through a connecting pipe d³, where the remainder of the free ammonia
above described is eliminated; from these boilers the gas liquor is afterwards
conducted through another pipe de to a tank f containing lime, which is agitated
by means of a perforated pipe f¹ connected with the said boilers e. The fixed
ammonia or sulpho-cyanide of ammonia left in the liquor is here eliminated, and is
taken back to the tower b through a pipe f provided for this purpose, and which
also serves as an overflow pipe to prevent the overfilling of the said tower; then, as
herein-before described, the ammonia thus set free is taken away to the saturator or
saturators, in which by being combined with sulphuric acid it forms sulphate of
ammonia.
The sulphuretted hydrogen generated in the said saturators is passed through
the aforesaid condensers c, which are constructed of wrought iron, and are provided
with small tubes arranged vertically. Within the surrounding space there is a
continual flow of the crude ammoniacal liquor from the crude liquor tank to the
tower b. This liquor condenses, and at the same time, is heated by the sulphuretted
hydrogen passing through the vertical tubes, whence the uncondensed sulphuretted
hydrogen is conveyed to the boiler furnaces to be burnt or being ignited in a

page_text: fire-clay retort passes to the acid chambers, where the sulphurous acid formed is
utilized for the formation of sulphuric acid, but it is preferable to use oxide of iron
purifiers to absorb the sulphuretted hydrogen, air being drawn into these purifiers
by a suitable exhauster to obviate the necessity of removing the oxide for
revivification. The spent lime in the agitating tank is blown off through pipes into
a series of precipitating tanks g.
I may construct the tower b either of wrought or cast iron, and either round or
square, but I prefer to make it square, and of wrought-iron plates, and I provide
within the same a series of angle iron bars arranged in tiers crossing each other.
Previous to the descent of the liquor down or through the said tower it enters a
wrought-iron tumbling box 6* or other suitable device for distributing the liquor
equally over the entire area of the top tier of angle bars, thereby causing the liquor
to drip evenly through all of the openings between the said bars to the bottom of
the tower or still b.
It will be understood that I may employ a series. comprising any number of
the parts of the apparatus above described as may be desirable, according to
circumstances.
In working the above apparatus I do not use the vapor from the steam boilers e
for agitating the lime and liquor containing fixed ammonia until it has been boiled
some time, so that steam, which is quite clear, or but slightly contaminated, is
obtained, and I thus prevent waste of lime. In order to ensure this result I take
the steam from the boilers e alternately.
According to a modification of my said Invention I treat the crude ammoniacal
liquor by the aid of the apparatus illustrated in Figures 4 and 5 as follows, that is
to say-The crude ammoniacal liquor is pumped into a closed tank or cistern a
provided with an interior coil of pipes a', through which steam mixed with heated
ammonia gas will pass from. the steam boilers h to an open saturator i; the said
boilers are fed from the tank or cistern a by a small forcing boiler j; by this process
the free ammonia is eliminated in the tank a. by means of the heated coil in
conjunction with the vacuum caused by an air pump or exhauster k, whence it
passes off to a closed saturator l.
The said exhauster or air pump k is worked by steam, or in any other suitable
manner, and is connected with the said closed saturator l. By means of the said.
air pump or exhauster a vacuum is created in the closed saturator, whereby the
free ammonia is drawn from the ammoniacal liquor in the tank or cistern into the
said closed saturator, which is charged with sulphuric acid; at the same time, the
sulphuretted hydrogen generated in the closed saturator is exhausted from it, and
treated in the manner first above described. By this process considerably less coal
will be required than would be required for the evaporation of the ammoniacal
liquor. The remaining ammoniacal liquor in the steam boilers h, after having been
well boiled, is blown off to an agitating tank m, in which it is treated with milk of
lime forced into the agitator from an auxiliary tank n; by these means the
fixed ammonia is given off, and taken, as herein-before described into an open
saturator.
Having thus fully described the said Invention and the manner of performing the
same, I wish it understood that I claim,-
First. In the manufacture of sulphate of ammonia generating high-pressure steam
from the ammoniacal liquor, as and for the purpose set forth.
Second. In such manufacture the concentration of the residual liquor in such a
manner that the cyanides therein may be coveniently and advantageously recovered
or eliminated.
Third. The apparatus shewn in Figures 1, 2, 3, of the Drawings constructed and
operating as and for the purpose specified.
Fourth. In the manufacture of sulphate of ammonia the volatilization of the
ammonia by the aid of a vacuum in a closed saturator, as and for the purpose
nocified

page_text: Fifth. The apparatus shewn in Figures 4 and 5 of the Drawings constructed and
operating as and for the purposes specified.
In witness whereof, I, the said Roger William Wallace, have hereunto set my
hand and seal, this Eighteenth day of March, in the year of our Lord
One thousand eight hundred and seventy-nine.
ROGER WILLIAM WALLACE. (L.S.)