from Ammoniacal Liquors and for the Treatment of the Resulting Ammoniacal Vapors.
Year: 1885

page_text: from Ammoniacal Liquors and for the Treatment of the
Resulting Ammoniacal Vapors.
1
I, HENRY SIMON of No 20 Mount Street Manchester in the County of Lancaster,
Civil Engineer, do hereby declare the nature of my invention for "IMPROVEMENTS
IN APPARATUS FOR THE DISTILLATION OF AMMONIA FROM AMMONICAL LIQUORS AND
FOR THE TREATMENT OF RESULTING AMMONICAL VAPORS to be as follows:-
"
This invention relates to apparatus for distilling and concentrating ammoniacal
liquors in a continuous manner, wherein such liquors are caused to pass downward
through a column wherein as they flow successively from one tray to the next
below they are brought into intimate contact with steam passing in a contrary
direction whereby the steam is made to liberate the ammonia from the liquor, the
latter being then made to flow into a chamber containing milk of lime whereby
any ammonia remaining in a combined state is rendered free.
According to one of the present improvements there is arranged below the
chamber containing the milk of lime, a second chamber, having firstly a central
pocket or well into which the milk of lime and impurities together with the spent
ammoniacal liquor flows from the upper chamber through a central tube and in
which any solid suspended matter can deposit. From the top of this well, the
mixed liquid overflows on to a stepped surface, the steps of which gradually increase
in diameter as they descend, so that the liquid as it flows downwards is gradually
spread out in layers of decreasing depth until at the lowest steps it is in an
exceeding fine state of subdivision, and flows at a very slow rate.
Below the lowest step is a perforated steam coil and above each step is a corre-
sponding angular partition reaching down to near the surface of the liquid, so that
the steam in rising is brought into intimate contact with the liquid flowing down
each of the steps and us this is in a very fine state of subdivision and flows at a
very slow rate as it arrives on the lower steps the steam effectually takes up all
the free ammonia still contained therein. The steps may consist merely of a series

page_text: of vertical rings over the edges of which the liquor flows. Arrived at the top of
the chamber which contains the said steps, the steam passes into the upper chamber
by means of tubes, each arranged concentric and inside corresponding and inverted
tubes which force the steam to pass entirely through the compartment containing
the lime water and thus in heating the same, a certain quantity of the ammonia
from the liquor mixed therewith is liberated. From this chamber the steam then
passes successively through the trays of the column in the known manner and
finally issues from the top of the latter together with the ammoniacal vapor
liberated thereby. This mixed steam and ammoniacal vapor is then made to pass
into a closed vessel through which the ammoniacal liquor is made to flow before
entering the column so that by this means the double purpose is gained of cooling
the mixture of ammoniacal vapors and steam and of warming the ammoniacal
liquor before it enters the column.
In order to bring the vapors into intimate contact with the liquor it is preferred
to introduce the latter through a pipe dipping down into the liquid in the vessel
and having a branch connected to the escape pipe for the ammoniacal vapor so that
both the liquor and the vapor enter the vessel through the same pipe, and the
vapor in escaping from the lower end of the pipe has to bubble up through the
liquor so as to become still further cooled thereby.
The warmed liquor flows from the upper part of this vessel through a bent pipe
into the top of the distilling column while the cooled ammoniacal vapor is conducted
from the top of the vessel to either of the two other vessels containing milk of lime
through which the vapor is made to pass so as to free it from any carbonic acid &c.
The said pipe is for this purpose provided with two branches one leading to each
of the lime vessels, and each provided with a stop-cock, the branches being connected
to vertical tubes passing down to the bottom of the vessels where they are perforated
so as to cause the vapor to issue in a divided state into the milk of lime. The tops
of the vessels are connected by pipes provided with stop cocks, either with a cooling
chamber for the production of concentrated ammoniacal liquor or with the necessary
apparatus of known construction for the production of either spirit of sal-ammoniac
or sulphate of ammonia.
When the milk of lime in the one lime vessel has become spent, the stop-cocks
communicating with the supply pipe for ammoniacal vapor and with the condensing
vessel &c are closed while those connecting the second vessel with those parts of
the apparatus are opened and while the process of purification and condensation is
thus continuously carried on the spent lime liquor in the first vessel is in the first
instance treated with steam introduced through a branch pipe into the before
mentioned vertical pipe, so as to drive off any ammonia that may have been taken
up by the lime liquor, the resulting mixture of ammoniacal vapor and steam being
led through a pipe back into the distilling column.
The spent line liquor is then discharged from the first vessel through a stop cock
at bottom and a fresh charge of milk of lime having been introduced this vessel
is now made to communicate with the supply pipe for ammoniacal vapor, while
the second vessel is in its turn cut off.

page_text: "
Resulting Ammoniacal Vapors.
I, HENRY SIMON, of No 20 Mount Street, Manchester in the County of Lancaster,
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:-
This invention relates to apparatus for distilling and concentrating ammoniacal
liquors in a continuous manner, wherein such liquors are caused to pass downward
through a column, wherein, as they flow successively from one tray to the next
below, they are brought into intimate contact with steam passing in a contrary
direction, whereby the steam is made to liberate the ammonia from those salts in
the liquor which volatilize on boiling, the liquor being then made to flow into
a chamber containing milk of lime, whereby that part of the ammonia is dissociated
which is combined with the fixed salts of the liquor. Apparatus operating in this
manner was described in the Specification to Grüneberg's Patent No 5075 of 1879.
The present improvements relate firstly to an improved construction of the
still or apparatus for disengaging the ammonia from the liquor, and, secondly, to
apparatus for concentrating and otherwise treating the ammoniacal vapors after
they have left the still.
I will proceed to describe the said improvements with reference to the accom-
panying drawings, in which Fig. 1 shews an elevation, partly in section, of the
entire apparatus, Fig. 2 shews a plan, Fig. 3 shews a sectional elevation of the still,
Fig. 4 shews a cross section of the same at XX. Fig. 3.
The still consists of the well known arrangement of a column A in which the
ammoniacal liquor is caused to flow downward successively through a number of
trays, while steam is caused to flow upward in intimate contact with liquor, so as
to liberate the ammoniacal vapor therefrom. Arrived at the bottom tray b, more
or less deprived of its ammonia, the liquor flows through the pipe c into the
chamber & containing milk of lime, so that by mixing with this, any ammonia
remaining in the liquor in a combined state is rendered free; the milk of lime,
which is continuously fed into the chamber, overflows through the pipe e and
descends into a well f in a second chamber F. In this well any solid suspended
matter becomes deposited, while the liquor overflows its edge on to the stepped
surface T, consisting of a series of circular steps of increasing diameter, so that the
liquor in flowing down over them becomes spread out in layers of gradually
decreasing deptb, until at the lowest step, it is in an exceedingly fine state of sub-
division and flows at a very slow speed. Below the lowest step is a circular
perforated pipe S into which steam is supplied through the branch S¹ and the
steam issuing thence is caused by the concentric annular partitions to pass
upward in intimate contact with the liquid flowing down over the steps, so as to
take up what free ammonia is still contained therein. Arrived at the top of the
steps, the mixed steam and ammonia vapour passes into the upper chamber d
through tubes k situated concentrically within other tubes 1, closed at their upper
:

page_text: ends and open at the lower ends, so that the mixed steam and vapor after rising
through the tubes k, has to descend again through and issue in a finely divided
state into the mixture of milk of lime and liquor contained in the chamber. The
steam is thus caused to disengage a further quantity of ammonia from the liquor,
and then passes up through the tower A in the well known manner, finally issuing
at top together with the ammonia vapor through the pipe n.
The deposit in the well fis discharged from time to time through the discharge
valve operated by the lever f³.
Also, in
Instead of constructing the stepped surface T as shewn at Fig. 3, it may consist
of a number of concentric rings of graduated height, as shewn in section at Fig. 5.
It may also be made of polygonal or segmental form instead of circular.
place of the annular partitions i the casing of the apparatus may be formed inclined
as shewn in the modification at Fig. 6, so, as to, cause the steam to pass, in close
contact with the liquid.
The pipe n conducts the mixed steam and ammoniacal vapour into a vessel B,
into which the ammoniacal liquor that is to be fed into the still is also caused to
enter through a pipe m opening into the same box m² into which the mixed steam
and ammoniacal vapors pass, so that the liquor and vapour are brought into
intimate contact, and issue together through the pipe m² into B, where the vapor
is made to bubble up through the liquor on its way to the pipe o.
.
"
The ammonia vapor thus becomes effectually cooled, while, at the same time, the
liquor becomes heated before flowing off through the bent pipe a into the still.
This modification is only used in connection with the concentrating arrangements-
it is not used in connection with apparatus for sulphate.
Fig. 7 shews a modified arrangement of the above described combined heater
and cooler, wherein the upper part of the vessel B contains a coil B¹ through which
cold water is made to flow, entering at B2, and issuing at B³ into a tank B₁
surrounding B, whence it overflows through a pipe B³. By this means, the
ammonia vapor, contained in the upper part of the vessel B is still farther cooled
before issuing through o. The cooled ammoniacal vapor is conducted from the
vessel B, through the pipe o, to the one or other of the two vessels C₁ C² cou-
taining milk of lime, through which the vapor is made to pass so as to free it.from
any carbonic acid &c.
For this purpose, the pipe o is provided with two branches o¹ o² leading
respectively into the vessels C¹ C, in which they descend to near the bottom where
they are perforated, so as to allow the ammonia vapor to issue in divided streams
into the lime liquid. Each branch pipe is provided with a stop cock 1 and 3,
so that while the ammonia vapour is being admitted into the one vessel, the
communication with the other one can be cut off.
From the tops of the vessels C¹ C², other pipes, p, also provided with stop
cocks, 2 and 4, pass either to a cooling apparatus D, for the production of
concentrated ammoniacal liquor, or with the necessary apparatus of known
construction for the production of either spirits of sal ammoniac, or sulphate of
ammonia. The construction of the apparatus D is shewn slightly modified in the
enlarged elevation at Fig. 8; it consists of a casing D within which is a vessel i,
into which passes the pipe p from the lime vessels, and which contains a coil j, for
the circulation of cold water, entering at top through the pipe q and issuing at j¹
at bottom into the casing D whence it passes away at r.
The ammoniacal vapor
entering the vessel i from the pipe p and becoming refrigerated and condensed by
contact with the coil j, flows off through the bent pipe 8.
When the milk of lime in the one vessel, say C¹, has become spent by the passage
of ammoniacal vapor through it, the cocks 1 and 2 are closed, and 3 and 4 are
opened, so that the ammoniacal vapor will now pass from o into C³ and thence to
the cooler D. A steam pipe g provided with branches and stop-cocks communicates
with the pipes o¹ 03 of the vessels C₁ C, so that after C¹ has been cut off from the
supply pipe o, steam is admitted into the milk of lime so as to drive off any.
ammonia taken up thereby, the resulting mixture of ammoniacal vapor and steam

page_text: being led back into the still A through a pipe a¹, also provided with stop cocks.
The spent lime liquor is then discharged from C¹ through a discharge cock 5, and a
fresh charge of milk of lime having been introduced through the pipe n², C is
again put in communication with o and D, and the communications of Care
closed so soon as the contents hereof have become spent. Thus the continuous
operation of the still and the purifying and condensing apparatus is maintained.
Fig. 9 shews a vertical section of a somewhat modified form of the vessels C₁ C²,
in which these are provided with stirring apparatus t consisting of revolving
inclined vanes, situated immediately below the orifice of the pipe o¹, through which
the ammoniacal vapor enters, so that an intimate admixture of the latter in a finely
divided state with the milk of lime is insured. The shaft ¹ of the vanes passes up
through the pipe o¹ and is rotated through gearing by any convenient motor.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what
I claim is
1. In apparatus for distilling ammonia from ammoniacal liquor, the use of a
clamber containing a stepped surface on to which the lime liquor charged with
weak ammoniacal liquor flows from the lime chamber above, the liquor on flowing
down in a thin stream over the stepped surface being subjected to intimate contact
with steam whereby the last trace of ammonia is disengaged therefrom and carried
back into the lime chamber, substantially as herein described.
2. In combination with the stepped surface referred to in the preceding claim,
the use of a well or pocket into which the liquor flows from the lime chamber
before passing on to the stepped surface, in order to separate solid suspended matter
therefrom substantially as herein described.
3. In combination with the stepped surface referred to in the preceding claims,
the use of annular partitions or equivalent appliances for causing the steam to
come into intimate contact with the liquor flowing over the steps, substantially as
herein described.
4. The use, in combination with apparatus for distilling ammonia from ammo-
niacal liquor, of a vessel through which the liquor to be treated in the still is made
to pass before entering the still and into which the mixed ammonia vapor and
steam proceeding from the still is also made to pass in such manner as to effectually
mix with the liquor, in order both to cool the ammonia vapor and to heat the liquor
before entering the still, substantially as herein described.
5. The use, in combination with apparatus for continually distilling ammonia
from ammoniacal liquor, of two or more vessels containing milk of lime so
connected with the said apparatus by means of pipes having stop cocks, that the
ammonia vapor can be alternately introduced into one or other of the said vessels,
or sets of vessels, so that while the vapor is being acted upon by the lime liquor
in the said vessel, the spent lime liquor in the other vessel through which the
vapor has previously passed can first be treated with steam for the liberation of
aminonia and then be discharged and the vessel be filled with a fresh charge of
lime liquor, substantially as herein described.
Dated this 94th day of Novemba 1002