Improvements in and connected with the Distillation and Con- densation of Ammoniacal and other Liquids and in Apparatus therefor.
Year: 1889

page_text: Belgium),
Date of Application (in United Kingdom), 16th May, 1889
Complete Specification Left, 17th Feb., 1890-Accepted, 3rd May, 1890
PROVISIONAL SPECIFICATION.
Improvements in and connected with the Distillation and Con-
densation of Ammoniacal and other Liquids and in Apparatus
therefor.
We, SOLVAY AND COMPANY, of Brussels, in the Kingdom of Belgium,
Manufacturers, do hereby declare the nature of this invention to be as follows:-
Heretofore the apparatus used for the distillation of ammoniacal liquors has been fed
directly with weak ammoniacal liquor, either cold or heated by passing through an
apparatus for condensing the products of the distillation, or through a reheater. The
said ammoniacal liquor, before passing to the distilling apparatus has lost none of its
carbonic acid (CO2), sulphuretted hydrogen (SH), and ammonia (NH³), and the
products of distillation contain the whole of the CO, SH, and NH which were
present in the liquors when they entered such distilling apparatus. These products
of distillation are usually directed into a condenser and according to the construction
thereof, a small quantity of the CO and SH* may be sometimes disengaged. In no
apparatus, however, so far as we are aware, are the CO2 and SH2 removed from the
ammoniacal liquors before such liquors enter the distilling apparatus proper. This
operation can, however, be effected by the process and apparatus forming the subject
of this invention and whereby a concentrated liquid may be obtained having a per-
centage in ammonia which may reach 32% and even more in some cases and which
only crystallises on cooling to a temperature of nearly 0° C.
The construction and operation of our improved apparatus is based upon the differ-
ence in the degrees of solubility at various temperatures, of the gases which are in
solution in the liquid requiring to be distilled. The gases of different solubility are
differently retained by successive washings in liquids having a variable temperature.
The accompanying drawing shews partly in vertical section and partly in elevation
the construction of a separator, according to this invention having a multiple action
and suitable for the treatment of weak ammoniacal waters for the manufacture of con-
centrated waters. a is the main distilling apparatus which may be of any suitable
construction; bb1 62 63 64 are a series of chambers forming part of the separator;
they are formed of trunks or tubular casings which may be of cast iron or other
suitable metal. cccc¹ are worms or coils of lead or other suitable metal ;
dddd are pipes carried by the hottoms of the chambers etc. and serving for
the passage
of gases; e e e e are plunger caps supported above the pipes d' dctc.,
ffare pipes for the passage of ammoniacal liquor from one chamber to
the other. g is the apparatus for condensing the gases proceeding from the main
distilling apparatus.
It is a reservoir for supplying the weak ammoniacal liquor to be treated. i is a con-
k is a
densing worm or coil through which the weak ammoniacal liquor passes.
washing apparatus or washer supplied with liquor from the worm or coil i. is a pipe
for conveying gas and vapour from the upper coil to the condenser y wherein
they are condensed. m is a pipe for the disengagement of the separated gases which
escape from the separator and which are conducted to the washer k. m² is an outlet

page_text: ů
pipe to permit of the gases escaping from the washer k. n is a pipe for conveying the
weak animoniacal liquor from the reservoir to the inlet of the worm i in the con-
denser g.
is a pipe for conveying the ammoniacal liquor from the outlet of the
worm to the washer k. p is a pipe for conveying the ammoniacal liquor from
the washer to the upper chamber of the separator. is a pipe for conveying the
ammoniacal water from the outlet of the lower chamber of the separator to the inlet »
of the main distilling apparatus a. t is a pipe for conveying the products of the
distillation from the distilling apparatus a to the inlet of the worm c. u is a inain pipe
for condensed water from the worms c' c² c³ c; to it is joined the piper. is a reservoir
for storing the concentrated ammoniacal waters as they issue from the condenser g.
The course of the vapours from the distilling apparatus a through the various
apparatus, the course of the ammoniacal liquor requiring to be distilled, and the course
of the gases disengaged in the chambers 66263 are as follows:-
The volatile products of the distillation of the distilling apparatus a pass through
the pipe and enter the lower extremity of the worm, passing through the whole
length of the same and continuing their ascending motion by passing from the
worm a to the worm e' by means of the curved pipe IC. In the same manner the said
products traverse the worm the curved pipe w the worm e the curved pipe w² the
worm c³ the curved pipe w³ and the worm and pass to the pipe w*. They are then
led through the pipe to the condenser y wherein they are condensed by contact with
the worm and pass in the form of concentrated liquor, through the pipes which
conveys them to the reservoir it. The products of the distillation are cooled in their
passage through the various worms, a part of the steam and of the gases contained
therein being condensed.
Each of the curved pipes w w w² we may be provided with a pipe for collecting
the products condensed in the coils c¹³ and for conveying them to the main u
whence they are returned into the distilling apparatus a ate with the ammoniacal
liquor to he distilled.
The worin e etc. may be replaced by any other suitable arrangement for
transmitting to the liquor, before its entrance into the main distilling apparatus,
the heat necessary for the separation of the gas or gases to be evolved therefrom.
The ammoniacal liquor requiring to be distilled and which is stored in the reservoir /
descends in a cold state through the pipe and enters the lower end of the lower
worm of the condenser J. The liquor circulates methodically through the worms i
from bottom to top and becomes heated by condensing the ammoniacal vapours which
enter the condenser through the pipe. The ammoniacal liquor heated to a suitable
temperature say about 40° Centigrade passes from the worm and proceeds through
the conduit o to the washer & where the gases escaping from the casing are washed
and freed from the ammonia which they may contain, the CO and SH gases
escaping almost entirely, through the pipe me. The ammoniacal liquor afterwards
descends through the pipe and enters the upper chamber of the separator. Here
it becomes heated by contact with the wori e and descends through the overflow
pipe into the chamber where it is still further heated by contact with the worm c³.
It then passes through the overflow pipe f³ to the chamber 2, then through
the overflow pipe to the chamber and through the overflow pipe to the
lower chamber, whence it passes through the overflow pipe and pipe and
cuters the distilling apparatus a at v. The ammoniacal liquor is successively
heated in each of the chambers bat increasing temperatures as it passes
from the top to the bottom of the separator. The evolution of CO2 and SH2 com
mences to take place in the upper chambers 663 and continues in the chambers b² b
and the temperature in the chambers and being such that the NH³ gases are
disengaged at the same time as the CO2 and SH2 gases but the ammonia (NH3)
bubbles up in the liquid contained in the chambers ² 36 which liquid is of gradually
decreasing temperature from bottom to top and is condensed therein, whereas the
CO2 and SH are not condensed and continue their ascending course through the
apparatus in a gaseous state.
The gases disengaged in the chamber pass through the pipe d', bubble under the

page_text: plunger cap el and owing to this bubbling favor the disengagement of the gases con-
tained in the liquor within the chamber 61 and carry them away through the pipe d²
and under the plunger cap e² so as to bubble through the liquid within the chamber 62,
where they abandon a part of the ammonia and carry away a fresh quantity of CO₂
and SH. The same actions take place in the chambers 63 and 64.
A small
The gases that escape through the pipe m are only CO2 and SH2 gases and a small
quantity of ammonia which is retained on its passage through the washer k.
washer with acid may be used for finally washing the gases escaping through the
pipe m from the washer k.
The concentrated ammoniacal liquor obtained in the reservoir a may reach the
desired richness in ammonia according to the working of the apparatus. A caustic
liquid of a specific gravity nearing 1 or even inferior to the unit or near 0° of
Beaume's areometer, may be obtained at will, and contains from 20 to 30% of
ammonia or a liquid partially caustic and still more concentrated may be produced.
We have described the application of the separator apparatus to the manufacture of
concentrated liquors. The application is similar in the manufacture of the volatile
alkali for which its use will even be of greater importance by reason of the economy
of lime resulting therefrom.
The separator or multiple acting apparatus may advantageously be used in the
purification of lighting gas. The use of caustic ammonia has already been indicated
for this object. Our process, which provides an easy means of imparting causticity to
the weak liquors produced in gas works, solves the difficulty which has heretofore
stood in the way of this application.
As will be obvious, other liquors besides ammoniacal liquors may be treated
according to this invention.
Dated this 16th day of May 1889
W. LLOYD WISE.
COMPLETE SPECIFICATION.
Improvements in and connected with the Distillation and Con-
densation of Ammoniacal and other Liquids, and in Apparatus
therefor.
We, SOLVAY AND COMPANY, of Brussels, in the Kingdom of Belgium, Manu-
facturers, 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 :-
Heretofore the apparatus used for the distillation of aminoniacal liquors has been
fed directly with weak ammoniacal liquor, either cold or heated, by passing the liquor
through an apparatus for condensing the products of the distillation, or through a
reheater. The said ammoniacal liquor, before passing to the distilling apparatus
has lost none of its carbonic acid (CO2), sulphuretted hydrogen (SH), and
ammonia (NH), and the products of distillation contain the whole of the CO2, SH³,
and NH which were present in the liquors when they entered such distilling
apparatus. These products of distillation are usually directed into a condenser and
according to the construction thereof, a small quantity of the CO2 and SH2 may be
sometimes disengaged. In no apparatus, however, so far as we are aware, are
the CO2 and SH2 removed from the ammoniacal liquors before such liquors enter
the distilling apparatus proper. This operation can, however, be effected by the
process and apparatus forming the subject of this invention and whereby a con-
centrated liquid may be obtained having a percentage in ammonia which may
reach 32% and even more in some cases and which only crystallises on
a temperature of nearly 0° C..
cooling to
The construction and operation of our improved apparatus is based upon the
difference in tlie degrees of solubility at various temperatures, of the gases which
are in solution in the liquid requiring to be distilled. The gases of different solubility

page_text: are differently retained by successive washings in liquids having a variable
temperature.
The drawing filed with our provisional specifiation shews partly in vertical section
and partly in elevation the construction of a separator according to this invention
having a multiple action and suitable for the treatment of weak ammoniacal liquor
for the manufacture of concentrated liquor. is the main distilling apparatus which
may be of any suitable construction; bb62 13 are a series of chambers forming
part of the separator; they are formed of trunks or tubular casings which may be of
cast iron or other suitable metal. cc' e² cc are worms or coils of lead or other
suitable metal; d¹ d' d³ d'are pipes carried by the bottoms of the chambers b₁ h² etc.,
and serving for the passage of gases e e e e are plunger caps supported above the
pipes etc. are overflow pipes for the passage of ammoniacal
liquor from one chamber to the other.
is the apparatus for condensing the gases proceeding from the main distilling
apparatus. his a reservoir for supplying the weak ammoniacal liquor to be treated.
i is a condensing worm or coil through which the weak ammoniacal liquor passes. k is
a washing apparatus or washer supplied with liquor from the worm or coil i. is a pipe
for conveying gas and vapour from the upper coil to the condenser g wherein they
are condensed. m is a pipe for the disengagement of the separated gases which
escape from the separator and which are conducted to the washer k. m is an
outlet pipe to permit of the gases escaping from the washer k. n is a pipe for
conveying the weak ammoniacal liquor from the reservoir to the inlet of the
worm in the condenser g. o is a pipe for conveying the ammoniacal liquor from
the outlet of the worm i to the washer k. p is a pipe for conveying the ammoniacal
liquor from the washer to the upper chamber of the separator. r is a pipe for
conveying the ammoniacal water from the outlet of the lower chamber of the
separator to the inlet of the main distilling apparatus a. is a pipe for conveying
the products of the distillation from the distilling apparatus a to the inlet of the
worin c. is a mainpipe for condensed water from the worms c c¹ c² c³ c; to it is
joined the pipe r. a is a reservoir for storing the concentrated ammoniacal waters
as they issue from the condenser 9.
The course of the vapours from the distilling apparatus a through the various
apparatus, the course of the ammoniacal liquor requiring to be distilled, and the
course of the gases disengaged in the chambers are as follows:-
l
The volatile products of the distillation of the distilling apparatus a pass through
the pipe and enter the lower extremity of the worm c, passing through the whole
length of the same and continuing their ascending motion by passing from the worin e
to the worm c¹ by means of the curved pipe w. In the same manner the said products
traverse the worm c², the curved pipe w¹, the worm c³, the curved pipe w², the worm c³,
the curved pipe w³, and the worn c', and pass to the pipe to. They are then led
through the pipe to the condenser wherein they are condensed by contact with the
worm and pass in the form of concentrated liquor through the pipes which conveys
them to the reservoir a. The products of the distillation are cooled in their passage
through the various worms, a part of the steam and of the gases contained therein
being condensed. Each of the curved pipes w w' w³ ³ w may be provided with a
pipe for collecting the products condensed in the worms c¹ c² c3 c and for conveying
them to the main u whence they are returned into the distilling apparatus a at v with
the ammoniacal liquor to be distilled.
The worms c, c, etc. may be replaced by any other suitable arrangement for trans-
mitting to the liquor, before its entrance into the main distilling apparatus, the heat
necessary for the separation of the gas or gases to be evolved therefrom.
The ammoniacal liquor requiring to be distilled and which is stored in the
reservoir descends in a cold state through the pipe n and enters the lower end
of the lower worm i of the condenser g. The liquor circulates methodically through
the worms from bottom to top and becomes heated by condensing the ammoniacal
vapors which enter the condenser through the pipe 1. The ammoniacal liquor heated
to a suitable temperature say about 40° Centigrade passes from the worm i and

page_text: proceeds through the conduit c to the washer k where the gases escaping from the
casing are washed and freed from the ammonia which they may contain, the CO
and SH gases escaping almost entirely, through the pipe m'. The ammoniacal
liquor afterwards descends through the pipe p and enters the upper chamber of the
separator. Here it becomes heated by contact with the worm and descends through
the overflow pipe finto the chamber 63 where it is still further heated by contact
with the worm c³. It then passes through the overflow pipe to the chamber 62,
then through the overflow pipe f to the chamber b¹ and through the overflow pipe fi
to the lower chamber b, whence it passes through the overflow pipe and pipe and
enters the distilling apparatus a at v. The ammoniacal liquor is successively heated
in each of the chambers ³ ³ bb, at increasing temperatures as it passes from the
top to the bottom of the separator. The evolution of CO2 and SH commences to take
place in the upper chambers 64, 63, and continues in the chambers 62, 61 and 6 the
temperature in the chambers band being such that the NH3 gases are disengaged
at the same time as the CO2 and SH' gases but the ammonia (NH3) bubbles up in the
liquid contained in the chambers which liquid is of gradually decreasing
temperature from bottom to top and is condensed therein, whereas the CO² and SH²
are not condensed and continue their ascending course through the apparatus in a
gaseous state.
The gases disengaged in the chamber 6 pass through the pipe d¹, bubble under the
plunger cap el and owing to this bubbling favour the disengagement of the gases con-
tained in the liquor within the chamber and carry them away through the pipe d
and under the plunger cap e² so as to bubble through the liquid within the chamber 62
where they abandon a part of the ammonia and carry away a fresh quantity of CO*
and SH. The same actions take place in the chambers 3 and 4.
The gases that escape through the pipe m are only CO and SH gases and a small
quantity of ammonia which is retained on its passage through the washer k. A small
washer with acid may be used for finally washing the gases escaping through the
pipe m' from the washer k.
The concentrated ammoniacal liquor obtained in the reservoir a may reach the
desired richness in ammonia according to the working of the apparatus. A caustic
liquid of a specific gravity nearing 1 or even less than 1 or near 0° of Beaume's
areometer, may be obtained at will, and contains from 20 to 30% of ammonia ; or a
liquid partially caustic and still more concentrated may be produced.
We have described the application of the separator apparatus to the manufacture of
concentrated liquors. The application is similar in the manufacture of the volatile
alkali for which its use will even be of greater importance by reason of the economy
of lime resulting therefrom.
The separator or multiple acting apparatus may advantageously be used in the
purification of lighting gas. The use of caustic ammonia has already been indicated
by chemists for this object. Our process, which provides an easy means of imparting
causticity to the weak liquors produced in gas works, solves the difficulty which has
heretofore stood in the way of this application.
As will be obvious, other liquors besides ammoniacal liquors, may be treated
according to this invention.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed we declare that what
we claim is —
1. The process of caustifying (or rendering caustic) ammoniacal liquors, in com-
bination with the distillation or concentration of the same in one and the same
apparatus specially arranged in such a manner that the liquors enter the distiller
after having been freed from carbonic acid and sulphuretted hydrogen gases.
2. The apparatus for separating inert gases as hereinabove described, and composed
essentially of a series of trunks or tubular casings communicating by overflows and
traversed by coils that heats them to temperatures which decrease gradually from the
bottom to the top by means of the products of distillation of the main distilling

page_text: apparatus whilst the inert gases escapo through central tubular parts that are covered
with caps which compel the gases to bubble through liquor in the trunks or tubular
casings and to draw along with them the analogous gases from such liquor up to the
exit, whilst the ammonia that is disengaged at the bottom is redissolved at the top.
3. The employment of distilling, caustifying or separating apparatus substantially
such as hereinabove described for other purposes requiring the distillation of a mixed
liquid one of whose constituents is to be separated from the others, and one or
some of which is or are required to be eliminated in the state of inert gas or gases.
Dated this 17th day of February 1890.
W. LLOYD WISE.