Improvements in the Method of and Apparatus for Distilling, Separating, and Concentrating Acids or Mixed Liquids, and for Treating Substances in Solution.
Year: 1892

page_text: Date of Application, 22nd June, 1892
Complete Specification Left, 21st Mar., 1893-Accepted, 13th May, 1893
Improvements in the Method of and Apparatus for Distilling,
Separating, and Concentrating Acids or Mixed Liquids, and for
Treating Substances in Solution.
I, EUGENE JEAN BARBIER, of 13 Rue des Archives, Paris, France, Manu-
facturer, do hereby declare the nature of this invention to be as follows:-
This invention has reference to improved methods of and apparatus for separating
by distillation two or more liquids having different boiling points and for concen-
trating the products obtained, also for treating liquids containing substances in
solution and for separating such substances.
The accompanying illustrative drawings show the general arrangement of
apparatus according to this invention,
Fig. 1 being a longitudinal section; and
Fig. 2 a transverse section thereof.
The apparatus is arranged in two groups one of which has for object to separate
the substances to be treated, and the other to concentrate the acids and the other
products resulting from said separation.
The separating apparatus comprises a furnace provided with evaporating troughs
or basins a a of material such as sandstone, porcelain, or metal with or without
suitable lining or coating, and usually of refractory and unattackable material,
which can be varied in form and capacity to suit requirement. At the sides of the
furnace there are arranged doors which allow of easily and immediately replacing
any of the basins. The basins are arranged in a baffle-wise descending series with
the object of directing the liquid and of lengthening its course; they rest on
plates c c of metal or refractory and unattackable material, which are provided or
not with perforations for facilitating the access of flame from the heating furnaces.
These plates are formed with draining channels d d which discharge outside and
indicate when there is a breakage, and also the point where such breakage has
taken place. Above the basins is arranged the condensing apparatus e composed
of superposed domes of unattackable material arranged in pairs in such a manner
as to form narrow chambers m n of large surface in which the vapors to be condensed
circulate. These chambers may be separated from one another by a space o
wherein the external cold air circulates. The vapors enter the first chamber m
through holes, slits or fissures f which may vary in shape and number; they then
pass through external conduits t or internal conduits into the following chanibers n
which may or may not be arranged baffle-wise.
The liquid to be treated is fed into the apparatus or separating furnace from a
trough g by any suitable means such as a syphon h.
The vapors condensed under the domes flow off by suitably arranged channels i
and the uncondensed vapors and gases pass through a tower provided with baffle
plates and charged with coke, flint or any other suitable unattackable material, and
to which they are conveyed by the pipe k. These vapours and gases escaping from
the tower are finally discharged into a chimney which produces the necessary
suction throughout the apparatus. In some cases the vapors formed during the
heating of the basins, are transformed or converted by an injection of hot air or
steam according to requirements. This steam or air may with advantage be
discharged under the domes from a chamber 9 arranged to be heated by the fuel
in the fireplace j.
The liquid flowing off from the last basin through the conduit is collected in a
receptacle which I will call the "mixing evaporator" that communicates with
a refrigerator y. The liquid is then passed into the concentrating furnace A which

page_text: is also composed of basins or troughs covered over by one or more condensing
domes M which may be smaller than in the first furnace. I may however if desired
employ a single dome arranged to form merely a conduit for the vapors; or if
required the concentration may be effected in the open air.
In the special case of treating mixtures, such for example as sulphuric acid and
nitric acid, the weak sulphuric and nitric waters liberated from the basins of the
concentrating furnace are condensed, and then conducted by a conduit into the
'evaporating receptacle".
«
The vapors issuing from said receptacle x, return through the conduit D into
the separating apparatus and are condensed under the domes.
The apparatus described serves for separating and concentrating substances in
solution, or mixtures of liquids having different boiling points.
I will now proceed to describe the special arrangement of my apparatus in its
application to the separation of sulphuric and nitric acids.
Figs. 3 and 4 of the accompanying drawings illustrate this special application of
the apparatus herein before described, the same letters of reference being used in
all the figures to indicate like parts.
Fig. 3 shows partly in vertical longitudinal section and partly in elevation, the
general arrangement of the apparatus.
Fig. 4 is a transverse section thereof, on the line 1-2 of Fig. 3.
This arrangement is applicable to the treatment of mixed sulphuric and nitric
acids obtained from any source. In this special case I have found it more
advantageous to place the mixing evaporator to the rear and above the concen-
trating furnace.
In order to separate the two acids, viz. sulphuric and nitric acids, at their
maximum point of concentration by my processes, I proceed in the following
manner :-
The mixture is fed in at the upper part of the mixing evaporator from a
receptacle y simultaneously therewith, the vapors produced in the concentrating
furnace A are led into the bottom of the said evaporator. The vapors are intro-
duced by means of an injecting device u that may advantageously be operated by
hot air.
The hot vapors from the concentrating process dilute the mixed acids, raise
their temperature, and effect almost the complete denitration thereof. The nitric
acid escaping from the mixture is led by the pipe into the battery of con-
densers provided for this purpose, and thence into the tower G whence
uncondensed nitric acid vapors pass to the chimney. The sulphuric acid which is
now, as already stated almost free from nitric acid, flows into an intermediate
reservoir E and is thence led by the pipe F into the basins a in the concentrating
furnace A where it is finally and completely denitrated and concentrated.
finally passes from the last basin into the receptacle K completely denitrated and
concentrated to 66° Be.
It
In order to ensure the completely denitration of the acid I may, if necessary,
pass a small current of sulphurous acid into the mixing evaporator or into any other
part of the apparatus.
In all cases, my processes require the simultaneous or successive use of the
following apparatus :—
A distilling or separating furnace; a concentrating furnace comprising, as in
the case of the distilling furnace, a series of basins with discharging spouts or lips
arranged baffle-wise or not; doors for allowing of the easy and immediate replacing
of any of the basins; draining channels formed in the plates supporting the basins,
and serving to indicate breakage of the basins and the spot where such breakage
has taken place; basins surmounted by a single dome or by a number of super-
posed domes forming multiple condensing chambers, between which there may be
passed at will, currents of air for the purpose of increasing the condensing surfaces
if such be thought necessary; mixing evaporator which may be located either
below the concentrating furnace or above the same in which latter case it may be

page_text: employed in place of the separating furnace, and into which there are passed the
liquids to be separated and the products of distillation from the concentrating
furnace, either condensed and cold, or condensed and hot, or it may be in a state of
vapor as above described; a condensation battery; and finally a collecting tower
for collecting the last traces of the distillation.
Dated this 22nd day of June 1892.
E. J. DARDIER,
By L. W., per F. B.
COMPLETE SPECIFICATION.
Improvements in the Method of and Apparatus for Distilling,
Separating, and Concentrating Acids or Mixed Liquids, and for
Treating Substances in Solution.
I, EUGENE JEAN BARBIER, of 13 Rue des Archives, Paris, France, Manu-
facturer, 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 has reference to improved methods of and apparatus for separating
by distillation two or more liquids having different boiling points and for con-
centrating the products obtained; also for treating liquids containing substances in
solution and for separating such substances.
The drawings filed with my Provisional Specification show the general arrange-
ment of apparatus according to this invention,
Fig. 1 being a longitudinal section; and
Fig. 2 a transverse section thereof.
The apparatus is arranged in two groups or parts one of which has for object to
separate the substances to be treated, and the other to concentrate the acid or other
product resulting from said separation.
The separating apparatus comprises a furnace provided with evaporating troughs
or basins a a (hereinafter called basins) formed of material such as sandstone,
porcelain, or metal with or without a suitable lining or coating, the basins, or the
lining or coating thereof, as the case may be, being of refractory material, not
liable to be injuriously attacked by the material treated therein. The form and
capacity of the basins can be varied to suit requirement. At the sides of the
furnace are arranged doors 6 which allow of easily and immediately replacing any
of the basins. The basins are arranged in a step-wise descending series with the
object of directing the liquid and of lengthening its course; they rest on plates cc
of metal or refractory and practically unattackable material, which may be provided
with perforations for facilitating the access to the lower sides of the basins of flame
from the heating furnaces. These plates are formed with draining channels d d
which discharge outside the furnace and serve to indicate when there is a breakage
of a basin, and also the point where such breakage has taken place. Above the
basins is arranged the condensing apparatus composed of superposed domes or
covers e of practically unattackable material arranged in pairs in such a manner as
to form narrow chambers m n of large surface in which the vapors to be condensed
circulate. These chambers may be separated from one another by a space o
wherein the external cold air may be caused to circulate. The vapors enter the
first chamber m from the space above the basins through holes, slits of fissures f
which may vary in shape and number and are formed in the innermost cover e;
they then pass through external conduits t, or it may be internal conduits, into the
chamber n, which may, or may not be provided with vertical partitions arranged
baffle-wise as shewn in Fig. 1.
The liquid to be treated is fed into the apparatus or separating furnace from a
trough g by any suitable means such as a syphon h.

page_text: The vapors condensed under the covers e flow off by suitably arranged channels i
in which the covers rest, and the uncondensed vapours and gases are passed through
a tower provided with baffle plates and charged with coke, flint or any other suitable
unattackable material, and to which they are conveyed by the pipe k. The
uncondensed vapours and gases escaping from the tower are finally discharged into
a chimney which produces the necessary suction throughout the apparatus. In
some cases the vapors formed during the heating of the basins, may be transformed
or converted into other compounds by an injection of hot air or steam according to
requirements. This steam or air may advantageously be discharged under the
covers e from a chamber q arranged to be heated by the fuel in the fireplace j.
2
The liquid flowing off from the last basin through the conduit is collected
in a receptacle that I will call the "mixing evaporator" which communicates
with a refrigerator or cooling vessel y into which the liquid passes. The liquid
is then passed into the concentrating furnace A shown at the left hand side of Fig. 2
which is also composed of basins or troughs a covered by condensing covers M which
may be smaller than those employed in the first mentioned furnace. I may however if
desired employ a single cover M-arranged to form merely a conduit for the
vapors; or if required the concentration may be effected in the open air.
In the special case of treating mixtures such for example as sulphuric acid and
nitric acid, the weak sulphuric and nitric acid watery vapours liberated from the
basins of the concentrating furnace are condensed, and then conducted by a conduit
into the mixing evaporator x.
The vapors issuing from said mixing evaporator x, return through a conduit D
into the separating apparatus and are condensed under the covers e.
The apparatus described serves for separating and concentrating substances in
solution, or mixtures of liquids having different boiling points.
I will now proceed to describe the special arrangement of my apparatus in its
application to the separation of a mixture of sulphuric and nitric acids.
Figs. 3 and 4 of the said drawings illustrate this special application of the
apparatus hereinbefore described the same letters of reference being used in all
the figures to indicate like parts.
Fig. 3 shows partly in vertical longitudinal section, and partly in elevation, the
general arrangement of the apparatus.
Fig. 4 is a transverse section thereof, to a larger scale, on the line 1-2 of Fig. 3.
This arrangement is applicable to the treatment of mixed sulphuric and nitric
acids obtained from any source. In this special case I have found it more
advantageous to place the mixing evaporator a to the rear and above the concen-
trating furnace.
In order to separate the two acids, viz. sulphuric and nitric acids, at their
maximum point of concentration by my processes, I proceed in the following
manner :-
The mixture is fed in at the upper part of the mixing evaporator from a
receptacle y; simultaneously therewith, the vapors produced in the concentrating
furnace A are led into the bottom of the said evaporator, the vapors being
introduced by means of an injecting device u fed preferably with hot air under
pressure.
These hot vapors resulting from the concentrating process, dilute the mixed
acids in the mixing evaporator, raise their temperature, and effect almost the
complete denitration thereof. The nitric acid vapors escaping from the mixture is
led by the pipe v into the battery of condensers C provided for this purpose, and
thence into the tower G whence uncondensed nitric acid vapors pass to the
chimney. The sulphuric acid which is now, as already stated, almost free from
nitric acid, flows into an intermediate reservoir E and is thence led by the pipe F
into the basins a in the concentrating furnace A where it is finally and completely
denitrated and concentrated. It finally passes from the last basin into the
receptacle K completely denitrated and concentrated to about 66° Be.
In order to ensure the complete denitration of the acid I may, if necessary pass

page_text: a small current of sulphurous acid into the mixing evaporator, or into any other
suitable part of the apparatus.
In all cases, my processes require the simultaneous or successive use of the
following apparatus
:-
A distilling or separating furnace; a concentrating furnace comprising, as in the
case of the distilling furnace, a series of basins with discharging spouts or lips
arranged baffle-wise or not; doors for allowing of the easy and immediate replacing
of any of the basins; draining channels formed in the plates supporting the
basins, and serving to indicate breakage of either of the basins and the spot where
such breakage has taken place; basins surmounted by a single cover or by a
number of superposed covers forming multiple condensing chambers between which
there may be passed at will, currents of cold air for the purpose of increasing the
condensing action if such be thought necessary; a mixing evaporator which may
be located either below the concentrating furnace or above the same, in which
latter case it may be employed in place of the separating furnace and into which
there are passed the liquids to be separated and also the products of distillation
from the concentrating furnace, either condensed and cold, or condensed and hot,
or it may be in a state of vapor as above described, a condensing vessel or battery;
and finally a collecting tower for collecting the last traces of the products of
distillation.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. For the treatment of acids or mixed liquids, or of substances in solution, for
the purpose of distilling, separating, and concentrating the same, apparatus
comprising evaporating troughs or basins arranged step-wise in a descending series
within a heating furnace, constructed with lateral doors through which the trough
or basin can be readily passed, and perforated or non-perforated plates or supports
provided with suitably arranged draining channels and upon which the said troughs
or basins rest, substantially as hereinbefore described for the purpose specified.
2. Apparatus of the kind referred to in the preceding claim constructed with
superposed domes, or covers forming condensing chambers that may be separated
by spaces through which the external air can circulate and are connected together
by suitable conduits, the innermost dome or cover being formed with openings for
the passage of vapors given off from the basins substantially as herein before
described.
3. In the treatment of liquid for the purpose of distilling separating and con-
centrating the same, the employment of the hot vapors and products of distillation
produced in the concentrating operation for diluting and heating the mixed liquids,
and facilitating their separation, as for example for separating nitric acid from a
mixture of sulphuric and nitric acids substantially as hereinbefore described.
4. The special arrangement of the mixing evaporator above the concentrating
furnace for the purpose of effecting the separation of the mixed liquids before they
pass into the said concentrating furnace as for example in the separation of nitric
acid from sulphuric acid, as hereinabove described with reference to Fig. 3 of the
drawings.
5. For separating and concentrating mixed liquids or substances in solution
apparatus constructed arranged and operating substantially as hereinbefore
described with reference respectively to and shown in Figs. 1 and 2, and in Figs. 3
and 4 of the drawings.
1
1 1000
E. J. BARBIER,
By L. W., per F. B.