A New or Improved Process for Obtaining Chlorine from the Spent Liquors of Soda Ash, from Brine, and from other similar Substances, and Means and Apparatus for Producing Chloride of Lime therefrom.
Year: 1893

page_text: Date of Application, 18th Mar., 1893
Complete Specification Left, 15th Sept., 1893-Accepted, 28th Oct., 1893
PROVISIONAL SPECIFICATION.
A New or Improved Process for Obtaining Chlorine from the Spent
Liquors of Soda Ash, from Brine, and from other similar
Substances, and Means and Apparatus for Producing Chloride of
Lime therefrom.
We, HENRY COSNETT of 76 Beech Lane, Macclesfield, Gardener, BENJAMIN
CHARLES BENNISON of 47 Brock Street, Macclesfield, Chemist, SAMUEL HAYES
of Rose Lodge, Upton, Macclesfield, Clerk and PETER SMALLWOOD of Witten,
Northwich, Insurance Agent, do hereby declare the nature of our said invention to
be as follows:-
"
Our invention has for its object to obtain chlorine from the spent liquors
Solway's
produced in the manufacture of soda ash, by what is known as
ammouia soda process or from brine or other similar substances and to utilise such
chlorine in the manufacture of chloride of lime in the manner hereinafter described.
In accordance with our invention we employ a series of metal retorts of an oval
or other suitable shape which are built into the roof of a furnace with their lower
extremities projecting into the furnace so that the flames and heat evolved in said
Into each of these retorts
furnace shall impinge thereon and so heat the contents.
we place a solution of the spent liquor, brine or other substance to be treated with
a quantity of potassium permanganate in or about the proportions of one part of
potassium permanganate to twenty parts of the spent liquor or brine or other
substance, said solution being introduced through a suitable funnel and pipe. Said
pipe communicates with each of the retorts through branches fitted with cocks or
valves to enable the communication between each retort to be closed as soon as the
retorts are supplied and thus enable them to work independently of each other.
Through another funnel and pipe a set of which is provided for each retort, we
introduce a quantity of sulphuric acid.
By now applying heat of about 100° Fahrenheit a chemical action takes place
in the retorts, chlorine being freely formed or produced, which readily escapes
through pipes from the top of the retorts to a chamber, there to be converted into
chloride of lime. In order to remove the bye products left in the retorts we
provide a pipe or tube from the bottom of each retort bent downwards and fitted
with a cock or valve and if desired leading into a pipe arranged along the furnace
for carrying all the bye products away to the front of the furnace.
The chamber to which the gas is conveyed is of by preference rectangular
construction and is lined with zinc and formed with apertures to admit of the gas.
A layer of slaked lime is strewn upon the floor of said chamber, which being exposed
to the chlorine absorbs said gas producing chloride of lime. The chamber is fitted
with a set of sbutters closed and cemented during the converting action, but
opened as soon as the action is complete to admit fresh air and allow of the
removal of the lime. This latter is effected by preference through a trap door in
the bottom of the chamber.
The charging of the chamber with lime is effected through a door in the end of
the chamber. To facilitate the examination of the lime under treatment a small
window is fixed in each end of the chamber and to allow of a small sample of the
lime being withdrawn for testing purposes we provide a small orifice closed by a
shutter or door.
1
C MonaL 1002

page_text: COMPLETE SPECIFICATION.
A New or Improved Process for Obtaining Chlorine from the Spent
Liquors of Soda Ash, from Brine, and from other similar
Substances, and Means and Apparatus for Producing Ohloride of
Lime therefrom.
We, HENRY COSNETT of 76 Beech Lane, Macclesfield, Gardener, BENJAMIN
CHARLES BENNISON of 47 Brock Street, Macclesfield, Chemist, SAMUEL HAYES
of Rose Lodge, Upton, Macclesfield, Clerk, and PETER SMALLWOOD of Witten,
Northwich, Insurance Agent, do hereby declare the nature of our said invention and
in what manner the same is to be performed, to be particularly described and
ascertained in and by the following statement :-
66
"
Our invention has for its object to obtain chlorine from the spent liquors
produced in the manufacture of soda ash, by what is known as Solvay's
ammonia soda process or from brine or other similar substance and to utilize such
chlorine in the manufacture of chloride of lime.
In accordance with our invention we employ a series of metal retorts of an oval
or other suitable shape which are built into the roof of a furnace with their lower
extremities projecting into the furnace so as to heat or warm the contents thereof.
Into each of the retorts we place the spent liquor, brine or other substance to be
treated with a solution of potassium permanganate in or about the proportions of
one part of potassium permanganate to twenty parts of the spent liquor or brine or
other substance, said solution being introduced through a suitable funnel and pipe.
Through another funnel and pipe, a set of which is provided for each retort, we
introduce a quantity of sulphuric acid.
By now applying a heat of about 90° to 100° Fahrenheit a chemical action takes
place in the retorts, chlorine being freely evolved which readily escapes through
pipes from the top of the retorts to a chamber there to be converted into chloride
of lime. In order to remove the bye products left in the retorts we provide a pipe
or tube from the bottom of each retort bent downwards and fitted with a cock or
valve and if desired leading into a pipe arranged along the furnace for carrying all
the bye products away to the front or side of the furnace.
A
The chamber to which the gas is conveyed is of, by preference, rectangular
construction and is lined with lead and formed with apertures to admit of the gas.
layer of slaked lime is placed upon the floor of said chamber which being exposed
to the chlorine absorbs said gas producing chloride of lime. The chamber is fitted
with a set of shutters closed and cemented during the converting action, but opened
as soon as the action is complete to admit fresh air and allow of the removal of the
lime. This latter is effected, by preference, through a trap door, hopper, or shoot
in the bottom of the chamber.
And in order that our invention may be the more readily understood and carried
into practical effect, we have hereunto annexed two sheets of drawings and will now
proceed to describe the same with the assistance of the various figures and letters of
reference marked thereon.
Fig. 1 (Sheet 1) is a longitudinal section of the furnace or heating chamber with
the retorts shewn in elevation.
Fig. 2 (Sheet 2) is an elevation, Fig. 3 a plan and Fig. 4 a side view of the lead
chamber with the retorts shewn in connection therewith.
In all the views similar letters are used to denote similar parts.
A, A, A, Fig. 1 (Sheet 1) are (by preference) three metal retorts built into a
furnace or chamber B, the fire grate of which is seen at B', the lower portions only
of the retorts being exposed to the heat of the chamber. Said retorts are fitted
with gauge glasses C for indicating the level of the liquid in the retorts, and
man-holes D (see Sheet 2 Fig. 3) for cleaning out. The three retorts are connected

page_text: together at the bottom by a pipe E and a draw-off cock E', is fitted to this pipe at-
a convenient position for drawing off the residuum from the retorts. From the top
of each retort a gas pipe F, F1, F, rises and is led off to a lead chamber (herein-
after more particularly described) and fitted with slide valves G, G¹, G. Each of
the retorts is also fitted with a funnel, stop-cock, and pipe H, H', H', for introducing
the sulphuric acid and a similar set of pipes I, I, I, for introducing the potassium
permanganate. The first retort A is also fitted with an additional pipe and stop
cock J for introducing the spent liquor or brine from a suitable storage tank.
The lead chamber K (see Sheet 2. Figs. 2, 3 and 4) is constructed in the usual
manner and fitted with doors K', K', for charging and "trap" doors L, L', L', for
discharging the lime after treatment. A window or windows M may also be
introduced for observation. Louvres N are also fitted in the chamber capable of
being thrown open after the process is completed to allow the free chlorine ready
egress preparatory to the emptying of the chamber. A door O (seen more clearly
in Fig. 5) is also fitted at the end of the chamber opening outwards and a drop
door O¹ is arranged inside capable of being opened and closed with a cord O³ for
testing the action of the chloride on the lime.
The mode of working our invention is as follows:-
The lead chamber is charged through doors K', K' in the usual manner,
care being taken that some of the lime is placed near the door O. The trap
door O' being raised as illustrated and left in this position during the operation of
the gas.
Spent liquor or brine is allowed to flow into the retorts through the pipe J and
connecting pipe E till they are about two thirds full when the stop-cock is
closed. The potassium permanganate is then introduced through the pipes and
funnels I, I, I, and lastly the sulphuric acid is introduced through the funnels and
pipes H, H, and H. The proportions we prefer to use are about 20 parts of
spent liquor or brine, one of potassium permanganate and one of sulphuric acid.
The sulphuric acid being allowed to enter the retorts a little at a time. We do not
confine ourselves to these proportions but we have found them give good results in
practice.
A gentle heat of 90° to 100° Fahrenheit is maintained in the retorts B by a
small fire at B' and chlorine gas now comes over freely and is conveyed by the
main pipes F, F', F2 to the lead chamber K where, finding the slaked lime it
combines therewith forming chloride of lime in the well known manner. We
proportion the capacity of the retorts to the lead chamber, so that one charge of
the retorts is about sufficient to produce enough chlorine to effectually fill the lead
chamber. When this has been effected and no more gas comes from the retorts we
close the valves G, G' and G' in the main pipes F, F' and F³, and after clearing
out the residuum from the retorts by opening the tap we recharge the retorts with
spent liquor or brine preparatory to a second production of chlorine as soon as the
lead chamber is in a condition to receive it as will be understood by those conversant
with the manufacture of chloride of lime.
The progress of the action of the chlorine on the lime may be observed by
lowering the drop door O¹ and opening door O and extracting a sample of the
chloride of lime. It will be obvious that the previous closing of the door O¹
prevents the escape of chlorine when the door O is opened.
When the lime has been sufficiently treated with the chlorine the process is
stopped and the lead chamber ventilated by the louvres and the chloride of lime is
discharged through the doors L, L', L'.
Having thus particularly described the best methods with which we are
acquainted for carrying our invention into practical effect we desire it to be
understood that we do not confine ourselves to the exact proportions of the
ingredients in the retorts as herein before mentioned nor to the precise form of
apparatus described (as for instance a steam or hot water heat may be substitute.!
for a furnace heat in warming the retorts) as the same might be considerably varied

page_text: without departing from our invention. We desire also to say that we make no
claim to the production of chloride of lime by the mere action of chlorine on lime
but what we consider to be our invention and therefore claim is―
1st. Treating the spent liquor produced in the manufacture of soda ash by what
is known as 66
Solvay's" ammonia soda process with potassium permanganate and
sulphuric acid in the manner described for the production of chlorine therefrom.
2nd. Treating brine with potassium permanganate and sulphuric acid in the
manner described for the production of chlorine therefrom.
3rd. In the production of chlorine from the spent liquor produced in the
manufacture of soda ash by what is known as Solvay's" ammonia soda process
by the process hereinbefore described and the production of chloride of lime
therefrom the use and employment of retorts A, A1, A2 or their equivalent, heated
from the furnace B or by other suitable means fitted with pipes, cocks, etc., in
combination with a lead chamber K substantially as herein before described and
illustrated on the accompanying drawings..
Dated this 14th day of September 1893.
JOHN G. WILSON & Co.,
55, Market Street, Manchester, Agents for the Applicants.