Improvements in Apparatus for the Production of Chlorine.
Year: 1888

page_text: Date of Application, 16th Oct.,. 1888
Specification Accepted, 23rd Nov., 1888
Improvements in Apparatus for the Production of Chlorine.
1, JOHN AUGUST JUST, of Syracuse, in the County of Onondaga, and State of
New York, United States of America, Chemist 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 an improvement in apparatus for making Chlorine; and
it consists in certain novel details of the construction and arrangement of the same,
substantially as will be hereinafter more fully set forth and more specifically pointed
out in the claims.
In order to enable others skilled in the art to which my invention pertains, to make
and use the same, I will now proceed to describe its construction and operation,
referring to the accompanying drawings, in which :
Figure 1 is a diagram view of a plant arranged as I shall describe.
Figure 2 is a transverse section of a part of the plant, used for recovering the
manganese dioxide, and nitric acid, part of the devices appearing in elevation.
Figure 3 is an enlarged detail section of one of the stills or generators, showing
its connections to the different pipe systems, and also the manner of operating the
syphon.
Figure 4 is a section taken longitudinally through the washer.
Figure 5 is a detail plan view of the trap into which the lower end of the syphon
is received, and through which the residue liquor is entered to the drain, and conducted
to the cistern or well, and
Figure 6 is a detail cross-section of the pan placed over the furnace, to separate the
constituents of the residue liquor, and recover the manganese dioxide.
In the manufacture of chlorine on a large scale, commercially, a number of stills
or generators are required, and as I desire in this apparatus to so arrange the parts,
that the process of manufacture shall be practically continuous and there will be a
continuous charging of the stills, recovery of the ingredients, and immediate re-use
of the same, I have arranged my stills or generators in a series of rows or batteries,
connected with the charging, and recovery devices by a series of pipe systems arranged
as shown, to be out of the way of the operators and attendants in their work, but

page_text: t
in perfect position to best carry on the work continuously, as will be now described
fully and in detail.
1
I use any desired and suitable number of stills, in the formation of a battery, the
series forming each battery, being placed in a trough-a, preferably of wood lined
with sheet lead of requisite strength as clearly indicated at-a', and in the bottoni
of the trough I place a coil of steam pipes-a²,-for heating the stills, as will be
hereinafter more fully explained.
Each still or generator consists of an earthen-ware vessel-b,-of suitable size and
form, which vessel is provided with a removable cap or cover- --the rim of which
fits into a groove-62,-in the top of the still, and this groove is filled with water or
other liquid to form a seal into which the rim of the cover is received, and the
admission of air or escape of gas, around the edges of the cover is thus effectually
prevented, while the cover is readily removed or replaced as it becomes necessary in
the working of the apparatus.
Upon one side of the still, in its side wall, is formed a passage--the lower end
of which opens inwardly to the interior of the still at or near its bottom, while the
upper end of said passage opens outwardly through the side of the still, at a suitable
height, and to this opening is secured a section of rubber tubing-c¹,-connected to a
glass tube-c, which latter is extended downward, and opens into a trap-c³-
seated upon the drain system which carries off the residue liquor, after the charge in
a still is fully worked. All this will be fully seen in figs. 1 and 3.
The passage in the side of the still, together with the rubber and glass connections
forms a syphon for draining the still of its residue liquor, and this syphon is started
and operated by a simple contrivance shown in Figure 3, as follows: Above and at
one side of the still I secure two shelves-d-d-one above the other.
Upon the
upper shelf is a pair of air-tight jars-d',-containing liquid such as water, which
partially fills them, and connected by a flexible tube-,-as shown. One of the
jars is also connected by a rubber tube-d³,-with the syphon, and provided with any
suitable compress-d-When the syphon is to be started, the second jar is lowered
to the lower of the two shelves, and the compress-dis loosened. This at once
causes the liquid in the upper jar-d-to flow into the lower one, and draws the air
out of the syphon till the residue liquor rises in the passage-c, and flows over
through the rubber and glass tubes. As soon as this flow is started, the compress is
tightened, the second jar returned to its place on the upper shelf, and the syphon
continues to draw off the residue liquor from the still to the drain till all has
been exhausted, and the still is empty. This forms a very efficient mode of emptying
the stills, which needs little attention, and is automatic in its action after having
been started. It is evident that a glass tube may be used upon the inside of the
still to take the place of the passages-c, but I prefer the form described, with this
passage formed in the still body as shown. It will be understood that each still of
the battery is provided with its own syphon, connected to the drain, exactly as has
just been described.
;
t
Within the still is placed a perforated vessel-e, to receive and hold a portion of
the charge and the top or upper part of the still is, upon one side of its central
opening provided with a nozzle-e--for the escape of the chlorine gas, which nozzle
is connected to a gas conducting system presently described. Upon the opposite side of
the central opening the still top is provided with another opening-e, which is
formed with a grooved flange-e-in which rests a cover-e', having its rim on.its
lower edge, notched out as shown, and this forms an inlet for the reception of the acid
charge, which flows under the notched edge of the cover, and so enters the still,
sufficient always remaining in the groove, to form a seal to the cover in the same
manner as described for the main cover of the still, and so prevent the gas from
escaping as it forms therein, except by the opening provided for it.
In a plant of any size, the batteries are arranged in parallel rows, as in figure 1,
with sufficient space left between them for the free and convenient passage of the
workmen and attendants; and at a convenient point I construct, in the ordinary way,
of stone and cement a tank or cistern-f,-for the reception of the residue liquor left
3

page_text: in the stills after the working of a charge, which liquor contains certain elements
'which it is necessary to recover, and must therefore be saved till subjected to the
recovery process. From this cistern, a main drain--is laid, (preferably under-
ground so as to be out of the way), past the ends of the batteries of the plant, and of
course with an inclination toward the cistern, so the liquor may run freely through it.
Connected to this main drain, are a series of branch mains--which are extended
laterally along side of the series of batteries, and in each of these branches, at proper
intervals, is inserted a trap-c³,--as best shown in figures 3 and 5. These traps
simply consist of small cups, suspended by lugs, in openings of the drain, and their
object is to retain sufficient liquid to seal the lower ends of the syphons, which rest
in them. Each trap is by a syphon such as I have already described, connected to
one of the stills of the battery, and thus when these syphons are started, the residue
liquor contained in the stills, is automatically drawn off, and flows readily through the
branch and main drains, to the cistern. These mains and the cistern are clearly
shown by dotted lines in figure 1, and their location and operation will be clearly
understood.
The acids used in the manufacture, by my process, are two in number, viz.; Hydro-
chloric acid and nitric acid. These are contained in a divided receptacle-g;- -con-
veniently located and each provided with a draw-off cock, which empty into the open
ends of a---9,-connected to an acid main-g2,-which is extended down past
the ends of the batteries, as in figure 1, inclining away from the acid receptacle to
give a free flow of the same; and this acid main is also provided with a series of
branches g, extending laterally past the stills of the batteries. These branch and
main pipes, are connected by two way cocks, so the whole flow of acid may be directed
from the main into any particular branch at pleasure; and each branch is provided
also with a series of discharge cocks-y-corresponding to the number of stills on
the line, and these discharge cocks convey the acids to the receiving openings of the
stills. In the charging of the stills it is always advisable to begin with the still
nearest the main acid pipe, and charge them consecutively, as it is thereby possible to
drain out all the acid in the pipes, at the charging of the last still of the series
or battery. This is a matter of advantage in practice that will be at once clearly
seen.
It will be noted that the arrangement of the acid supply system being above the
stills is out of the way of the attendants and does not interfere with them in their
duties; and that the connections to the stills are such that any one or all of the stills
are charged at pleasure, and thus each still is under independent control, and can be
worked separately from the rest of the battery.
Alongside of each line of stills, or battery, and above the same, out of the way, is
also arranged a branch gas-pipe-h, to which the gas outlet of each still is connected
by a pipe of lead or material to resist the action of the chlorine. These
pipes as seen in figure 3, are preferably carried above the gas pipe--and
connected thereto by a bend in order that the moisture which may be carried into the
pipe by the gas shall not be drained back into the stills, but shall run through the gas
system to the washer, where it can do no harm.
These gas branch pipes all connect with a main gas conductor-2,-which is connected
to a washer--as in figures 1 and 4, in which the gas is forced to spread out, and
passes over the surface of water as illustrated. From thence the gas conductor is
led off to its connection with a chloride of lime chambers--at any convenient
point.
Some of the ingredients used in the manufacture of the chlorine, are to be
recovered from the residue liquor, for re-use, and to accomplish this I use the devices
as follows:
A furnace-k-of any suitable size and economical form and construction is located
conveniently; and over it is set a shallow pan-k-closed in as shown in figure 2. In
this pan I place the residue liquor from the cistern, and apply heat from the furnace
at a slowly rising temperature, till the maximum heat is obtained for the purpose
intended. The closed pan is connected by a pipe-k-with a condensing tower-k³—

page_text: provided with an air inlet-k-near its lower end. Within the tower are arranged a
series of shelves-m-having openings arranged therein at alternate sides, and in the
upper part of the tower is provided a jet or spray of water, as at―m³,-which flows
down over the shelves through their zig-zag openings to the bottom. A series of con-
densing jars mare provided connected together by pipes-m³,-and syphons—m³,
and the upper end of the condensing tower-k³-is connected by a pipe-n, -with the
first one of the series of condensing jars, this pipe passing through an intermediate
cooler as clearly seen in figure 2. The lower end of the tower is also connected
by a glass tube-n-with the last jar of the series, as clearly illustrated. From the
last jar of the condensing series, a pipe-o-extends to a second tower-o¹,-also
provided with a water jet or spray, and having from its lower end, a glass tube-o²,
for conducting the slightly acid water back to the last jar, as shown.
When heat is applied in the furnace, the residue liquor is caused to throw off one
of its ingredients, in nitrous vapors, and the other is finally left solidly in the pan in
the form of pure manganese dioxide. The nitrous vapors pass off through the proper
connections, to the tower-k³,-where they are mixed with air, and rise over the shelves,
through the tower, and are cooled and greatly condensed by contact with the water
flowing down. The condensed vapors forming weak acid are carried from the bottom
of the tower to the last jar of the condensing series, and are caused to travel through
the series, toward the first jar. The uncondensed vapors and commingled air, pass off
at the top of the tower through the pipe-n,-to the first of the series of jars, and pass
on through the series, subject to contact with, and in the opposite direction to, the
acid water. Should any uncondensed vapors remain on reaching the end of the series
of jars, they pass on to the second tower, and are there thoroughly condensed and
returned to the end of the series, as shown. Thus I obtain a perfect recovery of both
the ingredients contained in the residue liquor, and re-use them, in again charging the
batteries, effecting a considerable economy in practice, and making the process of
manufacture by the peculiar arrangement of the plant, practically continuous, and it
is not necessary to check the work while cleaning and recharging the stills.
The advantages of this arrangement of the plant will be obvious. In cannot only
be worked in whole or in part, according to the demand for the product, but it is very
cheaply and quickly enlarged at any time by simply extending the pipe and drain
systems, and adding another battery, or by adding more stills to the batteries already
in use, and extending their size. The arrangement is also compact and in such form
as to permit the work to be done automatically, and under perfect control.
I have named herein, as the ingredients used in the apparatus, Nitric Acid, Hydro-
chloric Acid, and Manganese dioxide, because these form the ingredients used in a
process for which I have applied for a separate patent of even date herewith, and this
apparatus is the one I prefer to use in carrying out said process, but I do not desire
to be understood as in any way confining myself thereto, as other processes, and
combinations of ingredients may be worked and recovered in this apparatus with equal
facility.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what 1
claim is :-
1-The combination with a series of stills, arranged in batteries, of an acid supply
tank, provided with a system of distributing pipes separately connected to each still, a
system of drain pipes also connected to each still, and to a cistern, and a system of
gas pipes separately connected to each still, and led through a washer to the desired
point, all constructed and arranged to operate, substantially as and for the purpose
set forth.
2-The combination with a drain system, and a cistern to which it leads, said drain
being provided with a series of traps at proper points, of a series of stills each
connected to one of the traps by a syphon substantially as and for the purpose set
forth.
3-The combination with a still provided with a syphon for emptying it, of a drain

page_text: system provided with the cup shaped traps-c³, for holding liquid in
which the end of the syphon is sealed, substantially as and for the purpose set
forth.
4-The combination with a still, provided with a syphon for draining of the liquid
residue after operation, of a pair of shelves one above the other, a pair of liquid vessels
connected by a syphon pipo and one of them adapted for removal from the upper
shelf to the lower, and back, and a pipe connecting the other vessel with the still
syphon, and provided with a compress cock, substantially as and for the purpose set
forth.
5-The combination with the condensing tower and a series of connected condensing
jars, of a pipe for the vapors connecting the upper part of the tower with the first jar
of the series, and a second pipe for the acid water connecting the bottom of the
tower with the last of the series of jars, substantially as and for the purpose set
forth.
6-The combination with the series of condensing jars-m², of a vapor pipe
connecting the end of the series with the tower-o¹, and a return tube-o³, -con-
necting the base of this tower with the last jar of the series, substantially as and for
the purpose set forth.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London,
Agents for the Applicant.