IMPROVEMENTS IN THE MANUFACTURE OF SODA
Year: 1860

page_text: LETTERS PATENT to Jacob Geoghegan Willans, of No. 2, Clarence Place,
Belfast, in the County of Antrim, in Ireland, for the Invention of
"IMPROVEMENTS IN THE MANUFACTURE OF SODA."
PROVISIONAL SPECIFICATION left by the said Jacob Geoghegan Wil-
lans at the Office of the Commissioners of Patents, with his Petition,
on the 4th February 1860.
I, JACOB GEOGHEGAN WILLANS, of No. 2, Clarence Place, Belfast, in the
County of Antrim, in Ireland, do hereby declare the nature of the said Inven-
tion for "IMPROVEMENTS IN THE MANUFACTURE OF SODA," to be as follows:-
Instead of decomposing the sulphate of soda in the usual manner by means
of a sufficiency of carbon intermixed therewith, my improvement in this respect
is to abstract the oxygen of sulphate of soda, which has little or none of the
usual carbonaceous matter intermixed therewith, by means of carbonic oxide
gas previously produced in any convenient manner, the said sulphate and gas
being brought together in a retort pipe, or other chamber or vessel, from
which air is excluded at a sufficiently high temperature for the purpose, when
the sulphate of soda will become converted into sulphuret of sodium, and its
oxygen will unite with the carbonic oxide gas to form carbonic acid gas for
after use or escape.
My further improvement is to remove the sulphur from the sulphuret of
sodium resulting from the decomposition of sulphate of soda, having little-or

page_text: none of the usual carbonaceous matter intermixed therewith by means of
water, steam, or the gas or gases obtained from the decomposition of water.
The said sulphuret being brought into contact with any of the above at a
sufficiently high temperature, when the sulphur will be carried off in combi-
nation with the hydrogen of the water made use of, and a useful soda alkali
will remain. The above process may be carried out either simultaneously
with the formation of the said sulphuret or afterwards.
My further improvement is to bring water or steam into contact with sul-
phate of soda, or sulphuret of sodium having the carbonaceous matter of turf
or peat intermixed therewith, the said mixed substance and water or steam
being then at a high temperature to favor the decomposition of the water,
when the sulphur will be carried off in combination with the hydrogen of the
water, and a useful soda alkali will remain.
My further improvement is to utilize the sulphuretted hydrogen so given off
in either of the preceding processes in any convenient manner for the final
production of sulphurous or sulphuric acid.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Jacob Geoghegan Willans in the Great Seal Patent Office on
the 2nd August 1860.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JACOB
GEOGHEGAN WILLANS, of Number 2, Clarence Place, Belfast, in the County of
Antrim, in Ireland, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Fourth day of February, in the year of our Lord
One thousand eight hundred and sixty, in the twenty-third year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me, the
said Jacob Geoghegan Willans, Her special licence that I, the said Jacob
Geoghegan Willans, my executors, administrators, and assigns, or such others
as I, the said Jacob Geoghegan Willans, my executors, administrators, and
assigns, should at any time agree with, and no others, from time to time and
at all times thereafter during the term, therein expressed, should and law-
fully might make, use, exercise, and vend, within the United Kingdom of
Great Britain and Ireland, the Channel Islands, and Isle of Man, an Inven-
tion for "IMPROVEMENTS IN THE MANUFACTURE OF SODA," upon the condition
(amongst others) that I, the said Jacob Geoghegan Willans, my executors or
administrators, by an instrument in writing. under my, or their, or one of

page_text: their hands and seals, should particularly describe and ascertain the nature of
the said Invention, and in what manner the same was to be performed, and
cause the same to be filed in the Great Seal Patent Office within six calendar
months next and immediately after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Jacob Geoghegan Willans, do hereby
declare the nature of my said Invention, and in what manner the same is to
be performed, to be particularly described and ascertained in and by the fol-
lowing statement, that is to say:-
The nature of my improvements consists, firstly, in the production of sul-
phuret of sodium from such sulphate of soda as has either no carbonaceous
matter, or an insufficient quantity so intermixed therewith, to effect its decom-
position when heated in contact together.
Secondly, in the removal of sulphur from the said sulphuret, and the pro-
duction of a useful soda alkali therefrom.
Thirdly, in the removal of sulphur from such sulphuret of sodium as con-
tains peat carbon, after it has been produced from the sulphate of soda by
means of the carbon of peat intermixed and heated in contact therewith, and
the production of a useful soda alkali therefrom.
And, lastly, my improvements consist in the collection and use of the
sulphur, removed in the aforesaid processes for the production of sulphurous or
sulphuric acids.
When effecting the first part of my improvements, I decompose the
sulphate referred to into sulphuret by means of carbonic oxide gas brought
into contact therewith at a red heat; the said gas having been previously
generated in any convenient manner, but, by preference, by the action of a
blast of atmospheric air upon burning coke in a cupola furnace; the gas
being withdrawn from the upper part thereof for conveyance elsewhere, as is
now usual at iron blast-furnaces where the gas is utilized. I bring the said
gas into a retort pipe, or other chamber or vessel in which the aforesaid
sulphate is being exposed at a red heat. I prefer to use an oven or furnace,
such as is commonly used in the second stage of the manufacture of sulphate
of soda, and known to soda manufacturers as a blind furnace, or a closed
furnace, in which the heat applied is transmitted through the brickwork com-
posing the floor and interior roof. The said roof or arch may be about
twelve inches apart from the floor, and the door capable of being fastened and
luted, so as to exclude air when closed. At the door end of the said furnace-
I admit the carbonic oxide gas through four or more pipes or openings placed
at even distances apart, and about one inch above the level of the floor, and
from which the gas may at any time be shut off by a valve or other means.

page_text: At the opposite further end of the furnace I have three openings (dividing the
wall equally) of about eleven inches diameter inwardly, and widening out-
wards to about fifteen inches diameter. At the interior upper part of each
opening I have a pipe, from which a jet of steam or fine jets of water may be
ejected in a downward direction towards the exit. I also have the water or
steam in connection (close to the furnace) with the pipes or openings
admitting the carbonic oxide gas, so that I may have the power to apply either
steam or water along with the gas, as herein-after described. Immediately
adjoining the outer part of the three openings before mentioned, I prefer to
have a shallow flat-bottomed channel or trough with sides, but no ends, con-
structed of flags or masonry the full width of the interior of the furnace, and
four or more times its length, closely joined to the furnace, at which junction
the bottom of the said trough is placed on a level with the lowest part of the
circumference of the openings, and with a very slight fall therefrom towards
the other end of the trough. I also have eight or more flat iron lids or covers,
well tinned or otherwise prepared, to prevent oxidation on the top of the
said trough, their edges dipping down into water in the manner now usual
with the covers of dry lime purifiers at gasworks; and I prefer that the said
lids or covers should approach to within about three inches from the bottom
of the trough, excepting at that part adjoining the furnace, where the lid must
be sufficiently distant from the bottom to cover and include the openings
before mentioned. The other end of the trough is open into a flue or
chamber for the removal of gaseous matter. When the furnace is at a bright
red heat I throw therein at the door, and spread evenly, as much finely-ground
sulphate as will cover the floor to a depth of about one inch; the door is then
fastened and luted so as to hinder the entrance of air. I then admit the
carbonic oxide gas, and turn on the steam or water jets at the opposite end,
which facilitate the flow and further propulsion of the gaseous matter; and
should the furnace become hotter than desired, or sufficiently hot to volatilize
the sulphuret formed, I prefer to admit some steam or very minute jets of
water along with the gas into the furnace, at the same time diminishing to a
corresponding degree the quantity admitted from the other pipes at the three
openings. The quantity of carbonic oxide gas necessary will be about equal
to that which has been produced from the well-arranged consumption of
double the amount of carbon that would be required if the said carbon were
intermixed and heated in contact with the sulphate operated upon; but as an
excess of that amount will not prove injurious, I prefer to allow the said gas
to pass slowly over the heated sulphate, turning the latter over occasionally, so
as to intermix and expose fresh surfaces, and I continue the operation until

page_text: samples withdrawn for examination prove to have been satisfactorily de-
composed into sulphuret. When the workman is satisfied with the result, and
that space has been made in the trough adjoining for its reception, he shuts
off the gas and steam or water, and pushes or withdraws the sulphuret
through the three openings before mentioned, raising any lids or covers
necessary, and afterwards spreads it in a minutely divided state evenly over the
unoccupied portion of the trough (it being first broken or crushed and pul-
verised to that state, if required). The workman then fastens down the lids
and charges the furnace again with sulphate; the door is then luted, and the
carbonic oxide gas turned on with the steam or water jets at the opposite end,
as before described.
;
When effecting the second part of my Invention the quantity of steam or.
water necessary must at least be that equal in weight to one-eighth part
of the anhydrous sulphate used in the production of the sulphuret to which it
is applied. But I prefer to use an excess of that quantity, so that the material
may be kept in a slightly moist state, yet not in a liquid state; and as the
temperature of the cooled gaseous matter from the furnace and of the con-
densed steam is sufficiently high for the chemical action required, namely, the
removal of sulphur in the form of sulphuretted hydrogen and the simultaneous
production of a useful soda alkali, I prefer to have jets of cold water falling
upon the exterior of the lids or covers in their warmest parts, so as to promote
a deposition of moisture from the watery vapour in contact with the sulphuret
in the trough. The lids are raised occasionally to allow the intermixture and
exposure of fresh surfaces as well as the removal of samples. When the
workman is satisfied from examination of the said samples that any part of the
contents of the trough has been sufficiently deprived of sulphur by its being
passed off in combination with the hydrogen of the water or steam made use
of, he removes the said portion in a finished state as a useful soda alkali,
spreading unfinished sulphuret in the place it occupied, and leaving that part
of the trough nearest the furnace at liberty for the reception of the next batch.
of sulphuret which may be delivered from the furnace. As the admission of
atmospheric air into the furnace or trough would be more or less injurious, the
steam or water and carbonic oxide gas should be turned off before the door of
the furnace is opened, also the lids or covers of the trough should not be kept
longer open than necessary. I prefer to use steam at any available pressure,
but if water be substituted it should be in the form of very fine spray, which
may be vapourized by the heat of the furnace or the gaseous matter therefrom,
and neither should be admitted at any time in so large a quantity as to create a
solution of the soda material.

page_text: When effecting the third part of my Invention, I bring steam or water
into contact with the sulphuret of sodium whilst being formed from the sul-
phate of soda by the agency of peat carbon intermixed therewith or afterwards,
and I admit them into first contact at a red heat to favour the partial removal of
the peat carbon particles, which had not been consumed by the oxygen in the
sulphate by their decomposing more or less of the steam or water, and uniting
with any of its elements become removed in a gaseous form.
I prefer to use a furnace and trough as before described when applying
carbonic oxide, but instead of the latter I admit a small quantity of steam or
water into the furnace in which the sulphate is being decomposed by the
agency of the peat carbon intermixed therewith at a red heat; I also have the
steam or water jets at the openings in operation whilst the decomposed
sulphate is being pushed slowly past.
In all other respects the said sulphuret of sodium is to be treated and the
operation carried on as before described in the first and second parts of my
Invention, and with similar results.
When effecting the last part of my Invention, I prefer to withdraw the
gaseous matter which may have passed through the channel or trough unused
or unabsorbed by the soda material into the flue or chamber, at the end of the
trough before mentioned, by means of any suitable exhaust apparatus, so that
the said gaseous matter may be propelled further, and overcome any resistance
it may be subjected to without increasing the pressure in the trough through
which it had passed. I bring the said gaseous matter into contact with and
through such revivifiable oxide of iron as is found effective in the purification
of coal gas from sulphur, and I use the same kind of apparatus, and revive it
in the same manner as is usual at gas works where such oxide of iron is made
use of, by this means the sulphur contained in the said gaseous matter will be
retained. After the said oxide of iron has been saturated and revived to the
required extent, I separate sulphur therefrom by sublimation in any conve-
nient manner for use in the production of sulphurous acid, or I burn it off as
sulphurous acid for the manufacture of sulphuric acid.
I wish to remark that the term little or no carbon is to be understood to
signify either no carbonaceous matter, or an insufficient amount thereof to
produce the desired effect.
Having thus stated the nature of my Invention, and described the manner
of performing the same, I would have it understood that I do not confine
myself to the exact details set forth, nor do I claim the use of carbonic oxide
for decomposing sulphate of soda, nor the application of steam or water
to sulphuret of sodium, nor the use of the carbonaceous matter of peat

page_text: for decomposing sulphate of soda, nor do I claim the utilization of sulphur
collected from sulphuretted hydrogen gas; but what I do claim is,―
First, the use of carbonic oxide gas and steam or water conjointly or con-
secutively for forming the sulphuret of sodium from such sulphate as has little or
no carbonaceous matter in contact therewith, also for the purpose of removing
sulphur from the said sulphuret in the form of sulphuretted hydrogen gas
and the simultaneous production of a useful soda alkali in other than a dis-
solved state.
Secondly, the application of steam or water to the sulphuret of sodium in
less quantity than sufficient for making a solution thereof, whilst being or
after having been formed from the sulphate, with peat carbon inter-
mixed for the removal of sulphur in the form of sulphuretted hydrogen
gas.
And, thirdly, the use of the sulphur contained in the sulphuretted hydrogen
given off in any of the preceding processes for the production of sulphurous
or sulphuric acids.
In witness whereof, I, the said Jacob Geoghegan Willans, have here-
unto set my hand and seal, this Thirtieth day of July, in the year of
our Lord One thousand eight hundred and sixty.