IMPROVEMENTS IN THE MANU- FACTURE AND UTILIZATION OF CARBONIC ACID, AND IN APPARATUS CONNECTED THEREWITH
Year: 1864

page_text: LETTERS PATENT to George Hyacinthe Ozouf, of 2, Rue Sainte Appoline
Paris, France, for the Invention of "IMPROVEMENTS IN THE MANU-
FACTURE AND UTILIZATION OF CARBONIC ACID, AND IN APPARATUS CONNECTED
THEREWITH "
Sealed the 13th December 1864, and dated the 16th June 1864.
PROVISIONAL SPECIFICATION left by the said George Hyacinthe Ozouf
at the Office of the Commissioners of Patents, with his Petition, on
the 16th June 1864.
I, GEORGE HYACINTHE OZOUF, of 2, Rue Sainte Appoline, Paris, France, do
hereby declare the nature of the said Invention for "IMPROVEMENTS IN THE
MANUFACTURE AND UTILIZATION OF CARBONIC ACID, AND IN APPARATUS CONNECTED
THEREWITH," to be as follows:-
Hitherto carbonic acid has only been commercially produced by decom-
posing calcareous carbonates with acids.
Now the object of my Invention is to separate from the carbonic acid other
gaseous products proceeding from the combustion of coke, charcoal, anthracite,
and other materials, and from the burning of lime, and is based on two
known chemical properties, first, on the facility with which soda and potash
combine in excess with carbonic acid to produce bicarbonates; second, on
[Price 8d.1

page_text: the property they possess of losing this excess of carbonic acid at a temper-
ature of 212° Fahrenheit.
My Invention then consists in making use of these known chemical
properties in the following manner-1st, by the employment of a furnace
with grate and ash-pit or a lime furnace or kiln ; 2nd, of several hermetically
closed cylinders communicating with one another, and provided with agitators;
Srd, of a wood boat; 4th, of distilling and refrigerating vessels; 5th, of
serpentine coils for containing steam at a temperature of about 296° Fah-
renheit; 6th, of a pump for forcing in air and liquids; 7th, of a gasometer.
I apply this new method of producing pure carbonic acid, 1st, to the
preparation of ceruse or white lead by means of natural absorption with or
without a lift and force pump; 2nd, to the production or manufacture of all
gaseous liquids, such as seltzer water, soda water, frothy or sparkling wines,
and the like; and 3rd, to the preparation of carbonates and bicarbonates
generally.
By employing pure carbonic acid, I am enabled to manufacture white lead
by healthy mechanical means, and at the same time with rapidity. White lead
made in the manner before described is of an equal chemical constitution,
and the carbonic acid is mathematically treated, and in such manner that a
white lead more or less hydrated, or more or less carbonated, may be
produced. The operation is carried on in vacuo; and consequently by means
of absorption.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said George Hyacinthe Ozouf in the Great Seal Patent Office
on the 15th December 1864.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, GEORGE
HYACINTHE OZOUF, of 2, Rue Sainte Appoline, Paris, France, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Sixteenth day of June, in the year of our
Lord One thousand eight hundred and sixty-four, in the twenty-seventh
year of Her reign, did, for Herself, Her heirs and successors, give and grant
unto me, the said George Hyacinthe Ozouf, Her special licence that I,
the said George Hyacinthe Ozouf, my executors, administrators, and assigns
or such others as I, the said George Hyacinthe Ozouf, 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,

page_text: should and lawfully might make, use, exercise, and vend, within the United
Kingdom of Great Britain and Ireland, the Channel Islands, and Isle of Man,
an Invention for "IMPROVEMENTS IN THE MANUFACTURE AND UTILIZATION OF
CARBONIC ACID, AND IN APPARATUS CONNECTED THEREWITH," upon the condition
(amongst others) that I, the said George Hyacinthe Ozouf, my executors
or administrators, by an instrument in writing under my, or their, or one of
their hands and seals, should particularly describe and ascertain the nature
of the said Iuvention, 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 George Hyacinthe Ozouf, 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
following statement, reference being had to the Drawing hereto annexed, and
to the figures and letters marked thereon, that is to say :-
Hitherto carbonic acid has only been commercially produced by decomposing
calcareous carbonates with acids.
Now the object of my Invention is to separate the carbonic acid from other
gaseous products proceeding from the combustion of coke, charcoal, anthra-
cite, and other materials, and from the burning of lime, and is based on two
known chemical properties; first, on the facility with which soda and potash
combine in excess with carbonic acid to produce bicarbonates; second, on the
property they possess of losing this excess of carbonic acid at a temperature
of 212° Fahrenheit.
My Invention, then, consists in making use of these known chemical
properties in the following manner:-1st, by the employment of a furnace
with grate and ash-pit or a lime furnace or kiln; 2nd, of several hermetically
closed cylinders, communicating with one another, provided with agitatorsand
the last one with a chimney; 3rd, of a wood reservoir; 4th, of distilling
vessels and refrigerators; 5th, of serpentine coils for the circulation of steam
at a temperature of about 296° Fahrenheit; 6th, of pumps for forcing in air
and liquids; 7th, of a gasometer.
I apply this new method of producing pure carbonic acid, 1st, to the pre-
paration of ceruse or white lead by means of natural absorption; 2nd, to the
production or manufacture of all gaseous liquids, such as seltzer water, soda
water, frothy or sparkling wines, and the like; and, 3rd, to the preparation
of carbonates and bicarbonates generally.
By employing pure carbonic acid I am enabled to manufacture white lead

page_text: By nearthy and mechanical means, and at the same time with rapidity. White
lead made in the manner before described is of an equal chemical constitution,
and the carbonic acid is mathematically dosed, and in such manner that a
white lead more or less hydrated, or more or less carbonated, may be produced.
The operation is carried on in vacuo, and consequently by means of
absorption.
By the foregoing description it will be seen that the object of my Invention
is to obtain pure carbonic acid, and in utilising it in every susceptible way,
but especially to the manufacture of white lead by means of natural absorption,
and by dosing it, if desired, with carbonic acid, and to the manufacture of
waters and gaseous lemonades, soda water, frothy wines, and the like.
The effect produced by my Invention is to separate the carbonic acid either
from the gases produced by the combustion of coke, of coal, of charcoal, of
anthracite, or other combustible materials, or from those which result from
the manufacture of lime from all the gases which accompany it; in uniting
it with the sub-carbonates of soda or potash, with which it produces bicar-
bonates; and to profit from the properties which these bicarbonates possess of
losing at a sufficient heat, at about, say, from 170° to 220° Fahrenheit, the
excess of carbonic acid which they have absorbed to return to the state of
sub-carbonates as they were before the operation. The carbonic acid gas being
separated, it passes under a gasometer, and the alcaline liquor returns to be
used again after having been sufficiently cooled, in order to absorb a new
quantity of carbonic acid, which it afterwards loses, the process which forms
the subject of my Invention then consists in an alternate and continuous com-
position and decomposition of bicarbonate of soda or potash to obtain carbonic
acid, and to apply it as before described.
My process then consists in producing carbonic acid in a state of mixture
by one of the means before indicated, that is to say, by burning coke, coal,
and the like, and in securing all the gases proceeding from the combustion, in
taking them to the upper part of the furnace by means of one or several
suction and force pumps, making it or them in such manner that the gases
from the combustion which are drawn be replaced by the new air introduced
through an ash-pit placed at the lower part of the furnace, in such manner.
that the air is decomposed as completely as possible by traversing the bed of
the combustible material. It must be understood that the diameter of the
furnace, the bed of the combustible material, its power or that of the air.
pumps must be in relation to one another, so that during the combustion
neither carbonic oxide nor free oxygen is formed, and to make the gases of the
combustion to pass into the cylinders which are quite closed, and three-

page_text: quarters filled with solutions of sub-carbonates of soda or potash, and provided
with winged stirrers. These cylinders are put in communication with one
another by tubes of an S shape. The last cylinder has at its upper part a
chimney to allow the gases from the combustion other than the carbonic acid
which have not been assimilated, and which are azote, oxygen, carbonated
and sulphurated hydrogen gases, to escape. A pipe is placed at the upper and
in the fore part of this same cylinder to be used for the passage of the solution
of the bicarbonate of soda or potash which has been produced and which falls
into a reservoir made of wood. This solution of the bicarbonate of soda or
potash is afterwards retaken by means of one or several pumps in order to
be injected into a distilling receiver heated to a sufficient temperature by a
serpentine coil for circulation of steam, from whence the carbonic acid issues
mixed with steam to go into a serpentine where the two are condensed, the
carbonic acid to pass under a gasometer, and the water into the reservoir,
which receives the solution of the bicarbonate from the last cylinder, in order
to maintain this liquor at an equal density. The solution of the bicarbonate
which has been injected into the distilling vessel to cause it to lose its excess
of carbonic acid is drawn by a pump to be injected into the first cylinder
after having previously lost its heat in passing through a serpentine surrounded
by cold water to again take up the carbonic acid produced by the combustion,
and again to pass into the state of bicarbonate. The manufacture then
becomes continuous, and is in effect a composition and decomposition of
bicarbonate of soda or potash, according to which base is used.
The accompanying Drawing illustrates the manner in which I manufacture
pure carbonic acid according to my Invention.
The manufacture comprises, 1st, a furnace a formed with a casing of sheet
iron lined inside with fire-brick; it has at its base a furnace b, arranged in
such manner that the quantity of air introduced gives a maximum product of
carbonic acid.
2d, a washer containing running water c, which enables me to obtain the
gases from the combustion as cold as may be; it has the advantage of
preserving intact the fittings of the pump, and maintaining at a low tempe-
rature the alcaline solutions into which the gases are injected.
3rd, an air pump d for drawing the gases from the fire-place; the size of
the cylinder of this pump must be such that the quantity of air necessary for
the maximun formation of the carbonic acid be brought into the furnace.
4th, a receiving cylinder e, which receives the gases from the combustion
after their cooling; this vessel receives the gases brought by several pumps at

page_text: a time; afterwards it collects the water, which is often drawn from the
washer, then from the working of the pumps; without this cylinder this
addition of water would change in a short time the density of the alcaline
liquors.
5th, the cylinders, the number of which may vary, are intended to effect
the absorption of the carbonic acid by the alcaline solutions; they are placed
horizontally, and furnished with stirrers g; these cylinders are put in com-
munication with one another by tubes of an S shape. On the last cylinder
is placed a pipe i, operating as a chimney to throw into the atmosphere other
gases than the carbonic acid, which combine with the soda or potash as it is
required for the alcaline solution of either of these two bases.
6th, a wood reservoir j, which receives the solution issuing from the last
saturating cylinder.
7th, two pump barrels k, l, mounted on the same column, and which work
alternately, but to attain a different end; the first, k, draws, then forces the
solution of bicarbonate into the separating vessels.
8th, the second, 2, serves to draw off from the separating vessel the solution
injected by the first pump barrel, and become basic again, after having lost by
the action of heat its excess of carbonic acid.
9th, a separating and complex vessel m; it is composed of two parts; the
first is a cylinder n containing a serpentine o for the circulation of steam; it
is provided at its lower part with a tap by which the alcaline liquid is drawn,
with the assistance of one or two pumps k, l, and which has become basic
again after the operation of the separation of the carbonic acid; it carries a
bent tube P, which conveys the carbonic acid and the volatilised water by
heat to the upper part of the appendix to the separating vessel.
10th, this appendix is formed of a cylinder q, carrying a refrigerating
column s, fitted inside with tubes t. The injection of the solution of
bicarbonate of soda is made between the tubest of the refrigerating column.
11th, a serpentine u, serving to cool the alcaline solution deprived of its
carbonic acid in excess before its return to the saturating cylinders.
12th, a bent tube v, terminating in a rose, conveys the liquor into the
interior of the refrigerating tubes.
13th, a serpentine refrigerator x.
14th, a separating vessel r.
15th, a gasometer w.
The foregoing apparatus operate in the following manner :-The furnace b
is suitably charged with coal in combustion and the washing vessel is sunnliad

page_text: with water by opening the cold water inlet tap. The saturating cylinders f
are also partially filled with a solution of sub-carbonate of soda or potash.
The separating vessel m is filled with a similar solution up to about half
the water mark, and the taps by which cold water is admitted into the
serpentine to cool the alcaline solution when it goes out of the separating
vessel after the carbonic acid is separated, being opened, the air pump is put
in motion. The air drawn by this pump d is taken to the under part of the
furr.ace, it arrives by the ash-pit door, and traverses a bed of the incandescent
fuel of a suitable thickness, where it becomes decomposed, and carbonic acid
is formed, & azote disperses without taking care for the other products
which form at the same time. Theses gases of the combustion become cooled
by passing into the washer supplied with running water c, and are injected
into the receiver e, to gain the centre of the alcaline solution contained in the
first cylinder f, then into the second, and so on. During this time care must
be taken to open the steam tap in the serpentine which is contained in the
separating vessel m, and to communicate motion to the pumps k, l, one of
which injects on one side the solution of the bicarbonate of soda or potash
into the separating vessel, while the other takes to the lower pump of the
same vessel for sending it to the first saturating cylinder the liquor which
has become again basic. The continuous movement is established, 1st, for
the simultaneous and incessant passage of the gases from the combustion in
the saturating cylinders f, which enclose the alcaline solutions; 2nd, by the
motion of the stirrers, the action of which never ceases. The gases from
the combustion, and the alcaline liquors to saturate with carbonic acid then
pass from the first cylinder into the second, then sucessively into the third,
and so on to the last; the gases other than the carbonic acid which do not
combine, will escape outside by the pipe i, which conducts them to the roof,
while the solution charged with carbonic acid will flow into the wood
reservoir j. This first part of the operation specially applies to the isolation
of the carbonic acid from other gases, and its absorption by the alcaline
solution. The carbonic acid obtained by this process is of the greatest purity,
since there is no better purifier of carbonic acid than alcalies. The bicarbonate
in liquor obtained by the process I have described, is injected by means of a
pump between the tubest of the refrigerating cylinders, which surmounts
theappendix of the separating vessel by bathing the exterior of the tubes with
it. Having arrived at the upper part of the separating vessel it issues from
it by a bent pipe v, and re-enters into the same cylinder by an aperture
formed in the upper part, from whence it is projected by a number of small
holes into the interior of the refrigerating tubes s, to descend afterwards into

page_text: the cylindrical portion q, of the appendix, from whence it naturally runs into
the principal separating apparatus by a pipe which establishes the equili
brium between the two vessels. The solution of the bicarbonate of soda is
heated to about 212° Fahrenheit, the carbonic acid and steam volatilise at
the upper part of the separating vessel m, to afterwards pass into the cylinder q
of the appendix by the bent tube p; these two substances also re-ascend into
the interior of the refrigerating tubest, when they become in part condensed
by the injection of the solution of the bicarbonate, which takes possession
immediately of the heat from the carbonic and aqueous vapors as much in
the exterior as in the interior of the refrigerating tubes. They come in the last
analysis to terminate their condensation in a lead serpentine x, surrounded
by cold flowing water. The water being condensed as well as the carbonic
acid entirely cooled, they pass finally into a small cylinder r; for this purpose
the water being condensed, returns in the reservoir to the solution of bicar-
bonate of soda, to compensate, that is to say, to restore to liquid, the quantity
of water it has lost by the distillation, in order that the density of the solution
be always the same, and the carbonic acid under the gasometer; then, to
terminate, the alcaline liquor from which the carbonic acid in excess is
separated, returns to the first cylinder by means of the pump, passing from
it by the serpentine, so as to arrive almost cold to the first cylinder, where the
operation of the absorption of the carbonic acid contained in the gases of
the combustion recommences in a continuous manner.
It must be understood that the apparatuses herein-before described are
susceptible of alterations and modifications of form and dimension without
departing from the Invention, for example, the parts may be arranged in any
convenient manner; more or less pumps may be used according to the
importance of the work; also the number of reservoirs may be altered, as well
as the saturators or other parts used in the manufacture of pure carbonic acid,
as before described.
And having now described the nature of my said Invention, and in what
manner the same is to be performed, I declare that I claim,-
First, the manufacture of pure carbonic acid substantially in manner
herein-before described.
Second, the employment of said carbonic acid made as before described to
the preparation of white lead by means of absorption, and in dosing it, if
desired, with carbonic acid as herein-before described.
Third, the employment of carbonic acids made as before described to the
preparation of gaseous liquids, such as seltzer water, soda water, effervescent,
sparkling, or frothy wines, and the like, all as herein-before described.

page_text: Fourth, the preparation of alcaline or other carbonates and bicarbonates, as
herein-before described.
In witness whereof, I, the said George Hyacinthe Ozouf, have hereunto
set my hand and seal, this Twelfth day of December, in the year of
our Lord One thousand eight hundred and sixty-four.
G. H. OZOUF. (L.S.)