IMPROVEMENTS IN THE MANUFACTURE OF SULPHURIC ACID, AND IN APPARATUS CONNECTED THEREWITH
Year: 1869

page_text: LETTERS PATENT to Pierre Adolphe Sidney Langlois, late Manu-
facturer of Chemical Products, and Léon Stanislas Thomassin,
Industrial Chemist, both of 13, Boulevard St. Martin, Paris, for the
Invention of "IMPROVEMENTS IN THE MANUFACTURE OF SULPHURIC ACID,
AND IN APPARATUS CONNECTED THEREWITH."
Sealed the 27th May 1870, and dated the 2nd December 1869.
PROVISIONAL SPECIFICATION left by the said Pierre Adolphe Sidney.
Langlois and Léon Stanislas Thomassin at the Office of the Com--
missioners of Patents, with their Petition, on the 2nd December.
1869.
We, PIERRE ADOLPHE SIDNEY LANGLOIS, late Manufacturer of
Chemical Products, and LÉON STANISLAS THOMASSIN, Industrial Chemist,
both of 13, Boulevard St. Martin, Paris, do hereby declare the nature of
the said Invention for "IMPROVEMENTS IN THE MANUFACTURE OF SULPHURIC.
ACID, AND IN APPARATUS CONNECTED THEREWITH," to be as follows:-
Our improvements in the manufacture of sulphuric acid have for their
object, 1st, a more rapid production of acid; and, 2ndly, to dispense with
most of the leaden chambers usually employed.

page_text: The improved apparatus by means of which we effect the object of our
Invention may be used in the ordinary manufacture of sulphuric acid
from sulphur or pyrites in connection with the ordinary furnaces.
Figure 1 of the accompanying Drawings shows a side elevation of
the apparatus; Figures 2, 3, and 4 being plans of the several parts
detached.
We first produce the vapors of sulphurous acid (SO2) by the aid of
the ordinary furnaces A from either sulphur or pyrites, to which vapors
we supply by the combustion (in the furnace or otherwise) of a nitrate
(such as ordinary nitrate of soda for example) the third equivalent of
oxygen necessary for transforming the sulphurous vapours. (SO) into
sulphurous acid (SO). The vapors of the latter acid pass into a small
lead chamber C, in which if desired a small jet of steam may be intro-
duced. Instead of producing the combustion of the nitrate as above
mentioned we may inject a stream of nitric acid either in chamber C or
if desired in a small additional chamber.
So far the process is the same as usual, but our improvements consist;
1st, in producing the oxidation of the sulphurous acid by means of ozone
as a substitute for the nitric acid or the combustion of a nitrate; and,
2ndly, in the use conjointly with said ozone of the nitrous compounds
above mentioned or the products of their decomposition, such as hypo-
azotic or nitrous acids, bin-oxide of azote, and others. The gases are
withdrawn from chamber C by means of a pump through vertical tubes
at different points, the lower ends of said tubes communicating with a
lead chamber placed below chamber C. A pump H constructed of
materials not liable to be acted on by acids (such as lead, regulus of
antimony, and lead lined or not with platinum, gutta percha, vulcanized
rubber, or other substance) supplies the sulphuric vapors (or sulphurous
vapors, as will be herein-after explained), and other gases or vapors
formed and contained in chamber C to the tube receiver placed below
said chamber, whence they are forced into cylinder J. This cylinder
consists of a closed apparatus similar to a steam generator and capable
of withstanding a pressure of several atmospheres. It is likewise con-
structed of materials not acted on by acids and provided with safety
valves, guages, and other similar appurtenances. This cylinder contains
a depth of water dependent approximately on the degree of concentration
of the acid desired. The vapors of sulphuric (or sulphurous) acid.
(as herein-after explained) are injected under pressure in the water in.

page_text: cylinder J, and with which they quickly combine owing to the great
affinity of the gazeous sulphuric acid therefor. In this manner hydrated
sulphuric acid of commerce is quickly produced in at least as con-
centrated a condition as the acid from the leaden chambers now in use.
The generator cylinder J is provided with a tube K lined with lead or
other material not acted on by the acids and fitted with an escape valve
for discharging the vapors of azote, hypo-azotic and nitrous acids, or
bin-oxide of azote and other vapors remaining uncombined (and which
might create a pressure in the generator) into what is known as a Gay
Lussac's cascade L, where the concentrated sulphuric acid absorbs the
nitrous gases, leaving those which are inert to pass away by a chimney.
The sulphuric acid charged with the nitrous gases above mentioned is
then passed through a column R of stone used for extracting the nitrous
gases; or the same result may be attained by the aid of a jet of steam,
after which they are returned to the chamber. C. to contribute anew to
the oxygenation of the sulphuric acid..
Instead of water being used in the generator J we may introduce
therein oxygenated water or bin-oxide of hydrogen. This arrangement
not only enables pipe K and cascade L to be dispensed with, but also
the combustion of the nitrate in or out of the furnaces and the cascade
of nitric acid in chamber C.
The pump is operated either by hand or steam power, according to the
extent of the manufacture, since by the modified arrangements of the
apparatus according to our Invention, which occupies but small space,
from five to six bottles (60 to 70 gallons) only of sulphuric acid may be
produced per twenty-four hours. Further, if sulphur be used instead of
sulphurous pyrites the manufacture may be intermittent instead of
A, furnace for the combustion of sulphur or pyrites; A', pipe for
conveying the gases from furnace A; B, connection between pipe S and
the column of stone before referred to; B', pipe for conducting the
gases to lead chamber C; D, pipes through which the gases pass from
chamber C to receiver E; F, pipe through which gases pass to the
pump; G, steam generator and engine; H, pump; I, pipe for con-
ducting the gases from the pump to the cylinder J, forming a generator

page_text: of the sulphuric acid; K, valve and discharge pipe through which the
inert and other gases pass from the generator J to the Gay Lussac
cascade L; M, case containing acid for the supply of L; M', reservoir
for the supply of M; N, pipe through which are discharged the inert
gases separated in the cascade L; O, glazed opening by the aid of which
the color of the gases discharged at pipe N may be ascertained; O¹,
opening at which the gases may be tested; P, flue for conveying the
gases to the draft chimney; Q, pipe through which the acid charged
with nitrous gases passes to the column R; S, pipe for returning the
nitrous vapours set at liberty in column R; T, reservoir of manufactured
acid; U, water guage; V, drawing-off cock.
Our Invention of improvements in the manufacture of sulphuric acid
also consists, 1st, in the use of a pump H constructed of materials not
affected by acids for raising the gazeous sulphuric acid contained in
chamber C into generator J; 2ndly, in the application of a cylinder or
generator J of similar materials to C for containing pure or oxygenated
water (bin-oxide of hydrogen) and to which the sulphuric vapors are
supplied under pressure by pump H, said cylinder (which should be
capable of withstanding a pressure of several atmospheres) being provided
with the necessary safety valves and other adjuncts.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Pierre Adolphe Sidney Langlois and Léon Stanislas
Thomassin in the Great Seal Patent Office on the 30th May 1870.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, PIERRE
ADOLPHE SIDNEY LANGLOIS, late Manufacturer of Chemical Products,
and LÉON STANISLAS THOMASSIN, Industrial Chemist, both of 13,
Boulevard St. Martin, Paris, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent bearing date the Second day of December, in the year of
our Lord One thousand eight hundred and sixty-nine, in the thirty-third
year of Her reign, did, for Herself, Her heirs and successors, give and
grant unto us, the said Pierre Adolphe Sidney Langlois and Léon
Stanislas Thomassin, Her special licence that we, the said Pierre Adolphe
Sidney Langlois and Léon Stanislas Thomassin, our executors, adminis-
trators, and assigns, or such others as we, the said Pierre Adolphe Sidney

page_text: Langlois and Léon Stanislas Thomassin, our 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 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
OF SULPHURIC ACID, AND IN APPARATUS CONNECTED THEREWITH," upon the
condition (amongst others) that we, the said Pierre Adolphe Sidney
Langlois and Léon Stanislas Thomassin, our executors or adminis
trators, by an instrument in writing under our, or their, or one
of 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 we, the said Pierre Adolphe Sidney Langlois
and Léon Stanislas Thomassin, 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 state-
ment, reference being had to the three Sheets of Drawings hereunto
annexed, and to the letters and figures marked thereon (that is
to say):
-
Our improvements in the manufacture of sulphuric acid have for their
object, 1st, a more rapid production of acid; and, 2ndly, to dispense
with most of the leaden chambers usually employed.
The improved apparatus by means of which we effect the object of
our Invention may be used in the ordinary manufacture of sulphuric
acid from sulphur or pyrites in connection with the ordinary furnaces.
Figure 1 of the accompanying Drawings shows a side elevation of the
apparatus; Figures 2 and 3 being views of parts detached.
We first produce the vapors of sulphurous acid (SO) by the aid of the
ordinary furnaces A from either sulphur or pyrites, to which vapors we
supply by the combustion (in the furnace or otherwise) of a nitrate (such
as ordinary nitrate of soda, for example) the third equivalent of oxygen
necessary for transforming the sulphurous vapors (SO) into sulphurić
acid (SO). The vapors of the latter acid pass into a small lead
chamber C, in which if desired a small jet of steam may be introduced;
Instead of producing the combustion of a nitrate as above mentioned

page_text: we may me
in a small additional chamber.
=
So far the process is the same as usual, but our improvements con-
sist, 1st, in effecting the oxidation of the sulphurous acid by means of
ozone as a substitute for the nitric acid or the combustion of a nitrate;
and, 2ndly, in the use conjointly with said ozone of the nitrous compounds
above mentioned or the products of their decomposition, such as
hypo-azotic or nitrous acids, bin-oxide of azote and others. The gases are
withdrawn from chamber C by means of a pump through vertical tubes
at different points, the lower ends of said tubes communicating with a lead
chamber placed below chamber C. A pump H constructed of materials not
liable to be acted on by acids (such as lead, regulus of antimony, and lead
lined or not with platinum, gutta percha, vulcanized rubber, or other
substance) supplies the sulphuric vapors (or sulphurous vapors as will
be herein-after explained) and other gases or vapors formed and con-
tained in chamber C to the tube receiver placed below said chamber,
whence they are forced into cylinder J. This cylinder consists of a
closed apparatus similar to a steam generator and capable of with-
standing a pressure of several atmospheres; it is likewise constructed of
materials not acted on by acids and provided with safety valves, guages,
and other similar appurtenances. This cylinder contains a depth of
water dependent approximately on the degree of concentration of the
acid desired. The vapors of sulphuric (or sulphurous) acid (as herein-
after explained) are injected under pressure in the water in cylinder J,
and with which they quickly combine owing to the great affinity of the
gazeous sulphuric acid therefor. In this manner hydrated sulphuric
acid of commerce is quickly produced in at least as concentrated a
condition as the acid from the leaden chambers now in use.
generator cylinder J is provided with a tube K lined with lead or other
material not acted on by the acids and fitted with an escape valve for
discharging the vapors of azote, hypo-azotic and nitrous acids, or bin-
oxide of azote, and other gases or vapors remaining uncombined (and
which might create a pressure in the generator) in what is known as a
Gay Lussac's cascade L, where the concentrated sulphuric acid absorbs
the nitrous gases, leaving those which are inert to pass away by a
chimney. The sulphuric acid charged with the nitrous gases above
mentioned is then passed through a column R of stone used for
extracting the nitrous gases by the aid of a jet of steam, after which
The

page_text: they are returned to the chamber C to contribute anew to the
oxygenation of the sulphuric acid.
Instead of pure water being used in the generator J we may introduce
therein oxygenated water or bin-oxide of hydrogen, by which means the
combustion of the nitrate in or out of the furnaces and the cascade of
nitric acid in chamber C are dispensed with. The pump is operated
either by hand, steam, or other power, according to the extent of the
manufacture.
Sheet 1 of the accompanying Drawings represents an elevation of the
whole series of the apparatus for the manufacture of sulphuric acid;
according to our improvements; Sheet 2 is a plan of the apparatus; and
Sheet 3, a longitudinal section of chamber C on an enlarged scale.
A, furnace for the combustion of sulphur or pyrites; A¹, pipe for
conveying the gases from furnace A.; B, connection between pipe S and
the column of stone before referred to; B', pipe for conducting the gases
to lead chamber C; D, pipes through which the gases pass from
chamber C to receiver E; F, pipe through which the gases pass to the
pump; G, steam generator and engine; H, pump; I, pipe for con-
ducting the gases from the pump to the cylinder J forming a generator
of the sulphuric acid; K, discharge pipe provided with a valve, through
which the inert and other gases pass from the generator J to the Gay
Lussac cascade L; M, case containing acid for the supply of L; M',
reservoir for the supply of M; N, pipe through which are discharged the
inert gases separated in the cascade L; O, glazed opening, by the aid of
which the color of the gases discharged at pipe N may be ascertained;
O', opening at which the gases may be tested; P, flue for conveying the
gases to the draft chimney; Q, pipe through which the acid charged
with nitrous gases passes to the column R; S; pipe for returning the
nitrous vapors set at liberty in column R; T, reservoir of manufactured
acid; U, water guage; V, drawing-off cock..
The advantages to be derived from the adoption of the herein-before
described improvements are, 1st, the saving of time as compared with
that required by the ordinary processes for the manufacture of sulphuric
acid; 2ndly, the saving of space occupied by the lead chambers; and,
3rdly, the saving of expense incurred in providing lead chambers.

page_text: Having described the nature of our Invention, and the manner of
performing the same, we would observe that we do not limit ourselves to
the precise form and dimensions of the pump or generator or their
accessories, and that we reserve the right of making such modifications
or improvements in the apparatus as experience may determine without
departing from our Invention, and that what we claim as our Invention
to be protected by the herein-before in part recited Letters Patent is,-
1st. The application of ozone, either alone or conjointly with the
combustion of a nitrate, or the introduction of nitric acid (or the
products of decomposition of such nitrous compounds) for converting
sulphurous acid into sulphuric acid, all as herein-before described.
2ndly. We claim the improved arrangement of apparatus illustrated in
the accompanying Drawings to be used in the above manufacture, the
chief features of which are, 1st, the lift and force pump H constructed
of materials not affected by acids for raising the gaseous sulphuric acid
and other vapors contained in chamber C into generator J; 2ndly, the
cylinder or generator J of similar materials to C for containing water,
which may be oxygenated (bin-oxide of hydrogen), and to which the
sulphuric vapors are supplied under pressure by pump H, said cylinder
(which should be capable of withstanding a pressure of several atmo-
spheres) being provided with the necessary safety valves and other
adjuncts, all as herein-before explained.
In witness whereof, we, the said Pierre Adolphe Sidney Langlois
and Léon Stanislas Thomassin, have hereunto set our hands and
seals, this Twentieth day of May, in the year of our Lord One
thousand eight hundred and seventy.