AN IMPROVED AND ECONOMICAL METHOD OF MANUFACTURING SULPHURET OF CARBON AND SULPHURIC ACID FROM THE PYRITES OF IRON AND COPPER SIMULTANEOUSLY, AND IN THE APPARATUS FOR THE PURPOSE OF SUCH MANUFACTURE
Year: 1879

page_text: LETTERS PATENT to Elie Célestin Ernest Labois and Léon Louis Labois,
Chemists, both of the City of Paris, in the Republic of France, for the
Invention of "AN IMPROVED AND ECONOMICAL METHOD OF MANUFACTURING
SULPHURET OF CARBON AND SULPHURIC ACID FROM THE PYRITES OF IRON AND
COPPER SIMULTANEOUSLY, AND IN THE APPARATUS FOR THE PURPOSE OF SUCH
MANUFACTURE"
Sealed the 16th April 1880, and dated the 27th October 1879.
PROVISIONAL SPECIFICATION left by the said Elié Célestin Ernest Labois
and Léon Louis Labois at the Office of the Commissioners of Patents on the
27th October 1879.
ELIE CÉLESTIN ERNEST LABOIS and LÉON LOUIS LABOIS, Chemists, both of the
City of Paris, in the Republic of France. "AN IMPROVED AND ECONOMICAL
METHOD OF MANUFACTURING SULPHURET OF CARBON AND SULPHURIC ACID FROM
THE PYRITES OF IRON AND COPPER SIMULTANEOUSLY, AND IN THE APPARATUS FOR
THE PURPOSE OF SUCH MANUFACTURE."
The object of the process forming the subject of the present Invention is to
extract by distillation of the pyrites the greatest possible amount of sulphur till
distillation ceases to yield further, and the incandescent and irreducible residues are
immediately transferred to a second apparatus, connected with the first by a pipe
where they are used to extract from them sulphuric acid.
The apparatus consists of a distilling retort with three branches or tubes con-
nected to an appropriate furnace supplied from above with the pyrites and charcoal
to be distilled, and conducting the gases in a pipe to a furnace heated with charcoal
for making the sulphuret of carbon, and discharging from itself the red hot residues
by a branch pipe below to the grates of the sulphuric acid making apparatus by a
pipe of refractory clay or iron.
The pipe connecting the distilling retort with the grate of the sulphuric acid
apparatus avoids all loss of heat, and if necessary can be replaced by a barrow
closing so as to retain the heat, and thus conducting the hot residues to the second
apparatus. This pipe is hermetically closed and abuts on the furnace of the second
apparatus, where the residues are treated for the extraction of the 25 to 30 per cent.
of sulphur that the pyrite residues still contain. A chimney communicating with
this furnace opens into a cylinder where the dust is deposited, and the gases enter
by an iron tube in a lead pipe. In this latter the impure gases are collected, and
in other pipes the purified gases as usually practiced by known methods.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said Elié Célestin Ernest Labois and Léon Louis Labois in the Great Seal
Patent Office on the 23rd April 1880.
ELIE CÉLESTIN ERNEST LABOIS and LÉON LOUIS LABOIS, Chemists, both of the
City of Paris, in the Republic of France. "AN IMPROVED AND ECONOMICAL
METHOD OF MANUFACTURING SULPHURET OF CARBON AND SULPHURIC ACID FROM
THE PYRITES OF IRON AND COPPER SIMULTANEOUSLY, AND IN THE APPARATUS FOR
THE PURPOSE OF SUCH MANUFACTURE."
Sulphur in a pyretic state is more difficult to extract by distillation than when
it is held in solfatara earth, and if the operation is carried to completion, after a
great consumption of fuel, the result would merely be to extract from 100 kilo-
grammes of chemically pure pyrites about 26 to 27 kilogrammes of sulphur. The
pyrites only containing from 40 to 40% of sulphur, by this method from 20 to 23
kilogrammes is all that is obtained.
The object of this Invention is to extract by distillation of the pyrites the
greatest possible amount of sulphur until distillation ceases to be remunerative, which
will occur when the first equivalent of sulphur is nearly eliminated, and then
immediately afterwards to use the irreducible residue whilst still hot in the manu-
facture of sulphuric acid.
From the successive operations to which the pyrites are submitted a considerable
saving of raw material, labour, and fuel results.
In the accompanying Drawings, as example, an apparatus is shown capable of
practically effecting the objects above mentioned.
Fig. 1 is a vertical section of an apparatus for manufacturing sulphate of carbon;
Fig. 2, which is connected to the preceding by a canal or filter, also shows in
section the first apparatus requisite for obtaining the sulphuric acid. In a suitable
furnace a a retort of refractory earth is arranged, or it may be of sheet iron
japanned supplied with three branches c, d, and f. The upper branch c is con-
tinued by a hopper e, furnished with a plug e¹, and in which the pyrites to be
treated are emptied. The second branch d is continued by a conduit d', below
which is the wood charcoal retort g; the conduit d¹ when desired is intercepted by
the damper d. Finally, the third branch f, or lower one, is continued by a canal h
in refractory earth or in cast iron, closed as hermetically as possible, and which
establishes the connexion of the retort b with the first apparatus for the production
of the sulphuric acid. In connecting the retort b to the furnace i one can, for
example, employ the tube k, of cast iron, with damper r or any other suitable
contrivance. The canal h abuts on the furnace i, which is continued by a
chimney j; this debouches in the furnace 7, where the dust which is drawn along
is deposited; thence the gases arrive by a cast iron pipe m into a first leaden
cylinder where the impure gases are collected, and in succeeding cylinders where
the purified gases are collected, as is now practised by known methods. During
the first operation the tube k, which can leave the end of the channel h free, is
merely closed by the japanned register r, or by this register and a cover of
refractory earth, which is destroyed before the connection of the channel h and the
opening of the register. From an opening ad hoc hit is easy to unstop the canal f
of the retort and draw down the pyrites with a poker or other implement. In the
distilling retort 6 the pyrites are placed in sufficient quantity, heat is then applied
by the combustion of charcoal charged through the orifice o. The vapours dis-
engaged pass through the tube d, thence to be submitted to the influence of the
incandescent coal at d³, and so produce sulphuret of carbon, which is then followed
by the usual operations. The wood charcoal in the first retort b may be partly
mixed, but care must be taken not to beat the first retort at too high a temperature
to avoid melting the mineral and destroying the retort. When sulphur only is to

page_text: be obtained the conduit & leads the vapours in a condensing chamber as is usually
practiced. When the pyrite has parted with about 15% of its weight, or 15 kilo-
grammes of sulphur for 100 kilogrammes of pyrites and more (which will be
experimentally determined) the register d¹¹ is closed, and having removed the
refractory earth cover of the tube k, the branching or connecting of the tube h
being effected, the register is opened to make the hot pyrites slide down the
tube h to the grates of the pyrites for making sulphuric acid. The whole of the
first equivalent may be removed, but, as observed, caution is necessary to avoid
melting the mineral; for this reason a mean distillation of 15% is taken for rich
pyrites at 45% of sulphur. It is scarcely necessary to remark that the distilling
retort b is placed above the grate, and separated from it by a more or less length
of channel or pipe, and is also isolated by a division or wall. It has been observed
that before opening the register r for discharging the hot pyrites the register dll
is closed to prevent the entrance of gas in the retort. When the retort b is dis-
charged is closed, and the mineral is introduced at e¹. The retort being filled to
a suitable height it is closed and luted above and below, the register du having
been opened and the operation recommenced. The determination of the time
necessary for obtaining the 12 to 15% of sulphur (and more) from the pyrites in
the first operation is obtained with respect to the dimensions of the apparatus, the
intensity of the heat of the fire, the nature of the mineral, and so forth. In other.
respects it is of little importance as what is lost in the first operation is regained by
the second. The pyrites leaving the retort b reach the grates by the pipe h, with
a coefficient of heat far superior to that of the grates. Regaining oxygen from the
surrounding air and from the bellows they leave in the next apparatus, and the
furnaces ad hoc the 25 to 30% of sulphur they still contained.
Observations. The Fig. 3 represents a longitudinal section of an apparatus for
the manufacture of sulphuret of carbon, and which we reserve the right to sub-
stitute for the Fig. 1. The conduit d of the principal apparatus debouches at d
and leads the gas in contact with the first layer of wood charcoal, thence it
circulates in the compartments, also supplied with wood charcoal, to flow in the
form of sulphuret of carbon by the pipe p. The advantage of this apparatus is
that in a small compass it admits of a long course to the vapours freed by the
distillation of the pyrites. Fig. 4 shows a reservoir in refractory earth in which
the hot pyrites are discharged by the pipes h, h, h, from the distilling apparatus,
Fig. 1, and from which the said pyrites are led by the pipe q still kept hot to the
grates. This reservoir admits if it is necessary of conducting the two operations
of distillation and calcining the pyrites independently of one another, whilst at the
same time always keeping the pyrites hot and profiting by the heat acquired for
the economical and subsequent manufacture of sulphuric acid. In place of the
conduit h, Figs. 1 and 2, if local requirements necessitated too great separation of
the two apparatus, then the hot pyrites can be transported by a closed barrow, a
specimen of which is shown at Fig. 5, or any other suitable contrivance may be
used. Again, instead of treating the pyrites by a first operation in the distilling
retort of a special apparatus, and then by a second operation immediately succeeding
it, in apparatus for making sulphuric acid one can as before profit by the economy
resulting by the immediately succeeding operations, that is to say, take advantage
of the heat the residues possess from the first operation by proceeding as follows:-
In a suitable retort a first distillation is effected in the limits above assigned,
evacuating the products of this distillation by a conduit similar to that of d in the
first apparatus; then closing this conduit, or a similar one is opened to those of the
sulphuric acid apparatus, air is introduced to the residues requisite to encourage
the utmost elimination of sulphur they contain. In a word, the two operations
succeeding each other can be effected in a single apparatus, first serving for dis-
tillation and then calcining.
Finally, we consider and claim as our Invention,-
1st. The novel idea of first extracting from a determined quantity of pyrites a
certain amount of sulphur in immediately conducting the hot residues to the grates,

page_text: that is to say, draw by distillation of the pyrites all the sulphur or the greatest
part thereof from the first equivalent, and directly use the hot residues in the
manufacture of sulphuric acid in making with the sulphur either sulphuret of carbon
or flour of sulphur or other commercial product.
2nd. The apparatus, shown as example by the Drawings, consisting of a distilling
retort with three branches or tubes situated in an appropriate furnace and receiving
the pyrites to be distilled from above (and, if necessary, wood charcoal), conducting
the gases to a wood charcoal furnace by a conduit for making sulphuret of carbon,
then getting rid of the residues heated through the lower conduit, which is
continued to the grates of the sulphuric acid apparatus by a channel of refractory
earth or sheet iron.
3rd. The conduit, establishing the connexion of the distilling retort and the
grates of the furnace of the sulphuric acid apparatus, preventing any loss of
heat, and if necessary capable of being replaced by a special barrow or other
contrivance.
4th. We claim the exclusive right of making in a single apparatus the two
principal and successive operations above mentioned.
5th. It should be clearly explained that we intend our rights to extend to and
claim the use of our apparatus for obtaining by distillation of the pyrites of iron,
copper, and galena, sulphuret of carbon and sulphuric acid, and any other product
that the said pyrites may contain, especially sulphur and its derivities, always
simultaneously with sulphuric acid.
In witness whereof, we, the said Elie Célestin Ernest Labois and Léon Louis
Labois, have hereunto set our hands and seals, this Nineteenth day of April,
in the year of our Lord One thousand eight hundred and eighty.
(L.S.)
LÉON LOUIS LABOIS.
(L.S.)