Improvements relating to the Treatment of Sulphur-ores, Crude Sulphur, Ozokerites, Heavy Oils of Petroleum, and other Materials for Extracting, Purifying, or Refining Purposes, and to Apparatus for use therein.
Year: 1891

page_text: Date of Application, 9th June, 1891
Complete Specification Left, 9th Mar., 1892-Accepted, 9th June, 1892
PROVISIONAL SPECIFICATION.
Improvements relating to the Treatment of Sulphur-ores, Crude
Sulphur, Ozokerites, Heavy Oils of Petroleum, and other
Materials for Extracting, Purifying, or Refining Purposes, and
to Apparatus for use therein.
I, LEON LABOIS, of 95, Boulevard Beaumarchais, Paris, in the Republic of
France, Engineer, do hereby declare the nature of this invention to be as
follows:-
My invention relates to the treatment of sulphur-ores, crude sulphur, ozokerites,
heavy oils of petroleum, and other materials for extracting, purifying or refining
purposes, and to apparatus for use therein
According to my said invention I extract by centrifugal action or removal of
the liquid, with the help of steam under pressure, substances which can be separated
in the liquid state by elevation of temperature of the gangues, ores, or raw
materials in general, which contain them.
In order to render the object of my invention clearly understood I will take the
case of sulphur. If the temperature of an earthy or other sulphur ore is raised
to 115 degrees there will be fusion in the mass. By physical means such as the.
pressure produced by a press or by centrifugal action in a turbine, the liquid
sulphur can then be separated from the gangue which will remain in the basket or
pannier of the turbine.
What I have stated about sulphur ores applies evidently also for example
to industrial residues from gas works and to crude sulphur from which all the
impuritics can be extracted by similar treatment in the turbine or pressure at a
high temperature. Moreover my invention enables earth wax or natural paraffins
known by the name of ozokerites to be treated under similar conditions as sulphur.
In fact the materials which can be separated from gangue become liquid between
39 and 63 degrees.
It is the same for treating heavy oils of petroleum and the like. In each of the
cases it will be sufficient to graduate the temperature and thus two substances may
be separated which have approximate melting points.
I will hereinafter describe how the operations are carried out in the case of
sulphur ores.
The centrifugal apparatus which I employ for this purpose comprises a vessel or
chamber provided with a curved bottom so as to present a space for holding a
certain quantity of liquid but this space need not be great owing to the employ-
ment of a reservoir for the liquid extracted. The said vessel or chamber is pro-
vided with a steam casing in order to obviate cooling and therefore resolidification
in the interior of the apparatus.
Movement may be imparted to the basket or pannier by means of a motor
adapted to the apparatus, or from any suitable shaft. In either case this move-
ment is transmitted to a vertical shaft through the medium of friction cones made
of compressed paper or any other suitable material or simply by a grooved pulley
keyed upon the said vertical shaft.
The steam designed for heating under pressure enters through a tube and
terminates at the bottom of the aforesaid vessel or chamber below the basket
or pannier or at any other point of the vessel or chamber, preferably at its
lower part.
A steam inlet is also arranged in the outer casing or mantle of the vessel or
chamber of the centrifugal apparatus and a tube serves for the outlet of this steam
which is expanded.

page_text: 1
.
The various vapours and gases issuing from the interior of the vessel or chamber
of the centrifugal apparatus escape through a tube arranged at the upper part. In
the case of very heavy charges upon the basket or pannier the apparatus is
strengthened. For this purpose the vessel is provided with cross-pieces or arms
for holding the rotary axis at its upper part. Any displacement of this axis will
thus be obviated, and the deformation of the basket or pannier can be prevented
by providing it with similar arms or cross-pieces.
A receptacle is provided for the molten sulphur and the water of condensation
produced during the centrifugal action until the withdrawal takes place.
This receptacle is surrounded by a jacket for steam under pressure in order to
prevent cooling.
The various cocks for the operation and withdrawal are likewise arranged for
the circulation of steam to avoid any obstruction, and the outlet tube for the
sulphur is arranged in such a manner that the steam cannot escape with the sulphur
from the above-mentioned receptacle.
The employment of this receptacle has the effect of preventing too great dimen-
sions of the vessel or chamber below the basket or pannier. The molten sulphur
flows into this receptacle in proportion as it is produced so that the bottom
of the said vessel or chamber, not holding any liquid, does not require a steam
casing, which diminishes the difficulties and price of construction of the
apparatus. This receptacle may be arranged so as io form as it were an
enlargement of the discharge pipe. As above stated it is provided with a
steam casing or jacket for preventing the solidification of the sulphur con-
tained in it.
This receptacle has a capacity corresponding to the quantity of raw material
treated in each centrifugal action which is on an average from 200 to 250 kilo-
grammes plus the water of condensation, which gives for this receptacle a total
quantity of from 70 to 80 litres at most with a very rich ore.
The apparatus is charged by means of closed sacks conveyed quite full to the
attendant. The attendant takes the sacks and arranges them in two or three
rows quite up to the edge of the basket or pannier. Stop bars fixed vertically
upon the bottom of the basket or pannier at distances of about forty
centimetres apart prevent the arrangement of these sacks being changed during
the operation so that the basket or pannier will be perfectly equilibrated at any
moment.
The sacks are simple cylinders of cloth having a diameter and length suitable
for the apparatus. These cylinders are pressed at their two extremities by a
string or in any other similar manner. A large iron ring sewed to the cloth serves
for moving the sacks. For this purpose the attendant holds an iron hook which
he causes to engage with the said ring, he thus avoids being burnt and does not
therefore require to wait until the materials remaining in the sacks have had time
to cool in the basket or pannier. According to the meshes in the cloth which
composes them, the sacks constitute more or less tight filters so that it is easy to
obtain liquids which are perfectly clean and totally free from any trace of dust or
powder of the original gangue. After the charging of the sacks in the basket or
pannier the vessel or chamber of the apparatus is hermetically closed at its upper
part by a cover. This movable cover is united with the body of the vessel or
..chamber by means of bolts turning each upon an axis fixed to the vessel or
*chamber. These bolts are placed in corresponding notches formed in the two
flanges that on the vessel or chamber and that on the cover, an india-rubber ring
being placed between these flanges to ensure tightness. Thumb nuts serve to hold
the aforesaid bolts in their respective notches.
The apparatus is provided with thermometers, pressure gauges, valves, and a
series of discharge cocks.
The cover may be moved in any suitable manner, but it is preferably suspended.
"from a chain having a counterweight, which chain passes around guide-pulleys
and is wound upon a small windlass. This arrangement enables the opening

page_text: and closing of the above-named vessel or chamber to be effected with ease and
rapidity.
To economize as much as possible the steam for the heating I prefer to use an
arrangement which enables the passage of the steam from the vessel or chamber of
one centrifugal apparatus through the pipe to that of the second apparatus, a
three-way cock serving to establish at will the communication between the two
apparatus on allowing the escape of the steam from one of them directly into the
atmosphere whilst other apparatus is isolated. In this case of conjugated apparatus
a single receptacle may be provided for the liquid extracted below this receptacle
being placed a receiving vessel heated from below.
The operation is conducted in the simplest manner, either the thermometer or
the pressure gange being observed and the temperature of the steam may be
optionally varied by the employment of an expansion device placed at any desired
point of the distributing tube.
As above stated the operation takes place in the same manner, if, in lieu of
sulphur ore, crude sulphur has to be refined, and also in case the industrial treat-
ment of ores and raw materials such as ozokerites, paraffins, heavy oils of petroleum
and the like is to be effected with the object of extracting from them liquefiable
materials susceptible of being separated from the crude mass by an elevation of
temperature and by centrifugal action as hereinbefore set forth for sulphur. In
each case it is sufficient to know the temperature at which each of the substances
to be separated becomes liquid. As will be readily understood a series of extrac-
tions can be effected in succession by modifying the temperature, commencing with
the extraction of the substance having the lowest melting point to finish with that
of the substance having the highest melting point.
Dated this 9th day of June 1891.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements relating to the Treatment of Sulphur-ores, Crude
Sulphur, Ozokerites, Heavy Oils of Petroleum, and other
Materials for Extracting, Purifying, or Refining Purposes, and
to Apparatus for use therein.
I, LEON LABOIs, of 95, Boulevard Beaumarchais, Paris, in the Republic of
France, Civil Engineer, do hereby declare the nature of this invention and in what
manner the same is to be perforined, to be particularly described and ascertained
in and by the following statement :-
My invention relates to the treatment of sulphur-ores, crude sulphur, ozokerites,
heavy oils of petroleum, and other materials, for extracting purifying or refining
purposes, and to apparatus for use therein.
According to my said invention I extract by centrifugal action or removal of the
liquid, with the help of steam under pressure, substances which can be separated in
the liquid state by elevation of temperature of the gangues, ores, or raw materials
in general, which contain them.
In order to render the object of my invention clearly understood I will take the
case of sulphur. If the temperature of an earthy or other sulphur ore is raised
to 115 degrees C. there will be fusion in the mass. By physical means, such as the
pressure produced by a press; or by centrifugal action in a suitable machine, the
liquid sulphur can then be separated from the gangue which will remain in the pan
of the machine.
What I have stated about sulphur ores applies evidently also, for example, to
industrial residues from gas works and to crude sulphur from which all the impurities
can be extracted by similar treatment in the machine or under pressure at a high
temperature. Moreover, my invention enables mineral waxes or natural paraffins

page_text: In each of the
It is the same for treating heavy oils of petroleum and the like.
cases it will be sufficient to graduate the temperature, and thus two substances may
be separated which have approximate melting points.
I will hereinafter describe how the operations are carried out in the case of
sulphur ores.
In the accompanying drawings I have shown how my said invention may be
conveniently and advantageously carried into practice.
Figure 1 is a vertical section through the axis of rotation of the pan of the
machine.
Figure 2 is an elevation of the same.
Figure 3 is a plan.
Figure 4 is a modification of Figure 1.
Figures 5, 6 and 7 show respectively a front elevation a plan and a vertical
transverse section of two centrifugal machines connected with the same drawing off
reservoir.
Figures 1, 2 and 3 represent my apparatus as used for industrial purposes.
The centrifugal apparatus which I employ for this purpose comprises a vessel or
chamber A provided with a curved bottom a so as to present a space for holding a
certain quantity of liquid, but this space need not be great owing to the employ-
ment of a reservoir for the liquid extracted. The said vessel or chamber is provided
with a steam casing C in order to obviate cooling and therefore resolidification in
the interior of the apparatus.
Movement may be imparted to the pan by means of a motor D adapted to the
apparatus, or from any suitable shaft d. In either case this movement is transmitted
to a vertical shaft d' through the medium of friction cones FF'made of compressed
paper or any other suitable material or simply by a grooved pulley keyed upon the
said vertical shaft.
The steam designed for heating under pressure enters through a tube t
terminating at the bottom of the aforesaid vessel or chamber below the pan as
shown in Figure 1 or at any other point of the vessel or chamber preferably at its
lower part.
A steam inlet is also arranged in the outer casing or mantle of the vessel or
chamber in the centrifugal apparatus and a tube serves for the outlet of this
steam when expanded.
The various vapours and gases issuing from the vessel or chamber of the
centrifugal apparatus escape through a valve W arranged at the upper part. In
the case of very heavy charges the pan of the apparatus is strengthened. For
this purpose the vessel is provided with cross-pieces or arms for holding the rotary
axis at its upper part. Any displacement of this axis will thus be obviated and
the deformation of the pan can be prevented by providing it with similar arms or
cross pieces.
A receptacle R. Figures 1. 2. 3 is provided for the molten sulphur and the
.water of condensation produced during the centrifugal action until their withdrawal
takes place.
This receptacle R is surrounded by a jacket m for steam under pressure in order
to prevent cooling (Figure 4).
The several cocks for facilitating the various operations are arranged for the
circulation of steam so as to avoid any obstruction and the outlet tube for the sulphur
is arranged in such a manner that the steam cannot escape with the sulphur from
the above mentioned receptacle.
The employment of this receptacle Robviates the necessity for the use of a
vessel or chamber of any considerable size below the pan. The molten sulphur
flows into this receptacle R as it is produced so that the bottom of the said vessel
or chamber not holding any liquid does not require a steam casing which obviates

page_text: many difficulties and decreases the cost of construction of the apparatus. This
receptacle may be arranged as shown in Figure 4 so as to form as it were an
enlargement of the discharge pipe. As above stated it is provided with a steam
casing or jacket m for preventing the solidification of the sulphur contained in it.
In the second mode of construction as represented in Figure 4, this receptacle
has a capacity corresponding to the quantity of raw material, treated at each
operation of the machines which is on an average from 200 to 250 kilogrammes
plus the water of condensation which gives for this receptacle a total capacity of
from 70 to 80 litres at most with a very rich ore. The receptacle is provided
with an outlet cock as at P and with a steam casing. The cock is operated by a
hand wheel actuating the piston by means of the rod 7. The sulphur escapes
at q. constitutes the casing for the steam which escapes through the cock
arranged for this purpose at the lower part of the said casing.
The apparatus is charged by means of closed sacks conveyed quite full to the
attendant he then arranges the said sacks in two or three rows up to a level with
the edge of the pan. Stop bars, not shown in the figures, fixed vertically upon
the bottom of the pan at distances of about forty centimetres apart, prevent the
disarrangement of these sacks during the process so that the pan will be perfectly
balanced at any one moment.
The sacks are plain cylinders of cloth having a diameter and length suitable
for the apparatus the said sacks being secured at their two extremities by a string
or in any other similar manner. A large iron ring sewed to the cloth serves for
handling the sacks. For this purpose the attendant holds an iron hook with which
he moves the sacks about by the aid of the said ring, he thus avoids being burnt
and does not therefore require to wait until the materials remaining in the sacks
have had time to cool in the pan. According to the size of the meshes in the
cloth which composes the said sacks they constitute more or less closed filters so
that it is easy to obtain liquids which are perfectly clean and totally free from any
trace of the dust or powder of the original gangue. After the charging of the
sacks in the pan the vessel or chamber of the apparatus is hermetically closed at its
upper part by a cover A'. This movable cover is united with the body of the
vessel or chamber by means of bolts B turning each upon an axis o. fixed to the
vessel or chamber (see Fig. 1). These bolts are placed in corresponding notches ec
formed in the two flanges so that on an india rubber ring being placed between the
flanges of the vessel and the cover, and the thumb nuts E screwed up a tight joint
will be formed (see Figs. 1, 2, 3).
The apparatus is provided with thermometers, pressure gauges M. valves S and
a series of discharge cocks.
The cover may be moved in any suitable manner but it is preferably suspended
from a chain 1 having a counterweight, which chain passes around guide pulleys 3, 3,
and is wound upon a small windlass 2 as represented in Fig. 5. This arrangement
enables the opening and closing of the above named vessel or chamber to be effected
with ease and rapidity.
In order to economize as much as possible the steam used for heating I prefer an
arrangement such as is represented in Fig. 5 which cuables the passage of the
steam from the vessel or chamber of one centrifugal apparatus T through the
pipe W to that of the second apparatus T2 by means of the pipe W' a three-
way cock serving to establish at will communication between the two apparatus
or allowing the escape of the steam from one of them directly into the atmosphere
whilst the other apparatus is isolated. In this system of duplicated apparatus
a single receptacle R may be provided for the liquid extracted below this
receptacle being placed a receiving vessel R¹ heated from below at R", as repre-
sented in Fig. 7.
The operation is conducted in an exceedingly simple manner either the reading
of the thermometer or the pressure gauge being noted and the temperature of the
steam may be optionally varied by the employment of an expansion device placed
at any desired point of the distributing tube.

page_text: As above stated the operation takes place in the same manner if, in lieu of
sulphur ore, crude sulphur has to be refined, and also in case the treatment of ores
and raw materials such as ozokerites paraffins, heavy oils of petroleum and the like is
to be effected with the object of extracting from them liquefiable materials
susceptible of being separated from the crude mass by an elevation of tempera-
ture and by centrifugal action as hereinbefore set forth for the extraction of
sulphur. In each case it is sufficient to know the temperature at which the
liquefaction of each of the substances to be separated takes place. As will be
readily understood a series of extractions can be effected in succession by
modifying the temperature commencing with the extraction of the substance
having the lowest inelting point and finishing with that of the substance having the
highest melting point.
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 I
claim is :-
First. The above described process of extracting sulphur from its ores,
characterized especially by the use of steam under pressure combined with a
separation in a closed apparatus.
Second. The employment, for this purpose, of the machine hereinbefore specified
and represented in the accompanying drawings.
Third. The employment of a drawing-off receptacle for diminishing the volume
of the digesting vessel containing the separating pan, this drawing-off receptacle
receiving in a continuous manner, in proportion to its production, the sulphur
subjected to centrifugal action.
Fourth. The method of charging by means of cylindrical sacks tied at their two
ends, as specified, for the purpose of simplifying the labour and increasing, as
stated, the rapidity of the work.
Fifth. The application of the improved process to the clarification or refining
of crude sulphur under the same conditions as specified for the treatment of
sulphur ores.
Sixth. The application of the improved process to the treatment of ozokerites,
heavy oils of petroleum, bogheads and the like, with the object of extracting
therefrom natural wax, paraffin and the like by the use of the machine and simply
modifying the pressure of the steam, that is to say its temperature according to the
melting point of the material to be separated from the raw material, the whole
as hereinbefore described and represented by way of example in the accompanying
drawings.
Dated this 9th day of March 1892.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.