Improved Process and Apparatus for the Extraction of Substances contained in Vegetable and other Bodies, especially applicable to the Extraction of Rubber, and the Recovery of the Solvents Employed.
Year: 1898

page_text: Date of Application, 10th Dec., 1898
Complete Specification Left, 6th Sept., 1899-Accepted, 4th Nov., 1899
PROVISIONAL SPECIFICATION.
Improved Process and Apparatus for the Extraction of Substances
contained in Vegetable and other Bodies, especially applicable to
the Extraction of Rubber, and the Recovery of the Solvents
Employed.
I, JEAN DE LA FRESNAYE, Engineer, of 42, Boulevard Bonne Nouvelle, Paris,
in the Republic of France, do hereby declare the nature of this invention to be
as follows:
i
The extractible substances contained in vegetable bodies are the more easily
extracted from them, the more finely said bodies are disintegrated. Therefore the
leaves to be treated are previously broken up so as to increase as much as possible
the surface of contact between the substance to be extracted and the solvents.
The new process and general arrangement according to this invention will now
be explained, describing as an example the extraction of rubber from the leaves
of an india rubber tree called isonandra.
Leaves of the rubber tree are taken in a dried, powdered form and placed in a
receptacle where the powder rests on a filter. This receptacle is constituted by a
vertical metal cylinder closed at its lower end by a removable bottom and in a
similar way at the top. This receptacle is enclosed throughout the whole of its
cylindrical part in a jacket. The interior of the receptacle is provided with a
bundle or series of vertical tubes. Each tube of this bundle is bent at both ends,
which ends communicate with a space comprised between the outer surface of the
receptacle and the inner wall of the jacket. This arrangement serves to surround
the receptacle with steam under pressure and to produce a circulation of said
steam in the interior of its body through the tubes.
Having placed the powder to be treated in the receptacle suitable cocks are
opened. One cock then admits the solvent of the extractible substance, which, in
this case, may be essence of petroleum. This essence enters an exhauster, and
probably water of condensation, that might have been formed in the essence
reservoir, owing to the change in temperature will appear. This water is drained
off by a cock and then the two cocks are closed. A branch cock is then opened
and the essence enters the receptacle in which the powder to be treated has been
placed. This essence is immediately absorbed by spongy capillarity of the powder.
When the absorption is completed, the receptacle is full up to the joint of its
closing device. Then exhaust steam is admitted into the jacket through a branch
pipe and passes into the bundle of tubes and raises the temperature of the
substances in the receptacle to the desired degree.
A branch pipe serves to lead away into the steam generator, any water of
condensation which may be formed.
When the level of the essence has reached the upper joint the supply cock is
closed and a draw-off cock opened. The essence, saturated with the substances
extracted enters outlet tubes and passes into a vessel preferably of glass so as to
enable the degree of saturation to be seen. The liquid rises in the tubular
extension of the vessel and passes through its bend and descends and is discharged
through a tube into a multi-tubular steam-still placed within a jacket. The
tubes of the still open into the space formed between the surfaces of the still and
[Price 8d1

page_text: the wall of the jacket. Dry steam for heating the still enters through a branch
tube and the condensation water is returned to the boiler through a pipe. As
soon as the saturated essence reaches the level indicated by a gauge steam is
admitted. The liquid contained in the still begins to boil almost at once, the
essence alone is evaporated and the rubber is left in the still. The vapours of
the essence rise in a vertical pipe which is enclosed in a tube forming a jacket
and containing steam.
When the vapours of the essence have reached the top of the still inlet pipe
they pass into a condensation coil immersed in water contained in a reservoir.
This water is maintained at a low temperature by admitting, as required fresh
cold water through a cock.
When the vapours of the essence enter the coil, they become condensed and are
discharged again into the original supply reservoir. The cocks between the
supply reservoir and exhauster and the latter and the extractor and between the
extractor and the still are then opened and are subsequently left open during
the whole of the operation. The essence is thus again admitted to the powder to be
treated, and, having been saturated with the extractable matter, flows into the still
where it is again distilled and so on, the operation being repeated as many times
as required in order to attain the condition when the essence after having been
in contact with the material to be extracted, appears quite white in passing
through the glass vessel.
When this point has been reached the communicating cocks are closed. Water
is introduced through a pipe into the still up to the level indicated on the gauge.
The distillation is then continued at a temperature of say 90° C., the essence
alone becomes vapourised and the rubber floats on the water in a compact state.
The degree of evaporation and formation of rubber and generally all the
phenomena taking place in the still, may be observed through windows secured
to removable plugs which close openings in the still through which the rubber
is withdrawn. The interior of the still may be lighted by means of electric
incandescent lamps. When the rubber has been collected, it only remains to
recover the essence retained in the receptacle by the spongy capillarity of the
powder from which the rubber has just been extracted. For this purpose the
pressure of the steam admitted is raised so as to raise the temperature of the mass
contained in the receptacle up to say 135 or 140° C. A cock is then opened and
the essence retained by the exhausted powder becomes evaporated by the heat.
These vapours pass into a tube and thence into a tubular still containing
vegetable oil up to a certain level. The vegetable oil produces, by absorption,
the condensation of the vapours admitted into the centre of its mass. When the
exhausted powder has been completely dried the heating is stopped. The cock is
closed, steam is admitted through a pipe, which heats the still, passing over all
its surface, and into the tubes opening into the space formed between its two
shells. Under the influence of heat, the essence absorbed by the oil contained in
this still, becomes separated from said oil by being vapourised and rises through
a vertical pipe from the still into a condensation coil immersed in running water
supplied through a suitable supply cock. The condensed essence then flows into
a reservoir. To return this essence to the main supply reservoir, compressed air
is forced into the reservoir by a pump or forcer and the essence being then forced
out through a pipe which communicates with the main reservoir. All these
operations being finished, the residue in the vessel in which the treatment takes
place has to be removed. In order to do this, the bottom of the vessel is lowered,
say, by suitably turning a hand wheel operating a screw threaded spindle sup-
porting the bottom by means of a pivotted shackle. The powder in the receptacle
being dry it will fall to the ground and can then be removed. Before removing
the bottom the outlet pipe connected to it must be disconnected. Similarly, there
is a detachable joint between the outlet cock at the top and its pipe which must
be also unscrewed when it is desired to open the top of the apparatus, the rest of
the operation being similar to that for opening the botton: the nuts are un-

page_text: screwed, then the handwheel is turned so as to raise the screw-threaded spindle,
suitable guides ensuring the proper guiding of the cover during its descent.
Similar guides may be employed for the bottom of the receptacle.
A non-return valve may be employed in order to prevent the oil contained in
the still from being drawn into the receptacle, when its temperature becomes
lower, and a partial vacuum is produced. A cock serves for complete removal of
the essence contained in the receptacle, into the still.
Apparatus constructed in accordance with my invention may be used for the
extraction not only of rubber, but also of other substances contained in vegetable
bodies.
T 10th
1000
COMPLEIE
DIEUITIVATION.
Improved, Process and Apparatus for the Extraction of Substances
contained in Vegetable and other Bodies, especially applicable to
the Extraction of Rubber, and the Recovery of the Solvents
Employed.
I, JEAN DE LA FRESNAYE, Engineer, of 42, Boulevard Bonne Nouvelle, Paris,
in the Republic of France, do hereby declare the nature of this invention and in
what manner the same is to be performed, to be particularly described and
ascertained in and by the following statement:-
The extractible substances contained in vegetable bodies are the more easily
extracted from them, the more finely said bodies are disintegrated. Therefore the
leaves to be treated are previously broken up so as to increase as much as possible
the surface of contact between the substance to be extracted and the solvents
employed.
The new process and general arrangement according to this invention will be
now explained, describing as an example, the extraction of rubber from the
leaves of an india rubber tree called isonandra. The apparatus is illustrated in
the accompanying drawings in which Figure 1b is a continuation of Figure 1.
Leaves of the rubber tree are taken in a dried, powdered form and placed in a
receptacle A where the powder rests on a filter B. This receptacle A is constituted
by a vertical metal cylinder A² closed at its lower end by a removable bottom A¹
and closed in a similar way at the top. This receptacle is enclosed throughout
the whole of its cylindrical part A2 in a jacket A³. The interior of the receptacle A
is provided with a bundle or series of vertical tubes. Each tube a of this bundle
is bent at both ends, which ends at communicate with the space a comprised
between the outer surface of the receptacle A, and the inner wall of the jacket A³..
This arrangement serves to surround the receptacle A with steam under pressure
and to produce a circulation of said steam in its interior through the tubes a.
Having placed the powder to be treated in the receptacle A cocks r and r¹ are
opened. The cock then admits the solvent of the extractible substance, which
in this case may be essence of petroleum. This essence enters an exhauster S
and probably water of condensation that might have been formed in the essence
reservoir owing to the change in temperature will appear. This water is drained
off by a cock r, and then the cocks and r are closed. The cocks of a branch
pipe is then opened and the essence enters the receptacle in which the powder to
be treated has been placed. This essence is immediately absorbed by spongy
capillarity of the powder. When the absorption is completed, the receptacle A is
full up to the joint of its closing device. Then exhaust steam is admitted into

page_text: the jacket space all through a branch pipe C. and passes through the bundle of
tubes and raises the temperature of the substances in the receptacle A to the
desired degree.
A branch pipe C₁ serves to lead away into the steam generator, any water of
condensation which may be formed.
When the level of the essence has reached the upper joint, the supply cock s is
closed and a draw-off cock 6 opened. The essence, saturated with the substances
extracted, enters outlet tubes 61 and 6", and passes into a vessel D preferably of
glass so as to enable the degree of saturation to be seen. The liquid rises in the
tubular extension D¹ of this vessel and passes through its bend 12 and descends
in the tube or extension D³ and is discharged through a tube D' into a multi-
tubular steam-still E surrounded by a jacket E'. The tubes e of the still open
into the space el formed between the surface of the still and the inner surface of
the jacket E. Dry steam for heating the still enters through a branch tube F
and the condensation water is returned to the boiler through a pipe F¹. As soon
as the saturated essence reaches the level f' indicated by a gauge f, steam is
admitted through the pipe F. The liquid contained in the still E begins to boil
almost at once, the essence alone is evaporated and the rubber is left in the still.
The vapours of the essence rise in a vertical pipe G which is enclosed in a tube G¹
forming a jacket and containing steam or heated in any convenient way.
When the vapours of the essence have reached the top of the still outlet pipe G
they pass into a condensation coil H immersed in water contained in a reservoir H¹.
This water is maintained at a low temperature by admitting, as required, fresh
cold water through a cock h.
When the vapours of the essence enter the coil H, they become condensed and
are discharged again into the original supply reservoir R. The cocks sand-b
are then opened and are subsequently left open during the whole of the operation.
The essence is thus again admitted to the powder to be treated, and having been
saturated with the extractible matter, flows into the still E where it is again
distilled and so on, the operation being repeated as many times as required in
order to attain the condition when the essence after having been in contact with
the material to be extracted appears quite white in passing through the glass
vessel D.
When this point has been reached, the communicating cocks rs and bare
closed. Water is introduced through a pipe g into the still E up to the level fl
indicated on the gauge f. The distillation is then continued at a temperature of
say 90° C; the essence alone becomes vapourised and the rubber floats on the
water in a compact state. The degree of evaporation and formation of rubber
and generally all the phenomena taking place in the still, may be observed through
windows I secured to removable plugs or covers i which close openings in the still
and through which the rubber is withdrawn. The interior of the still may be
lighted by means of electric incandescent lamps I. When the rubber has been
collected, it only remains to recover the essence retained in the receptacle A by
the spongy capillarity of the powder from which the rubber has just been extracted.
For this purpose the pressure of the steam admitted through the tube C is raised
so as to raise the temperature of the mass contained in the receptacle A up to
say 135 or 140° C. A cock J is then opened and the essence retained by the
exhausted powder becoming vapourised by the heat, passes into a tube J₁ and
thence into a tubular still K containing vegetable oil up to a level k. The
vegetable oil produces, by absorption, the condensation of the vapours admitted
into the centre of its mass.
When the exhausted powder has been completely dried the heating is stopped.
The cock J is closed, steam is admitted to the still K through a pipe L which
heats the still, passing over all its surface and through the tubes opening into
the space K¹ formed between its two walls. Under the influence of heat the
essence absorbed by the oil contained in this still becomes separated from said
oil by being vapourised and rises through a vertical pipe M from the still K and

page_text: passes to a condensation coil N immersed in running water supplied through a
suitable supply cock 0. The condensed essence then flows into a reservoir P.
To return this essence to the main supply reservoir R, compressed air is forced
into the reservoir P by a pump or forcer through a pipe P1, the essence being then
forced out through a pipe P2 which communicates with the main reservoir R.
All these operations being finished, the residue in the vessel A has to be removed.
In order to do this, the nuts el of the bottom A¹ are unscrewed and the bottom of
the vessel lowered, say, by turning a hand wheel Q operating a screw-threaded
spindle Q supporting the bottom by means of a pivotted shackle Q. The powder
in the receptacle A being dry, will fall to the ground and can then be removed.
Before removing the bottom the joint 7 of the outlet pipe connected to it must
be disconnected. Similarly there is a detachable joint between the outlet cock J
at the top and its pipe J¹ which must be also unscrewed when it is desired to open
the top of the apparatus A, the rest of the operation being similar to that for
opening the bottom: the nuts el are unscrewed, then the hand-wheel T is turned
so as to raise the screw-threaded spindle U to the same height as the floor V,
suitable guidest ensuring the proper guiding of the cover during its descent.
Similar guides u may be employed for the bottom of the receptacle.
A non-return valve j may be employed in order to prevent the oil contained
in the still from being drawn into the receptacle A when its temperature becomes
lower and a partial vacuum is produced. A cock m serves for complete removal
of the essence contained in the receptacle A into the still E.
Apparatus constructed in accordance with my invention may be used for the
extraction not only of rubber but also of other substances contained in vegetable
bodies.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is:-
1. A process of extracting the extractible matter contained in an unlimited
quantity of finely divided vegetable matter by means of a limited quantity of
solvent to be recovered afterwards, substantially as described.
2. Means for carrying out the process described comprising an apparatus for
the automatic extraction in a closed vessel of the extractible matter contained
in vegetable substances, and for the recovery of the solvent matter employed in
the process, consisting of a receptacle in which the vegetable substance is deprived
of its extractible matter, and for the recovery of the solvent employed in the
process, and contained in the powdered substance thus treated, the said apparatus
being provided with tubes by means of which steam is admitted to heat, evenly
and regularly, the whole mass to be treated, substantially as described,
3. In combination with the apparatus specified in Claim 2 a still for the con-
tinuous separation of the extracted matter from the solvent, the said still being
provided with pipes and a double jacket or casing for the purpose of quickening
the evaporation of the solvent which can be employed for the same purpose any
number of times, in combination with a water inlet for the purpose of securing
a complete evaporation and removal of the solvent and for causing the mass float
on its surface, substantially as described.
4. In the extraction, in a closed vessel, of matter contained in the leaves of
the india rubber plant, the recovery of the rubber solvent in a gaseous state by
bringing it in contact with oil, substantially as described.
5. The complete apparatus for use in extracting substances contained in
vegetable and other bodies substantially as described or illustrated in the
accompanying drawings.
Dated this 6th day of Sentomban 1900