An Improved Method of and Apparatus for Extracting and Purifying Perfumes, Oils, and other like Substances.
Year: 1890

page_text: [Communicated from abroad by LA SOCIÉTÉ ANONYME DES PARFUMES NATURELS D
CANNES, of 95, Boulevard Beaumarches, Paris, in the Republic of France.]
An Improved Method of and Apparatus for Extracting and Purifying
Perfumes, Oils, and other like Substances.
I, HENRY HARRIS LAKE, of the firm of Haseltine Lake, & Co., Patent Agents,
Southampton Buildings, in the County of Middlesex, 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 :-
This invention relates to a method of and apparatus for extracting and purifying
perfumes, oils and other like substances.
The improved apparatus for carrying the aforesaid method into practice, is illustrated
in the accompanying drawings in which,
Figure 1 is general plan of the apparatus forming a battery of ten extractors.
Figure 2 is a general view of the operating device.
Figure 3 is a side elevation of the same.
Figure 4 is a section on the line a x of Figure 2.
Figure 5 is a section on the line a¹¹ of Figure 2 drawn to an enlarged scale.
Figure 6 is a cross section of the cocks for operating the extractors, hearing even
numbers.
Figure 7 is a similar view of the cocks bearing uneven numbers.
Figure 8 is a detail of the cock showing the position of plug when the extractors
are not in circulation.
Figure 9 is a detail of the movable bar for the said cocks.
Figure 10 is a detail of the fixed bar with its connection to the cock in the position
it occupies when the two passages are closed.
Figure 11 is a section of the gauging vessel.
Figure 12 is a sectional plan of the same.
Figure 13 is a section of part of Figure 11 drawn to an enlarged scale.
Figure 14 is a plan of the same.
Figure 15 shows a plan of a battery of ten extractors.
Figure 16 is a front view of a battery of ten extractors.
Figure 17 shows several views of an automatic valve.
Figure 18 is a vertical section of an extractor.
11'
Figures 19, 20 and 21 show a vertical section, a cross section and a plan respectively
of a circulating valve.
Figure 22 is an elevation of the intermediate reservoir, filter, evaporator and purifier
with the condenser and vacuum pump and
Figures 23 to 28 show various details of the evaporator and purifier.
The improved apparatus comprises the following principal parts, viz. :-A reservoir
for the solvent; an operating device; a gauge vessel; extractors; automatic valves;
a pipe for conducting the fresh solvent; a circulating pipe a pipe in which the
charged solvent circulates; pipes for discharging the solvent for the parging with
their condensers; a gasometer; a reservoir for the compressed gas with a force
pump; an intermediate reservoir, a filter and evaporator and a purifier with their
condensers and a vacuum pump.
Use can be made of any volatile solvent, preference is however given to a light
petroleum, boiling at about 80 Centigrade. This petroleum is a common article of
commerce, its price is comparatively low, it is not decomposed like carbon disulphide
and its boiling point is sufficiently low to enable it to be separated by evaporation
from the perfumes and fatty substances without altering them.
Water under pressure is the means for conducting the fresh solvent from the
reservoirs to the apparatus where the treatment takes place.

page_text: :
Compressed air or preferably a mixture of air and the vapour from the solvent,
which is collected in the course of the operation and will hereinafter be termed com-
pressed gas is employed for producing the movement of the liquids (fresh solvent or
solvent more or less charged) in the battery proper.
The battery Fig. 1 hereinafter described comprises ten extractors, E but their
number can be varied to suit the requirements of the works wherein they are
employed, taking into consideration the size of the extractors, the nature of the
substances that have to be most frequently treated, the number of washing operations
necessary for obtaining a complete exhaustion, and the work which is to be done
every 24 hours. From this it will be seen that the number of extractors can be
greatly varied.
It may however be remarked that the number of washing operations to which the
substance under treatment in a certain battery can be submitted is not determined by
the number of the extractors, and that it can be optionally varied in the same battery
without at all changing the combination of the latter, which renders it possible
to effect a complete exhaustion irrespective of the number of extractors in use.
The reservoirs, as their name indicates, serve to receive the solvent which is not in
the circuit. These receptacles are closed and are provided with admission and dis-
charge pipes for the solvent and with an admission pipe for the water under pressure
by means of which the solvent is forced into the battery proper, so as to enter into the
working circuit.
The operating device A2 is represented in Figs. 2 to 10 Figs. 2, 3 and 4 of
which shows the general arrangement of the device, and the other views the details
of the operating cocks, and moro especially the positions of the orifices of two
connected cocks. Its chief use is to regulate from a distance the introduction of the
compressed gas into the extractors and the exhaustion of the said gas into the
gasomoter separately or together by combined movements; to put the extractors in
communication with the steam for the purging to discharge into the atmosphere, the
air contained in each extractor after charging the latter again with fresh substance
when the solvent is introduced therein.
It is mainly composed of cocks and pipes so arranged that the operation can be
conveniently effected.
The cocks R for operating the extractors, with their movable bar placed in two
connected groups, each cock corresponding to a certain extractor, with which it is
connected by a separate pipe M by means of which it can at will be put into com-
munication either with the admission pipe G C for the compressed gas or with the
pipe for discharging this gas into the gasometer G E. Some of these cocks have their
admission and discharge orifices for the compressed gas arranged in the opposite
direction to that of the orifices of the other cocks because the operation is such that
if the orifices bearing even numbers are opened those bearing uneven numbers are
closed. Both groups can at will be engaged with a movable bar A' which is actuated
by a hand lever A B, in such a manner that if the orifices of the one group
of cocks are opened by displacing the said movable bar from the right hand.
to the left hand side those of the other group are closed by the same movement,
and vice versa.
A fixed bar B¹ is provided with which are engaged the levers of the cocks R
for the extractors outside the circuit, for discharging, purging or charging purposes.
V V are cocks for the introduction of the steam into the extractors, which cocks
are connected with the steam admission pipe V1. Each of the said cocks correspond
to a certain extractor and puts it in communication with the pipe V' by means of a
branch from the pipe M which connects this extractor with its working-cock.
UU arc cocks which discharge into the atmosphere the air contained in the
extractors each time after they have been charged again with fresh material. Each of
these cocks like those above referred to, corresponds to a certain extractor and
.communicates with it by the same branch pipe and the same channel M which serves
to introduce the steam
The gauge-vessel H* is illustrated in detail in Figs. 11 to 14 its principal

page_text: function is to regulate automatically, and according to the substance to be treated, the
quantity of the solvent which has to enter the circuit for replacing the solvent which
passes to the evaporator. The quantity of the solvent used in the treatment thus
remains constant which ensures regularity in the operation.
A closed cylindrical vessel communicates at its lower end through a branch pipe 1
with the reservoirs for the fresh solvent and through a branch pipe 2 with the
extractors by means of the corresponding automatic cock and the admission pipe D, N
for the fresh solvent as shown in Fig. 1. At its upper end the said vessel
communicates through a tube 3 with the general pipe for the compressed gas. It
carries at the top a glass tube C closed at the upper end by means of a stuffing
box C. Inside this tube a rod F provided with an index H hereinafter referred to
rises and descends freely. In the interior of the gauge vessel is arranged a bell H¹
which serves to regulate the admission of the solvent; for this purpose it has in its
centre a vertical socket or sleeve H2 which extends through its entire length and the
upper extremity of which remains always visible in the glass tube where it indicate.
the level of the solvent in the gauge-vessel. Through the aforesaid socket or sleeve
extends the vertical rod F connected with the balanced valve I which controls the
orifice of the pipe 1. This rod carries at its upper end a movable index H
which is secured by means of a screw and against which the said socket or sleeve
of the bell abuts when the liquid has reached the desired level in the gauge-
vessel.
When the said bell is at its lowest point the valve I is open, if at this moment the
water is caused to exert its pressure in the reservoirs, the solvent forced by the
pressure passos into the gauge-vessel and raises the bell with its socket or sleeve
without carrying with it the valve, until the socket or sleeve comes in contact with
the index; but then the bell, continuing its ascending motion carries with it the valve
by means of the index H and the rod F, and thus closes the orifice for the admission
of the solvent.
In the pipe for conducting the solvent from the reservoirs, in front of the tube 1, is
included a valve which allows the introduction of the solvent into the gauge-vessel but
prevents its return to the reservoirs when the pressure of the compressed gas is applied
so as to cause the passage of the same into the circuit.
Inside the gauge-vessel a serpentine heating coil H³ is provided through the
medium of which the solvent can be slightly heated before passing into the extractor
so as to facilitate its action.
The extractors are designated in the general plan on Fig. 1 by the letters E;
Fig. 15 shows a general view of the extractors with their pipes; Fig. 16 gives a
partial view in elevation, and Fig. 18 gives the details of an extractor considered
separately.
These extractors are used for the purpose of placing the substances to be treated in
contact with the solvent so as to perform the extraction proper.
Each of the extractors consists essentially of a receptacle E of cylindrical shape
which is closed at the bottom and open at the top, and is provided with a cover, E1
capable of withstanding the pressure of the compressed gas; the body proper E
constitutes the lower part, and the prolongation Ex constitutes the upper part; the
prolongation is of a somewhat larger diameter than the body proper and thus forms
an interior seat upon which the basket or the like F containing the substance under
treatment can be placed.
The lower part of the extractor communicates with the corresponding automatic
valve and further through a cross tube X see Fig. 15. First with the admission
pipe DN for the fresh solvent and through it with the gauge-vessel; Second with the
pipe NS, for circulating the solvent used in the operation. Third with the pipe DC
for discharging the charged solvent. Fourth with the corresponding pipe P¹ for dis-
charging the purging solvent; so that there is in the extractor only a single orifice for
the admission and discharge of the liquids.
In the interior of the lower part is arranged a heating coil or serpentine F' which
receives the expanded steam for the purpose of enabling the solvent to be raised to a

page_text: sufficient temperature so as to considerably increase the dissolving power without
deteriorating the quality of the product which is to be extracted.
It communicates at its upper part with the operating device by means of a pipe
connected (1) with the corresponding operating cock R and through this with the
admission and discharge pipes for the compressed gas; (2) with the cock U communi-
cating with the atmosphere; (3) with the cock V of the steam admission pipe for
the purging.
As above stated the substance to be treated is not placed in the extractor itself, it is
placed in an open basket F at the top and provided with a bottom perforated with
holes to allow the solvent to pass through, whilst the sides are not perforated. .It is
nearly the same length as the body proper of the extractor, but its diameter is rather
less, and it carries at its upper end an angle-iron F2 the flange or web of which rests
upon the inner rim of the upper part and forms an hermetical joint by means of a
bayonet ring J and a screw K. The ring J is furnished with a certain number of
lugs J on the outside which pass under corresponding lugs L provided in the upper
part of the extractor. Under these conditions a space is left between the sides of the
said basket and the body of the extractor, which space can at will be put in communi-
cation with the upper part by means of a cock. Thus at the beginning of the
purging operation all the sides and principally those of the basket can be heated so
as to prevent the condensation of the steam which interferes with the progress of this
operation.
The automatic valves are designated in Fig. 1 and in Figs. 15, 16 and 17 by the
letter O Figure 17 shows the details of one of the automatic valves. Their number
corresponds to the number of extractors plus one for the gauge-vessel.
The chief use of those placed on the extractors is to automatically interrupt the
communication between one extractor and another extractor connected therewith
during the circulation of the solvent by means of the compressed gas as soon as the
solvent contained at first in the first has passed into the second so that, without
the aid of the workman and without operating a cock the compressed gas is prevented
from passing in its turn the same way as the solvent, and from passing through the
open discharge pipe to the second extractor and to the gasometer without performing
any useful work.
The one which is placed upon the gauge vessel has to fulfil a similar object between
the gauge vessel and the extractor with which it is put in communication so as to
introduce a fresh solvent into the same.
An automatic valve in a closed cylindrical vessel communicates through a side
opening or passage 1 with the corresponding extractor and through the lower opening
or passage 2, with the cross-pipe X and through this with the admission pipe for the
fresh solvent, for circulating the solvent used in the operation for discharging the
charged solvent, and for discharging the purging solvent. On the top of the valve is
a kind of box W which is open at the lower end so as to communicate with the body
proper of the said valve, and closed on the other sides and traversed on one of the
side walls by a bent lever ending in a fork having branches or arms the use of which
will hereinafter be explained.
Inside the said valve O is the bell or float O' which serves to automatically
interrupt the exit of compressed gas from the extractor towards the pipes for the
liquid. For this purpose it is connected with a double lift valve Q controlling the
lower orifice 2. When the solvent comes from the extractor through the orifice, it
raises the bell and the valve and passes through the orifice 2, also in case it passes in
the opposite direction from the pipe X, but if, after the solvent, gas comes from the
extractor, there will be a moment when the height of the liquid in the valve is no
longer sufficient to float the bell, so that the latter will fall and take with it the valve,
thus closing the orifice 2. From the purging operation towards the end of the
treatment the last parts of the solvent escape in a state of vapour and the bell or float
prevents the passage of the same without any special device.
The bell carries a vertical rod Y provided with a shoulder Z which penetrates the
box and extends between the branches or arms of the fork of the bent lever without

page_text: touching them. When the lever is in the position a b₁ the rod mounts and descend
freely and the bell operates without hindrance, but if the lever is caused to occupy the
position a b the two branches or arms of the fork raise the shoulder Z, taking with
them the bell and its valve Q so that the orifice 2 will remain open.
The admission pipe for the fresh solvent is designated in the general plan Fig. 1,
and in Figs. 15 and 16 by the letters D N. It connects the gauge-vessel H* with
the extractors through the medium of the pipes X and automatic valves. This pipe.
has for its object to conduct the necessary quantity of the fresh solvent from the
gauge vessel to each of the extractors in turn.
It is actuated by the valved cocks N which are specially arranged for the purging.
Each cock N opens upwards and presents at the upper part of its box a double pipe
arranged so as to enable the solvent coming from the extractor through the pipe X to
traverse this box above the valved cock when the latter is closed and rests upon
seat, and thence reaches the purging pipe on passing below the valves of the following
extractor, as hereinafter set forth.
its
For the purpose of rendering this arrangement better understood it is sufficient to
refer to Figs. 19 to 21 which show the details of a circulating valve S presenting a
similar arrangement with this differenco that in the valve S the solvent passes
through the lower part of the box below the seat of the valve instead of through the
upper part.
The pipe for circulating the solvent used in the operation or the circulating pipo
proper is indicated in Fig. 15 by the line N S. Its object is to ensure the regular
circulation of the solvent in a forward direction without any back-movement and
without operating the cock through all the extractors charged with the substance to
be treated so as to effect a methodical and rapid exhaustion, the passage of the solvent
taking place from the pipe to the extractor through pipes X and automatic valves as
in the case of the pipe for the fresh solvent. For this purpose it is provided with.
valves S one of which is shown in detail in Figs. 19 to 21. This valve opens upwards
in the same direction as that of the circulation. The number of the said valves corre-
sponds to that of the extractors, each of these valves being placed between two con-
secutive extractors so that the solvent can advance freely from one extractor to the
other in the desired direction, raising the valve which is between the two extractors
in that direction but cannot pass backwards.
Each of these circulating valves S is provided with a vertical rod which is secured
to the valve proper and keeps it immovable on its seat during the purging; each
valve is specially arranged for the purging. The valve box is provided at its lower
end and underneath the seat of the valve with branch pipes S1 S2 which permits
the solvent coming through the cock N from the preceding extractor to pass beneath:
the valve when the said valve is closed whence it passes to the purging pipe.
The pipe for discharging the charged solvent shown in the general plan Fig. 1
and in Figs. 15 and 16 by the letters D C is designed to conduct to the evaporator
the solvent when it has passed through the circuit in the extractors and has bee:
sufficiently charged with the substance to be extracted.
It is controlled by the valve cocks C and like the preceding pipes communicates
with the extractors by means of pipes X and the automatic valves.
The purging pipes, which are designated in Fig. 15 by the letters P¹ have for their
object (as their name indicates) to collect the solvent which proceeds from the
purging. They are controlled by the cocks P, and communicate like the pipes above
referred to, with the extractors through pipes X and valves. They terminate in the
purging serpentines.
It will be observed that the number of serpentines are only half that of the pipes or
extractors, each of the serpentines being used at the same time for an extractor of the
first half of the battery and for an extractor in the row of the second half of the
battery. This arrangement which is made for the sake of economy does not present
any inconvenience in carrying the operations into effect, in fact, in the operation of
the battery as above described there are never more than four consecutive extractors,
that is to say less than half the total number, wherein the purging takes. place

page_text: simultaneously, so that in the above described arrangement the two extractors served
by the same serpentine are in no case subjected to the purging operation at the same
time.
The gasometer G has for its object to collect the mixture of air and vapour from
the solvent proceeding from the various parts of the battery in the course of the
operation and to restitute it to the force pump so as to obviate the loss of the solvent
which might escape into the atmosphere; it is therefore connected with this pump by
suitable pipes. A pipe terminating in the interior at the upper level of the water
enables the liquid furnished by the vapours from the solvent which condense in time
to be collected. Another pipe terminating at the upper part of the gasometor enables
from time to time, after a rest which has allowed the vapours from the solvent to be
separated from the air by gravity and to accumulate in the lower part of the bell, the
withdrawal of the excess of air which has found its way into the same during the
operations.
Furthermore it communicates in a general manner with all the parts of the apparatus
wherein vapours from solvents which are susceptible of being carried away into the
atmosphere may be produced.
The force pump and reservoir for the compressed gas are designed to supply the
motive fluid by the aid of which the circulation of the solvent in the battery can be
effected through the medium of the operating device. For this purpose the force
pump communicates on the one hand with the gasometer and on the other hand with
the reservoir for the compressed gas, and this reservoir is in its turn connected with
the operating device through the pipe G C.
The intermediate reservoir K is designed to receive the charged solvent discharged
from the extractors and to keep it momentarily as a kind of intermediate depôt
between these apparatus and the evaporator and purifier so as to obtain a certain
independence in the operation of the same.
Accordingly it communicates on the one hand with the extractors and on the other
hand through the filter with the evaporator and purifier.
The filter L of any suitable construction has for its object to arrest any dust which
may be carried away and to cause the solution proceeding from the extractors to
undergo a first filtration before conveying it to the evaporator.
M is the evaporator and N the purifier Fig. 22. Although the evaporator and the
purifier are for the sake of greater convenience connected in the battery they form in
reality two distinct apparatus; they will therefore be described separately.
Fig. 22 shows a general view of the intermediate reservoir, filter, ovaporator and
purifier with their condenser P and vacuum pump Q. Figs. to 28 illustrate the
details of the evaporator and the purifier.
The evaporator M has for its object to concentrate the solution of the fatty sub-
stances or perfume in the solvent or charged solvent, and to evaporate the solvent as
far as practicable by means of heat and a vacuum.
It comprises a receptacle of cylindrical form provided with the pipe 1 for the
introduction of the charged solvent, the pipe 2 for the discharge of the concentrated
solution, and the pipe 3 for the outlet of the vapours from the solvent. In the interior
is provided a vertical partition m in the form of a spiral wherein circulates the
solution, and in this spiral arranged near the bottom of the evaporator without
touching it is placed a serpentine or coil m' wherein circulates the steam in the
opposite direction to that of the solution. The pipe 3 communicates with the con-
denser P which is connected with a pump Q for creating the vacuum On passing
from the evaporator M. the steam from the solvent leaving through the pipe 3× passes
through a safety vessel M' designed to collect the parts of the solution which may
escape together with the vapours. The safety vessel here constitutes a cylindrical
chamber included between the evaporator and the purifier.
The object of the purifier N is to expel from the extracted substance (fatty substance
or perfumed wax) the last traces of the solvent which have not been separated by the
evaporator, by subjecting it in a state of as great a division as possible to the simul-
taneous action of steam and a vacuum.

page_text: This method of purification is applicable not only to fatty substance but also to
perfumed wax; however it is preferable in this case to replace the steam by vapour
from alcohol.
The purifier N comprises a boiler N' which has a double bottom wherein circulates
the steam. On the top of the boiler is arranged a vertical hollow column N2 of
trays n and divided into two parts by a diaphragin N³.
At
At the upper part the purifier carries a pipe 4 for the inlet of the concentrated
solution or material to be purified, and the pipe 5 for the admission of the steam.
the lower part the purifier is provided with a pipe 6 for the outlet of the vapour from
the solvent. Interiorly are provided the aforesaid trays n made of cloth. These trays
are of conical form, and placed one above the other alternating in direction and size.
The fatty substance and the perfumed wax. being admitted in a liquid state through
the pipe 4 spread in the form of thin strata as they descend from one tray to the
other.
As above stated the lower part or column N2 is separated from the upper part or
purifier by a diaphragm N³ made of conic shape like the aforesaid trays of cloth, and
is arranged as shown in Fig. 23 so as to allow the passage of the liquids at its
centre, but not the vapours. Below the said diaphragm is arranged a pipe 7 for the
outlet of the vapour from the solvent. Trays of cloth are also arranged below the
diaphragm as in the upper part. In its interior the column N2 is also provided a
cylindrical casing N* which is concentric with the column, open at its upper part,
and closed below by a diaphragm N³ which separates it from the boiler, and permits,
as above stated, the passage of the liquids, but not the vapours at its central part.
The trays n of cloth are in the interior of this casing. Between the sides of this
casing and those of the column is left an annular space into which the vapours from
the boiler can pass through the openings n¹ optionally provided at the circumference
of the diaphragm.
:
The boiler is provided below with the pipe 8 for the discharge of the purifiel
material, and on one side with a cock for taking samples, and with a glass enabling
the course of the operation to be watched. It has a flat bottom so as to maintain a
thin uniform layer of the material to be purified and to favour the regular evaporation
upon a large surface of the water (or alcohol) condensed in the column.
The double bottom is in communication with the vacuum pump so that a lower
temperature than 60 degrees C. can be maintained therein when all the water condensed
in the column has been evaporated and when the purified material comes in contact
with the partition of the double bottom.
It will be observed that in the two parts of the column the steam (or the vapour
from alcohol) enters from above whilst the vapour from the solvent escapes below.
This arrangement is based upon the same principle which underlies the purging
operations, which are effected by introducing the steain below the material to be
purged and discharging the solvent below, as the vapour from the solvent is much
heavier than the steam (or the vapour from alcohol), so that it will not readily mix
with the latter and will always tend to separate therefrom in order to reach the lower
parts. It is therefore much easier to displace the vapour from the solvent by means
of steam (or vapour from alcoliol) by a downward pressure than by a pressuro in the
opposite direction; for in the former case the great weight of the vapour from the
solvent aids in the movement whilst in the second case it forms an obstacle to the
same.
The pipes 3 and 31, 6 and 7 are connected with the condenser, which latter is
in communication with the vacuum pump that maintains a suitable vacuum in the
corresponding apparatus.

page_text: extractors E1, E3, E5, do not contain a solvent, whilst the extractors E2, E4, E6, are
filled with the solvent the positions of the cocks are as follows:-
In the case of the extractors E8, E9, E10, wherein the purging operation takes
place and which have pipes X crossing each other, the circulating valves S8, S9, $10,
are held down upon their seats likewise the valve S; the cocks N8, N9, N10, of the
pipe for the fresh solvent are closed, likewise the cocks C8, C9, C10, of the pipe for
the charged solvent; the cock P8 of the purging pipe P8¹ is closed whilst the
cocks P9, P10, of the purging pipes P91, P1, are open, and also the cock P1 of the
pipe P1 the bells of the automatic valves 08, 09, 010, are kept raised; the steam
cocks V8, V9, V10 of the operating device are open for the admission to the
extractors E8, E9, E10, and the solvent is discharged from these through the purging
pipes P91, P10, P11, passing through X8, N8, S9, P9, X9, N9, S10, P1, X10, N10,
SI, P1, and traversing as above explained the boxes of the cocks N8, N9, N10, at the
upper part, and the boxes of the valves S9, S10, S1, at the lower part; the corre-
sponding operating cocks RS, R9, R10, are disengaged in the position of rest at the
neutral point, the two openings are closed (position Fig. 3 Sheet 3) and consequently
the communications of E8, E9, E10, either with the admission pipe or with the
discharge pipe for the gas, are interrupted.
In the case of the extractor E7 which is being discharged and charged again all
the cocks of the pipe X are closed and the corresponding operating cock R7 of the
operating device is at the neutral point as R8, R9, R10.
In the case of the extractors included in the circuit E1, E2, E3, E4, E5, E6, with
the pipes X the cocks N1, N2, N3, N4. N5, NG, of the pipes for the fresh solvent
are closed and also the cocks C1, C2, C3, C4, C5, C6, of the pipe for the charged
solvent the cock P, of the purging pipe Pi, is open for the purging of E10, whilst
the cocks P2, P3, P4, P5, P6, P7, of the purging pipes P2, P3, P4, P5, P61, P71,
are closed; the corresponding operating cocks R1, R2, R3, R4, R5, R6, of the
operating devico are engaged with the movablo bar position indicated in Fig. 1 on
sheet 3; the openings in the position indicated in Fig. 2 on the same sheet;
lever of the movable operating bar in the position A, B.
the
For continuing the lixiviation it is expedient (1) to include in the circuit of the
solvent the extractor E7 which has been charged again with fresh material; and
(2) to introduce a fresh solvent into the extractor E¹, for the last lixiviation preceding
the purging.
From the fixed bar B7 is disengaged the lever of the operating cock R7, which was
in the position of rest in order to engage it with the movable bar in the same position
as the cocks R1, R2, R3, R4, R5, R6, and the valve of the circulating pipe S7
is set free.
Then the lever of the movable bar Al is moved from the right hand to the left
hand side from A B to A B1, so as to put the extractors E2, E4, E6, in communi-
cation with the admission pipe G C for the compressed gas through the
cocks R2, R4, R6, and the extractors E3, E5, E7, in communication with the
discharge pipe CE for the gas through the cocks R3, R5, R7. The solvent then
passes from E2 to E3 through X2 N2 S3, traversing the box of the cock N2 at
its upper part. In like manner it passes from E4 to E5 through X4 N4, S5, and
from E6 to E7 through X6, N6, S7.
It will be observed what part at this moment the valves in the circulating pipes
perform. As they open upwards S3, S5, S7, enable the solvent coming from the
extractors E2, E4, E6, to be simultaneously introduced into the extractors E3, E5, E7,
whilst S2, S4, S6, prevent the return of the solvent.
During this time a fresh solvent is introduced into El. For this purpose the
gauge vessel is first filled, the solvent being introduced into the same from the
reserves by the pressure of the water; the gauge-vessel having been filled to the
height regulated as hereinbefore described, the water pressure in the reservoirs is
discontinued, the flap valve inserted in the pipe for conveying the solvent from the
reservoirs to the gauge-vessel is automatically closed, and the fresh solvent is then
ready to be introduced into the circuit. The cock N, is opened and the fresh solvent

page_text: passes into the extractor E', through N1, X1, the gas contained in El escapes to the
gasometer through the discharge pipe GE with which it has been put in communi-
cation at the same time as E3, E5, E7, because R1, was engaged with the movable
bar like R3, R5, R7.
At this moment the extractors E1, E3, E5, E7, are filled with the solvent, whilst
the extractors E2, E4, E6 have no solvent in them; moreover the solvent contained
in the extractor E7 is sufficiently charged with the material to be extracted, and
must in the following movement discharge its contents into the evaporator. It is,
sufficient for this purpose to open the cock C7 of the pipe for discharging the charged
solvent from this extractor without any other change.
It may here be remarked that in order to ensure the regularity of the operation
the charged solvent is first received, on leaving the last extractor in an intermediate
reservoir whence it is drawn by the vacuum pump into the evaporator through the
filter, thence into the purifier proportionately to the progress of the operation.
If the lever of the movable bar is moved from the left hand to the right hand
side, from A B1 to A B in order to pass the solvent from the extractors E1, E3, E5
into the extractors E2, E4, E6, connected therewith it will be seen that by the same
movement the discharge of the charged solvent from E7 to the intermediate reservoir.
is effected.
Moreover the material contained in the extractor E', is exhausted and the latter is
then purged, the valve S2 being rendered immovable, the cock P2 of the purging
pipe P2 being opened and next the cock V1 of the steam pipe. At the commence-
ment of the purging operation care is taken as above explained when describing the
extractor to put in communication the upper part or prolongation and the annular
space between the sides of the basket and those of the body of the extractor by
opening the steam cock so as to obviate the condensation the inconveniences of which
have been set forth. Moreover, it is advisable to lower the lever of the automatic
valve so as to maintain the bell raised for the passage of the last parts of the
purging solvent.
The changes which are produced in the course of the operation in thus moving the
operating lever to its original position A B are as follows:
The extractor E7 which was not in the circuit is included and the first washing has
taken place therein the extractor El which was in the circuit is cut out. Another
washing operation has been effected in each of the extractors E2, E3, E4, E5, E6,
the extractors E2, E4, E6 being again filled with the solvent, whilst the extractors, E3,
E5, E7, have no solvent in them. During this time the extractor E8 has beer
completely purged and it is discharged and charged again; if then the cock G C7 is
closed for separating the extractor E7 from the discharge pipe for the charged
solvent, and if the operating lever is once more moved from the right hand to the left
hand side to A BI, the solvent is passed from the extractors E2 E4 E6 to the
extractors E3, E5, E7, and a complete cycle of movements has been gone through.
As at the commencement there are in the circuit six extractors E2, E3, E4, E5, E6, E7,
the order of the extractors filled with the solvent and the empty extractors being the
same that is to say an empty one first, then a full one, and so on continuing the
alternation to the last extractor which is full; an extractor E8 which is discharged and
charged again follows the last extractor which is filled with the solvent and lastly
three extractors E9, E10, E1, which are being purged.
However the lever of the operating bar is in the position A, B1, instead of being in
the position A B, and the extractors of one group are filled with the solvent whilst
those of the other group do not contain the solvent, so that the position of any one
extractor in the battery with regard to the course of the operation is exactly the same
as that of the extractor which immediately precedes it at the commencement, that is
to say the extractor ES for example performs in the next cycle of operations the
same part as the extractor E7 in the last cycle; in like manner E7 will replace E6;
E1 will replace E10 after three movements of the operating lever the latter again
occupies its original position A B after having passed through a cycle of operations
which has the effect of putting a fresh charge of material under treatment to convey
B

page_text: a fresh portion of the charged solvent to the evaporator and to subject a fresh charge
of exhausted material to the purging operation. The part to be performed by each
extractor in the operation during the following cycle will at this moment be the same
as the part which was performed by the extractor that preceded it by two rows during
the first cycle and therefore the operation can be taken up again in the same order and
in the same direction as in the case of this one.
The washing and lixiviating operations are continued in this manner until the
treatment is to be terminated for some reason.
During this time the purification is effected through the medium of the evaporator
and the purifier. The solution conveyed from the extractors to the intermediate
réservoir is drawn by the vacuum pump, traverses the filter where it is freed from any
dust which it may have carried away, and concentrates in the evaporator where it is
separated from nearly the whole of the solvent. Thence it passes into the purifier
where it penetrates the upper part of the column spreads in the form of a thin
stratum upon the first tray, then falls upon the second and so on and is thus gradually
freed from the last particles of the solvent which it has retained owing to the action
of the steam (or the vapour from alcohol) and of the vacuum, and finally falls into
the boiler wherein the purification terminates.
It now only remains to collect the purified product in special reservoirs whence it
is removed proportionately to the requirements.
The operation is thus performed in a regular and continuous manner under
conditions of economy and efficiency such as have not been realized up to the
present time.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed as communicated to me
by my foreign correspondent I declare that what I claim is :-
First. The method of extracting and purifying perfumes, oils and other like
substances, substantially as herein before described.
Second. In the above described method of purifying perfumes the substitution of
vapour from alcohol for steam used in the purification of fatty substances.
Third. For extracting and purifying perfumes, oils and other like substances, the
apparatus constructed and operating substantially as hereinbefore described with
reference to the accompanying drawings.
Dated this 18th day of April 1890.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.