IMPROVEMENTS IN THE DISTILLATION OF ESSENTIAL OILS OR PERFUMES
Year: 1874

page_text: LETTERS PATENT to Alphonso Piver, of No. 10, Boulevart de
Strasbourg, Paris, in the Republic of France, Perfumery Manu-
facturer, for the Invention of "IMPROVEMENTS IN THE DISTILLATION OF
ESSENTIAL OILS OR PERFUMES."
Sealed the 4th August 1874, and dated the 19th February 1874.
PROVISIONAL SPECIFICATION left by the said Alphonse Piver at the
Office of the Commissioners of Patents, with his Petition, on the
19th February 1874.
I, ALPHONSE PIVER, of No. 10, Boulevart de Strasbourg, Paris, in the
Republic of France, Perfumery Manufacturer, do hereby declare the
nature of the said Invention for "IMPROVEMENTS IN THE DISTILLATION OF
ESSENTIAL OILS OR PERFUMES," to be as follows :—
The object of my Invention is to obtain by the aid of new or improved
distilling apparatuses more essential oils or perfumes from any aromatic
substances than hitherto and with greater rapidity, and to convey the
said perfumes if desired directly into alcohol or oleaginous substances of
any kind.

page_text: :
Steam at low pressure carries off but slowly and imperfectly the
essential oils from the substances containing them; the said oils some-
times remain dissolved in the water and when operating with alcohol,
which is vaporised at a low temperature, but a small quantity of
perfume is carried off.
My improved process consists in distilling the aromatic substances at
a temperature higher than the boiling point, that is to say, a pressure of
between 1 and 5 atmospheres. The apparatuses by which I perform this
distillation consist of a steam generator of any suitable kind, a closed
vessel capable of sustaining the steam pressure, in which the aromatic
substances are placed, and which I term the "odorifère," and a cooling
vessel. The steam of water or alcohol proceeding from the boiler and
conveyed within the "odorifère" carrics off the perfumes of tho
substances contained in the said vessel. The steam laden with the
perfumes enters the worm of the cooling chamber, where it is condensed
and flows into a vase termed the "essencier." The essential oils being
much lighter than water float thereupon, and the old process of gathering
the oil was to suck it out with the mouth by means of a special tube and
topo ur it into a small bottle or flask.
The "essencier which I employ constitutes a second part of my
Invention. It is based on the methodical checking of the flow of the
liquid, this vessel being divided by vertical partitions into six or cight
compartments, through which the liquid is obliged to travel successively
up and down, a small quantity of essential oil being separated at the top
of cach compartment falls into a bottle while the water flows into
another vessel.
Another small apparatus for preventing overflow, and which I term
the "paraflux," constitutes a third part of my Invention. It is intended
to be placed on the end of the curled tube or worm, and outside of the
cooling chamber. If by a sudden increase in the intensity of the fire an
eruption or sudden flow of the liquid were to carry off the substance.to
be distilled, and if any particle of the said substance were to fall into the
receiver, the whole contents would be spoiled, and would have to be
distilled over again. With my "paraflux" this inconvenience is pre-
vented because the irruptive flow falls into a swing box, which by its
action at once brings a funnel under the outlet of the tubo of the cooling
vessel, and the liquid is thus conveyed into an open vessel placed under
the swing box.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Alphonse Piver in the Great Seal Patent Office
on the 17th August 1874.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, ALPHONSE
PIVER, of No. 10, Boulevart do Strasbourg, Paris, in the Republic of
France, Perfumery Manufacturer, send greeting.
WHEREAS Пer most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Nineteenth day of February, in the year
of our Lord One thousand cight hundred and seventy-four, in the thirty-
seventh year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said Alphonse Piver, Her special licence that
I, the said Alphonse Piver, my executors, administrators, and assigns,
or such others as I, the said Alphonse Piver, my executors, admini-
strators, and assigns, should at any time agree with, and no others, from
time to time and at all times thereafter during the term therein expressed,
should and lawfully might make, use, exercise, and vend, within the
United Kingdom of Great Britain and Ireland, the Channel Islands, and
Isle of Man, an Invention for "IMPROVEMENTS IN THE DISTILLATION OF
ESSENTIAL OILS OR PERFUMES," upon the condition (amongst others) that
I, the said Alphonse Piver, my executors or administrators, by an
instrument in writing under my, or their, or one of their hands and
seals, should particularly describe and ascertain the nature of the
said Invention, and in what manner the same was to be performed,
and cause the same to be filed in the Great Seal Patent Office within
six calendar months next and immediately after the date of the said
Letters Patent.
NOW KNOW YE, that I, the said Alphonse Piver, do hereby declare
the nature of my said Invention, and in what manner the same is
to be performed, to be particularly described and ascertained in and
by the following statement:-
The object of my Invention is to obtain quicker and more abundantly
with new distilling apparatus essential oils or perfumes from any
aromatic substances, and to obtain or convey the said perfumes either in
their genuine purity or diluted in alcohol or oleaginous substances of any
kind.

page_text: By the distilling process in actual use at low pressure the steam pro-
duced carries off but slowly and imperfectly the esssential oils from the
substances containing them. The said oils sometimes remain diluted in
the water, and when operating with acohol, which is vaporised at a
lower temperature, there is only a small quantity of perfumes carried off.
My improved process consists in distilling the aromatic substances at
a temperature higher than the boiling point, that is to say, betwixt
1 and 5 atmospheres' pressure, according to the nature of the substances
to be distilled. The compound apparatus which I contrived to obtain
this result is composed of a steam generator of any kind, an expanding
chamber into which the steam is directly conveyed, two "odorifère ”
vessels, within which the aromatic substances are placed, and two cooling
chambers in communication with the said "odorifèro" vessels. The
water or alcohol steam proceeding from the boiler runs into the
expanding chamber, where it expands from 4 or 5 to 1, or 2 atmospheres'
pressure. From the expanding chamber the steam is conveyed by turns
into the "odorifère" vessels, and it carries off the perfumes of the
aromatic substances contained in the said vessels. The steam carrying
off the perfumes from the odorifere” vessels enters into straight or
worm tubes of a cooling chamber within which it is condensed and
received in a special essence-gathering bottle "essencier." The essential
oil being much lighter than the condensed water swims or floats over the
latter as it issues from the cooling chamber. The old process of
gathering it was to suck it up with the mouth by means of a suitable
tube to pour it into a small bottle or flask.
The said "essencier" of my contrivance constitutes the second part of
my Invention. It is based on a methodical checking of the flow of the
liquid, the said vessel being divided by partitions into several compart-
ments or small chambers, through which the liquid is obliged to travel
successively up and down, a small quantity of essential oil being
seperated from the liquid at the top of each compartment falls into a
bottle whilst the water flows into another vessel.
"
Another small apparatus for preventing overflow, and which I call the
'paraflux," constitutes a third part of my Invention. It is intended to
be placed at the outlet of the cooling chamber of my distilling apparatus,
and to receive the liquid flowing out before its introduction into the
"essencier" intended to receive it. If on account of a sudden intense-

page_text: ness of the fire an irruption or sudden flow of the liquid contained in
the "odorifère" vessel or in a common alembic were to carry off the
substances to be distilled this overflow falls down in a swing box, which
by its movement brings at once a funnel under the outlet of the cooling
chamber to convey the said overflow into a special vessel, thus preventing
its mixture with the previously distilled liquid, which otherwise would
be spoiled and would have to be redistilled.
On the annexed two Sheets of Drawings I have represented my
improved perfumo distilling apparatus. On Sheet 1 are top and sec-
tional front views of the distilling apparatus; Figure 3 is a vertical
section of the expanding chamber alone; and Figure 4 the top view of
it; each on a scale of 11th.
On Sheet 2 I have represented the essence gathering bottle "essencier”
and the overflow preventer "paraflux " in full size.
The boiler as well as the steam expanding chamber and "odorifère"
vessels (Sheet 1) are provided with all the usual safety apparatus such
as level tube steam guage and other; the two "odorifère" vessels or
alembics are besides provided with purging chambers or anti-chloro-
philes," they must be strong enough to sustain 5 atmospheres pressure if
required.
"
The boiler is fed at first with water and afterwards with the bydrolates
resulting from previous distillations or which are produced during the
operation; the said liquid by its cohobation gives off the essential oil
which was still dissolved in it.
The "odorifère" vessels are filled up with flowers, plants, woods, or
other aromatic substances, and steam above the boiling point is let in
from the expanding chamber, where its initial pressure from the boiler
has been lowered as required, according to the kind of substance to be
distilled. The steam impregnated with the perfume is condensed as it
passes through the cooling chambers and the essential oil which
separates from the water is gathered in the bottle already mentioned.
One of the "odorifère" vessels must always work whilst the other
is unloaded from the exhausted substances and filled up with fresh ones.
To perform the alcoholic distillation or making alcoholates with any
aromatic substance I have disposed within one of the "odorifère"

page_text: vessels a helical tube made of tinned copper, which tube is to be heated
by means of water steam. The "odorifère" vessel being filled up to
two-thirds with pure alcohol which is vaporised by the passage of the
steam in the helical tube this "odorifère" vessel being then a alcohol
steam generator. The alcoholic vapors thus produced are conveyed into
the other "odorifère" vessel and runs through the flowers placed over a
wire cloth; this alcoholic steam carries off along with it the perfume of
the aromatic substance to be distilled. When the perfume thus obtained
wants intenseness the operation is stopped and begun anow with fresh
flowers or other aromatic substances through which the perfumed alcohol
previously obtained may be conveyed.
Some aromatic substances must be immersed in alcohol during the
distilling operation; in such case they must be placed directly in the
"odorifère" vessel which is provided with a steam helical tube to be
heated over water boiling point.
The alcoholates could also be rectified in the same apparatus if the
water contained in the flowers or other aromatic substances had weakened
the degree thereof.
I can also employ my apparatus for distilling in vacuum, viz., for
concentrating the hydrolates or alcoholates by taking away the excess of
water they might contain, and even to reduce the same either to a soft,
pasty, or even resinous or hard state.
In order to obtain this result I place in the "odorifère" vessel pro-
vided with a helical tubo either some hydrolate or alcoholate tincture,
and I distil by causing vacuum through a tubular aperture placed
at the top of the "odorifère" vessel by means either of a pneumatic
pump or other contrivance.
A is the boiler provided with all the usual safety implements; B,
odorifère vessels placed on either side of the boiler; they are both
provided with two doors P and Q, the first one for charging the aromatic
substances to be distilled, the second for removing the same after they
have become exhausted.
The steam from the boiler passes through the pipe U to enter the
expanding chamber W, the pipe U is provided with a stop-cock; the
steam is conveyed down through the pipe I near the bottom of the
expanding chamber within which its pressure falls to a lower pitch

page_text: The expanding chamber stands on a hollow column Y through which
the water of condensation is run out once in a while by means of a stop-
cock a from the expanding chamber; tho steam is conveyed alternately
through the pipes S provided with stop-cocks R into the "odorifère"
vessels. The substances to bo distilled are placed on a wire cloth 1,
forming the bottom of the said vessels; on the central part of the wire
cloth a perforated pipe X is fixed and the steam ingressing under the
said pipe passes through its perforations, penetrating every part of the
aromatic substances surrounding it, thus preventing the compact heaping
up of the said substances which might hinder the free passage of the
steam.
The juices which are produced by the first action of the steam fall
through the wire cloth, and gather in the chamber C, from which they
are drawn off by cock o. After its running through the "odorifère"
vessel, carrying off with it the essential oil contained in the aromatic
substances, the steam egresses through the pipe H to enter the cooling
chamber D, which can be fitted with a range of straight pipes t, t, as on
the right-hand side, or with a helical curled one as on the left-hand of
Sheet 1, of the Drawings; in the first case the steam enters the upper
chamber M in which open the tubes t, t, through which it runs to enter
the lower chamber N; as it runs through the tubes the perfumed
steam is condensed by the cooling effect of the water surrounding the
said tubes, tho water proceeding from an upper reservoir enters at E in
the cooling chamber within which it runs upwards around the tubes t
egressing through the tube 6 to enter the upper chamber K, and at last
escape through the surcharged tube d; the cooling chamber on the left
side is disposed as is usual.
The condensed steam containing perfume runs out at n and falls into
an "essencier" within which it circulates, as will be hercin-after
described, where it is successively deprived of the pure essence which
ascends to the upper part and is gathered in an essence bottle, whilst the
water which may still contain some fragrant principle falls into another
receiver and may be used to feed the boiler by means of the hand
pump J or other feeding contrivance.
Some essential oils require to be kept at some degree of heat to
prevent their coagulation during the passage through the "essencier" of
the liquid carrying them along; to effect this I place the said "essencier
"

page_text: in a vessel where I convey the water issuing from the surcharged tubo
of the cooling chamber still warm enough to maintain them in a fluid
state.
It is well understood that each alembic or " odorifère " vessel is used
alternately for the distillation, which is thus performed in an endless
manner; to this effect the stop-cocks R and V on one side must be
stopped, and the corresponding stop-cocks on the other side must be
opened, the "odorifère" vessel to which they pertain having been
charged with aromatic substances while the other one was worked; then
the first one is emptied and recharged with fresh substances while the
second is working.
The "essencier" of my Invention is an improvement of the one
before referred to, as used till now by perfumers; it is based on the
methodic checking of the distilled liquid for the purpose of causing it to
travel a longer way before running out, and to obtain thus a more 1
complete separation of the perfumes it contains.
The principle of the operation is illustrated in Figures 1 and 2, Sheet 2.
The distilled liquid as it runs out from the cooling chamber falls into
the receiver a, and enters the "essencier," within which it passes
successively through eight compartments as will be shown. Fig. 1 is a
vertical section, and Fig. 2 a top view of it, in which the tapered enclosure
has been removed to shew the interior of it; it is made with a tinned sheet
of metal of a cylindrical shape tapering towards the top, and is divided
into 8 compartments by a central tubo B, and seven partitions A, A.
The liquid received in a as mentioned runs down in the tube 6 to 1
enter the first compartment which communicates by means of a small
aperture at the lower part of the partition with the second compartment,
the latter communicates with the third by flowing over the top of the
partition, and so on, and thus the liquid enters successively the 8 com-
partments at the top and bottom. The curved red line, Fig. 2, shows the
course or passage of the liquid through the several compartments from
its entry at a to its exit at c, through the tube D which extends down
near the bottom, the small circles on the partitions, Fig. 2, show the
passage of the liquid at the lower part.
At the top of each compartment the liquid as it passes leaves some of 3
the essential oil it contains; this oil which swims over the liquid, as shewn

page_text: at E, enters the tube F, which conveys it to the essence bottle L, which
bottle has a graduated scale I over which a sliding handle I shews the
result of cach operation or of cach day. Now the essencier is stopped
at the top with a glass stopper G suitably adjusted so as to allow the
inward passage of the liquid to be seen.
As some essential oils are heavier than water, in order to separate the
oil from the liquid, carrying it along as the said liquid issues from the
cooling chamber, I modify the essencier as shown, Fig. 3, which
represents in vertical section the lower part of it; it is constructed
according to the same principle, but the essential oil instead of being
seperated at the top falls down to the bottom from each compartment,
and the partitions which are of a cylindrical form tapered to the lower
part force the liquid to travel up and down the whole length (as shewn
by arrows) before running out, leaving at each time some heavy
essence which drops down (as shown) into a special receiver E, on which
the essencier is fitted, and from which the essence is poured off by
means of a stop-cock C.
The "paraflux" or flood preventor before-mentioned is self-acting,
and by means of a small alarm bell in connexion with it the operator
may be warned when the accident occurs. The same apparatus may be
also advantageously employed in filtering liquids, such as saccharine
juices, sirups, or oils, to prevent the muddy liquid being mixed with the
filtered when the filter happens to burst or crack.
In all the Figures of Sheet 2 illustrating the paraflax from 4 to 9, the
same letters of reference designate the same pieces.
Fig. 1 is a general view showing it in longitudinal section through
the axis of the tubes through which runs the liquid, issuing from the
helical tube of a cooling chamber J; on the end of the said tubo
projecting out of the cooling chamber is fitted the tubulated bit A,
which forms the ingressing aperture of the liquid in the paraflux, which
hollow bit enters about % of an inch on the tubular part B of the
chamber C through which the liquid passes; the said chamber is closed
all around and on the top part, but it is open at the bottom.
The distilled liquid which flows on in a small stream in the tubulated
compartment A, meets with a small projecting picco a, which prevents it
overpassing the said impediment; the liquid falls into the recess D

page_text: within which a small partition 6 stops it; a tube E slightly inclined
opens in the recess D across the partition b, the liquid enters the said
tube which conveys it to the receiver F designed to receive it.
As long as the distillation goes on in a regular manner the liquid
condensed in the helical tube of the cooling chamber follows the direction
pointed out by red arrows, but as soon as sudden extra heating happens
and a superabundance of undistilled liquid is darted into the helical tube
carrying along sometimes solid substances, the said liquid falls no longer
into the recess D but is spurted further into the chamber C as shown by
the black arrow, and as the said chamber has no bottom the liquid falls
into the receiver H, consequently the quality of that previously gathered
in the receiver F will not be spoiled. Now after the sudden perturbation
caused in the distilling apparatus by the intensity of the fire and before
the operation resumes its normal course, it is important to prevent the
liquid now in the helical tube and which has been mixed with the
spurted flood to arrive in the receiver F, the contents of which would be
spoiled. I obtain this important result by joining to the paraflux a
simple self-acting contrivance. Under the chamber C through which
the overflow runs, which chamber is open at its lower part, I hang a
swing box G hinging round a pin I, so that its natural equilibrium
position be as shown, Fig. 1, when it contains no liquid, but the capacity
of this box into which the liquid falls being greater on one side than on
the other the equilibrium is instantaneously interupted; the box G
swings round its axis and takes the position G', as shown by red lines.
The box G is provided with a vertical picco L attached to its bottom;
in the swing movement of the box, the piece L which is touching at T
the end part of an inclined tube, pushes the said tube (the end of which
bears a small basin or receiver M) and brings it in the position M'
figured with red lines, the piece L being then in the position L'. Tho
basin M being then under the aperture of the tube E, the liquid issuing
from it runs through the inclined tube T, which conveys it to chamber
C, and it falls into II as long as the operator who has been warned by an
alarm bell, actuated by the swinging of the box G, may seo if the
distilling liquid issuing from the tube E be restored to its required
clearness, then he will push back the basin M to its place; in this a
sliding motion the crooked end T of the sliding tube pushes back the
piece L, and the box G is restored to its normal position where it is
maintained by the small balanco weight d.

page_text: a small basin which is brought under the outlet of the distilled liquid to
prevent its falling into the bottle, this being operated by the action of the
swing box when an overflow of the liquid is spurted out of the cooling
chamber, the said swing box by its movement causing a small alarm bell
to ring for warning the attendant, which restores all things right and
the distilled liquid runs clear, the said paraflux being represented on
Sheet 2.
Fifthly and lastly. I claim applying the "paraflux" for filtering
liquids, and preventing the muddy liquid being mixed with the clear in
the event of the filter being broken or bursting.
In witness whereof, I, the said Alphonse Piver, have hereunto set
my hand and seal, this Seventh day of August, in the year of our
Lord One thousand eight hundred and seventy-four.
Signed and sealed in the
presence of
L. D'AUBRÉVILLE, O.E.
ALPHONSE PIVER. (L.s.)