IMPROVEMENTS IN EXTRACTING ESSENCES AND PERFUMES AND ALSO OILS AND FATS FROM MATTERS CONTAINING THEM, ALSO IN BLEACHING AND PURIFYING OILS AND FATS, AND IN APPARATUS EMPLOYED THEREIN
Year: 1863

page_text: LETTERS PATENT to Heinrich Hirzel, Doctor of Philosophy, and Lecturer
on Chemistry and Pharmacy at the University of Leipzig, now residing
at the Terminus Hotel, London Bridge, in the Borough of Southwark
and County of Surrey, for the Invention of "IMPROVEMENTS IN EXTRACTING
ESSENCES AND PERFUMES AND ALSO OILS AND FATS FROM MATTERS CONTAINING
THEM, ALSO IN BLEACHING AND PURIFYING OILS AND FATS, AND IN APPARATUS
EMPLOYED THEREIN."
Sealed the 13th May 1864, and dated the 27th November 1863.
PROVISIONAL SPECIFICATION left by the said Heinrich Hirzel at the
Office of the Commissioners of Patents, with his Petition, on the 27th
November 1863.
I, HEINRICH HIRZEL, Doctor of Philosophy, and Lecturer on Chemistry
and Pharmacy at the University of Leipzig, now residing at the Terminus
Hotel, London Bridge, in the Borough of Southwark and County of Surrey,
do hereby declare the nature of the Invention for "IMPROVEMENTS IN Ex-
TRACTING ESSENCES AND PERFUMES AND ALSO OILS AND FATS FROM MATTERS CON-
TAINING THEM, ALSO IN BLEACHING AND PURIFYING OILS AND FATS, AND IN APPARATUS
EMPLOYED THEREIN."
This Invention has for its object improvements in extracting essences and
perfumes and also oils and fats from matters containing them, also in bleaching
and purifying oils and fats, and in apparatus employed therein.
For the purpose of extracting essences and perfumes from flowers, spices,
or other matters containing them, the flowers or other matters are placed in
cylindrical or other vessels which are closed air-tight, and purified petroleum

page_text: is allowed to enter at the top of one vessel from a reservoir above, and to
descend through the material contained therein; at the bottom of this
vessel the purified petroleum passes out and is then caused to enter a
second similar vessel, also containing the flowers or material to be treated,
amongst which it passes as before, and so on, the purified petroleum being
caused to pass through any convenient number of vessels, and it extracts in
each the essence or perfume from the materials they contain. The petroleum
then descends into a receiver and by steam heat it is distilled off, leaving
behind in the receiver the essence or perfume it had previously taken up.
The vapour of the petroleum is passed into a condenser placed above the
reservoir from which the petroleum is drawn for use, and when condensed it
falls back into the same vessel to be again used.
For extracting essences and perfumes the petroleum is prepared for use by
carefully separating from it by distillation oils having a high boiling point, and
it is otherwise carefully purified, so that it may impart neither taste or smell
to the essence or perfume. When the flowers, spices, or other materials in the
first of the vessels are exhausted the vessel is detached and another vessel con-
taining fresh material substituted for it, but at the end of the series, and by an
air pump or otherwise, a current of air is drawn through the vessel containing
the exhausted material, the same being at the same time heated by steam
circulating in a coil within the vessel; in this manner any remaining petroleum
is evaporated and drawn off; this is afterwards condensed and returned to the
reservoir.
In a similar manner oils and fats may be separated from seeds, bones,
and other matters containing them, but in this case the purification of the
petroleum need not be carried so far, as the boiling point of the petroleum may
without inconvenience be higher than is admissible for the extraction of
essences and perfumes.
The process above described is applicable for the extraction of the finest
essences from flowers, spices, woods, roots, herbs, and similar substances;
also for the extraction of oil from linseed, mustard, rape, and other seeds, and
fat and oil from bones. It is also applicable for extracting from wool the
oil which is applied to it in the processes of manufacture.
For the purification of oils and fats I cause the oils and fats to be dissolved in
purified petroleum and the solution to filter through animal charcoal. The appa-
ratus is slightly modified from that before described, the purified petroleum
descends from a reservoir into a vessel heated by steam and containing the crude
oil or fat, which it dissolves, and the solution then passes into cylindrical or other
vessels below; these vessels are filled with animal charcoal, the filters are heated

page_text: by steam, and the solution filters through the charcoal and then passes into a
receiver, where, as before, the petroleum is distilled off leaving behind the
purified oil or fat. The petroleum vapour also as before is condensed and
returned to its reservoir to be again used. When the animal charcoal is unfit
for further use it is washed with the petroleum to free it from oil or fat, and
then by drawing a current of air through it with the air pump the petroleum
is evaporated off.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Heinrich Hirzel in the Great Seal Patent Office on the
27th May 1864.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, HEINRICH
HIRZEL, Doctor of Philosophy, and Lecturer on Chemistry and Pharmacy at
the University of Leipzig, now residing at the Terminus Hotel, London
Bridge, in the Borough of Southwark and County of Surrey, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-seventh day of November, in the year of our
One Lord thousand eight hundred and sixty-three, in the twenty-seventh year
of Her reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said Heinrich Hirzel, Her special licence that I, the said Heinrich Hirzel,
my executors, administrators, and assigns, or such others as I, the said Heinrich
Hirzel, my executors, administrators, 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
EXTRACTING ESSENCES AND PERFUMES AND ALSO OILS AND FATS FROM MATTERS
CONTAINING THEM, ALSO IN BLEACHING AND PURIFYING OILS AND FATS, AND IN
APPARATUS EMPLOYED THEREIN," upon the condition (amongst others) that I, the
said Heinrich Hirzel, 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 Heinrich Hirzel, do hereby declare
the nature of the said Invention, and in what manner the same is to be

page_text: performed, to be particularly described and ascertained in and by the following
statement thereof, that is to say:-
This Invention has for its object improvements in extracting essences and
perfumes and also oils and fats from matters containing them; also in bleaching
and purifying oils and fats, and in apparatus employed therein.
For the purpose of extracting essences and perfumes from flowers, spices, or
other matters containing them, the flowers or other matters are placed in cylin-
drical or other vessels, which are closed air-tight, and purified petroleum is
allowed to enter at the top of one vessel from a reservoir above, and to descend
through the material contained therein; at the bottom of this vessel the purified
petroleum passes out and is then caused to enter a second similar vessel, also con-
taining the flowers or material to be treated, amongst which it passes as before,
and so on, the purified petroleum being caused to pass through any convenient
number of vessels, and it extracts in each the essence or perfume from the
materials they contain. The petroleum then descends into a receiver, and by
steam heat it is distilled off, leaving behind in the receiver the essence or
perfume it had previously taken up. The vapour of the petroleum is passed
into a condenser placed above the reservoir from which the petroleum is drawn
use, and when condensed it falls back into the same vessel to be again used.
For extracting essences and perfumes the petroleum is prepared for use
by carefully separating from it by distillation oils having a high boiling
point, and it is otherwise carefully purified, so that it may impart neither taste
or smell to the essence or perfume. When the flowers, spices, or other
materials in the first of the vessels are exhausted, the vessel is detached and
another vessel containing fresh material substituted for it, but at the end of
the series, and by an air pump or otherwise, a current of air is drawn through
the vessel containing the exhausted material, the same being at the same time
heated by steam; in this manner any remaining petroleum is evaporated and
drawn off; this is afterwards condensed and returned to the reservoir.
for
In a similar manner oils and fats may be separated from seeds, bones, and
other matters containing them; but in this case the purification of the petroleum
need not be carried so far, as the boiling point of the petroleum may without
inconvenience be higher than is admissable for the extraction of essences and
perfumes.
The process above described is applicable for the extraction of the finest
essences from flowers, spices, woods, roots, herbs, and similar substances; also
for the extraction of oil from linseed, mustard, rape, and other seeds, and fat
and oil from bones. It is also applicable for extracting from wool the oil
which is applied to it in the processes of manufacture.

page_text: For the purification of oils and fats I cause the oils and fats to be dissolved
in purified petroleum and the solution to filter through animal charcoal. The
apparatus is slightly modified from that before described; the purified petro-
leum descends from a reservoir into a vessel heated by steam and containing
the crude oil or fat, which it dissolves, and the solution then passes into cylin-
drical or other vessels below; these vessels are filled with animal charcoal, the
filters are heated by steam, and the solution filters through the charcoal and
then passes into a receiver, where, as before, the petroleum is distilled off,
leaving behind the purified oil or fat. The petroleum vapour also, as before,
is condensed and returned to its reservoir to be again used. When the animal
charcoal is unfit for further use it is washed with the petroleum to free it from
oil or fat, and then by drawing a current of air through it with the air pump
the petroleum is evaporated off.
And in order that my said Invention may be most fully understood and
readily carried into effect, I will proceed to describe the Drawings hereunto
annexed.
DESCRIPTION OF THE DRAWINGS.
Figure 1 is a front view of the apparatus I employ; Figure 2 is a vertical
section at the line y, y (Figure 1); Figure 3, a horizontal section at the line
z,, (Figure 1); and Figure 4 is a cross section of the compound pipe k, shown
full size.
A represents an hermetically closed reservoir for the reception of the
petroleum ether serving for extraction. This reservoir is situated above the
cylinders for extraction in order that the petroleum ether may easily run into
them. In some instances, however, I place the reservoir A lower, and drive
the petroleum ether into the cylinders by pressure; 6 and 6¹ are pipes with
cocks for passing the petroleum ether into the extraction cylinders B and B¹,
which are connected together by two pipes c and c¹, so that the petroleum ether
which runs into the one cylinder from above flows out of it from below, and is
led into the upper part of the second cylinder and flows through this and the
substances the cylinders are filled with. These cylinders have double walls,
and steam circulates between the inner and external wall, in order to warm
the contents of the cylinder when required for assisting the extraction and the
drying of the extracted material. At y and y¹ are the cocks to admit the
steam, and at x and x' the cocks to discharge it. The cylinders for extraction
are firmly fixed on suitable supports, and are hermetically closed by covers and
the screws o and o¹. In filling the cylinders the cover is to be taken off, and
the material to be extracted is either put at once into them, or, better, it
sieve that fits into the cylinders, so as to be easily put
is to be filled into a

page_text: in and taken out. Instead of having only two cylinders, as shown in the
Drawing for the sake of simplicity, three, four, or more in communication with
each other may be employed in the same way, the action of the apparatus
being carried on without interruption, and one cylinder after the other emptied
and filled and put into action again. To ascertain if the petroleum ether flowing
through either of the cylinders has dissolved any of the contents thereof, or
whether the extraction is finished, as regards the contents of this cylinder, the
pipes c and c¹ are furnished with small stop cocks p and p', through which a small
quantity of the petroleum ether may be drawn off and tested; C, C', are stills in
which the petroleum ether flows after having passed through the cylinders wherein
it has absorbed the greases, odoriferous or aromatic substances. The stills are
furnished with the guage glasses f and f¹, which show how much liquid they
contain; d and d¹ (indicated by dotted lines) is a pipe in the still into which the
steam can be admitted by the cocks 9 and g', whilst the escaping steam issues
from the still through the cocks w and w¹; e, e¹, (indicated by dotted lines) is
a steam ring underneath the steam pipe d; it is furnished with small holes to
lead the steam direct into the contents of the still if required, for which
purpose the pipe with its stop-cock and may be used. The short head on
the cover of the still is contracted into the ascending pipe h and h¹, which is
divided at the cock i in two pipes, one of which, k, leads to the cooling appa-
ratus D, whilst the other one m and m¹ leads from one still into the other, so
connecting them together in order to allow of distilling from one still into the
other as is sometimes required. In this arrangement it will be seen that the
uninterrupted action of the apparatus is possible, for when one of the stills is
filled two-thirds full the process of distilling is commenced, and the petroleum
ether flowing out of the cylinders is let into the other still. The vapour of
the petroleum ether formed by heating the still by the steam pipe is led into
the cooling apparatus by the pipe k rising as above mentioned to the appa-
ratus D. In order to prevent the condensation of this steam in the pipe k,
(which would cause it to run back into the still,) this pipe is a combination of
three pipes, one of which is larger than and surrounds the others. The inner-
most pipe k is for the distilling petroleum ether, the second pipe enclosing k
(see the sectional view, Figure 4,) is destined for the passage of air, which is
warmed by this means, and serves for drying the material in the cylinders
when the extraction is complete; the exterior widest pipe k" is connected
with the steam pipe of a boiler, or is otherwise, as herein-after mentioned,
furnished with steam, and acts as heating pipe for both the pipes enclosed by
it. The draw-off cocks n and n¹ of the still serve for emptying the still and
principally for drawing off the extracted fat, odoriferous and aromatic sub-
k'

page_text: stances.
F is a common air pump to be put in communication with one or
the other of the cylinders through the pipes u and u¹. When the substance
in one of the cylinders is sufficiently extracted with the petroleum ether all the
petroleum ether is to be drawn out of this cylinder into the still, after which
the cocks on the pipes connecting the cylinder with the reservoir A, with the
stills and the other cylinders, are to be shut; at the same time the cocks of
the pipe u or u¹ are to be opened as well as the cock of the pipe t or t¹, which
causes the warm air to enter through the pipe k into the cylinder. The
pump is now to be put into action, and by it the warm air is sucked through
the pipet or into the cylinder; it passes through the contents of the same,
which effects the evaporation of the petroleum ether; afterwards it passes,
together with the vapours of the petroleum ether in the pump, through the
pipe u and u¹, is led from here through the pipe v into the cooling apparatus D,
where the vapours of the ether are condensed again and flow into the appa-
ratus A. When a stream of warm air has passed for some time through
the cylinder all petroleum ether is evaporated and the extracted substance
becomes quite dry, and when the cylinder is opened can be taken out and
replaced by new substance. In some cases the drying can be accelerated
by letting steam into the space between the outer and inner wall of the cylinder
and so heating it. The air which is sucked through the cylinder to dry its
contents comes out of the upper part of the closed reservoir A, passes through
the pipe q, and enters at r into the middle pipe k, rises in this, and comes out
again of the pipe k at s, from where it is either conducted through the pipe t to
the one or through the pipe t' to the other cylinder, according as the contents of
one or the other cylinder are to be dried. In consequence of this construction the
same air is always circulating, and there is very little loss of petroleum ether. But
as during the operation a little gas is always formed from the petroleum ether,
and thus the pressure might become too high in the apparatus, the reservoir A
is furnished with a small safety valve which opens by the pressure, and allows
the gas to escape, or the reservoir A is by means of a pipe connected with a
small gasometer, where the gas can be collected. The cooling apparatus is a
kind of cylinder, which is furnished with cold water by the pipe z. This
cylinder contains a double casing, into which the vapours to be condensed are
led, and the condensed liquid passes by a pipe into the vessel A. At the front
of the cooling apparatus is the part E covered with a semi-globe of glass to
allow to be easily observed the quantity of liquid passing off from the cooling
apparatus.
The distillation is carried on in the following manner:-When one of the
stills C is filled two-thirds full with liquid it is cut off from the cylinders B. B¹.

page_text: by shutting the cocks so that no more petroleum ether may run into this still.
After this steam is admitted by the steam pipe in the still to make its contents
boil and distil through the pipe k into the reservoir A. The steam coming
out of the steam pipe at the cocks w or w¹, is led into k¹¹, in order to use all
its heat. When, by means of the heat of the steam pipe, the greatest part
of the petroleum ether is distilled into the reservoir A, the steam pipe is shut
because the beat would not be sufficient to distil all the petroleum ether, at
least not after the extraction of greasy substances. To complete the operation,
steam is admitted direct into the still by the steam ring e and e¹; thus the
remaining petroleum ether is evaporated and the extracted greasy substances
remain pure in the still, and can be taken out with the water that may have
collected through the cock m or m¹. As during this last operation a great
deal of water distills over with the vapours of the petroleum ether they are
not to be led through the pipe k into the cooling apparatus, but through pipe
m or m¹ into the other still, where they are condensed. In may happen some-
times that a little water comes into the reservoir A with the petroleum ether,
this may be let off by the cock e, as it always sinks to the bottom.
I will now proceed to give special explanations concerning the management
of the apparatus and the process of extraction.
According to the substance to be extracted different kinds of volatile petro-
leum ether should be applied. The petroleum ether is prepared from the
naphtha of the best Pennsylvanian petroleum in the following manner :-The
naphtha is distilled by steam, and that part is collected which distils at a
temperature of not more than 230° Fahrenheit; this is purified by shaking
it with sulphuric acid and caustic of soda; after this it is washed well with
water, and when it has been separated from the water it is again distilled.
The first part of the distillate, whose boiling point should not be higher than
140° Fabrenheit, is used for extracting the odours of flowers and aromatics
from spices; the second part, whose boiling point is about 170° Fahrenheit, is
used for extracting fats and greasy oils out of seeds and similar substances, as
well as for bleaching fat, wax, and other materials, and the third part, of
which the boiling point is about 220° Fahrenheit, is used for freeing wool,
cotton, and other fibre or substance from grease.
In the extraction of flowers and spices with petroleum ether the apparatus
used may be somewhat modified. The extraction cylinders do not require
double walls, as it is not necessary to heat them, and there is no steam led
direct into the stills, as the evaporation of this petroleum ether can be
effected by a very gentle heat. The scent remaining in the still (which is
but a small quantity) may be directly dissolved in spirit of wine and formed

page_text: into merchantible essence. The flowers may be filled loose into the extraction
cylinders, and are soaked for 2 or 3 hours with the petroleum ether; after
this the ether is drawn off into the still. Even the delicate odour of reseda
can be extracted in this way.
In the extraction of fats and greasy oils with petroleum ether the same
apparatus is used as is represented in the Drawing. A crushing mill is also
employed near to the apparatus wherein the seeds or materials are crushed,
and after this they are filled into sieves, which, when filled, can be put into
the extraction cylinders. The residues of these substances, after extraction,
are dry and without smell.
In the purification of greasy oils, wax, and similar substances by petroleum
ether the extraction cylinders are filled with animal charcoal. A kettle with
a mechanical stirrer is affixed to the apparatus. In this kettle the substances
to be purified are dissolved by heat if necessary, and mixed with sufficient
petroleum ether to cause it to run freely through the charcoal in the cylinders
into which the mixture is then passed. The petroleum ether is let down into
the kettle from a reservoir above, and from the kettle the mixture descends
to the cylinders. With these alterations the apparatus is the same as before
described.
In the extraction of fat out of wool, cotton, and similar fibres and substances
the apparatus is the same as described and shown in the Drawing.
Having thus described the nature of my said Invention, and the manner
of performing the same, I would have it understood that what I claim is,-
First, the extracting essences and perfumes, and also oils and fats, from
matters containing them by means of petroleum ether, as herein-before
described.
Second, I claim the bleaching and purifying oils and fats by mixing them
with petroleum ether, passing them through animal charcoal, and then distilling
off the petroleum ether, as herein-before described.
Third, I claim the method of constructing and arranging apparatus for con-
ducting the above processes, as herein-before described.
In witness whereof, I, the said Heinrich Hirzel, have hereunto set my
hand and seal, this Twenty-first day of May, in the year of our Lord
One thousand eight hundred and sixty-four.
HEINRICH HIRZEL. (L.S.)