Improvements relating to the Lixiviation of Dye-wood, Bark, Hops, and other Materials, and to Apparatus therefor.
Year: 1894

page_text: Date of Application, 1st May, 1894 -
Complete Specification Left, 30th Jan., 1995-Accepted, 9th Mar., 1895
PROVISIONAL SPECIFICATION.
Improvements relating to the Lixiviation of Dye-wood, Bark, Hops,
and other Materials, and to Apparatus therefor.
I, CHRISTOPH Ludwig WILHELM ALBACH, of Höchst-on-the-Main, in the
Empire of Germany, Copper-smith, do hereby declare the nature of this invention
to be as follows:-
My invention relates to lixiviation of dye-wood, bark, hops and other materials
and to apparatus therefor.
In order to extract from dye wood, bark, hops and similar natural products the
valuable substances which they contain I use the apparatus hereinafter set forth,
which is also particularly adapted for lixiviating materials containing ethereal oils,
resins or the like.
In this apparatus the materials to be lixiviated are first strongly heated by
superheated steam which passes through them from below, so that they will exude
the substances to be obtained, such as ethereal oils or the like. While the heating
is continued by steam entering from above, the said materials are then lixiviated
by the water condensed from this steam and which is continually conducted away.
Of special importance in this case is that the vapours introduced are superheated,
for a portion of the substances to be obtained can be extracted or exuded from the
materials only by such vapours, but not by boiling water or by vapours at the
ordinary pressure. Only when this has taken place will lixiviation by condensert
water be possible.
The extract obtained is then drawn off through suitable pipes, provided with an
overflow pipe which is surrounded by a glass casing and by which the progress of
the lixiviation may at any time be ascertained.
My improved apparatus comprises an evaporating vessel, a boiler and a condensing
vessel placed above the latter and connected with it by a large pipe.
The evaporating vessel is heated by a closed steam coil and is in connection with
the boiler by a steam pipe.
I introduce the liquids necessary for the lixiviation of the materials, such as
alcohol, ether or the like, through a funnel, while the water for the supply of the
steam generator is admitted through a cock, for which purpose use is preferably
made of the cooling water which runs off and is therefore preliminarily heated.
The boiler is of the simple vertical type, closed by a cover provided with an air
cock. Near its bottom this boiler possesses a discharge orifice adapted to be closed
by a lid. In the lower part of the boiler is placed a partition and a fine sieve, and
at its upper part another partition. The steam admission pipe terminates on the
one hand in the chamber above the upper partition and on the other hand in the
chamber beneath the lower partition. The admission of steam is regulated by
two valves. From the chamber beneath the lower partition a pipe provided with a
testing cock leads upwards and terminates in an overflow pipe. This overflow pipe
terminates in a vessel furnished with the spy-glass and having at the top an air cock.
A pipe extends from the said vessel to the collecting vessel. The large pipe
leading to the condensing vessel passes through the bottom of the casing of this
vessel and ends below a distributing cap in a lower cooling chamber which is
connected by cooling pipes with an upper cooling chamber. On the latter chamber
is an air discharge cap which is provided at its lower side with holes. These holes
prevent the formation of pressure in the condensing vessel and allow the admission

page_text: of the air necessary for condensing the steam. The aforesaid two cooling
chambers and the intermediate pipes in the condensing vessel are surrounded by
the casing of this vessel, this casing being provided with two cocks for regulating
the inlet and outlet of the cooling water circulating round the said cooling chambers
and pipes.
When the apparatus is to be set in operation the material to be lixiviated is
introduced into the boiler after removing the cover and the upper partition, so
that it will entirely fill up the space between the upper and lower partitions. Then
the upper partition is put in again and the cover secured by means of screws
fixed to turn on the boiler and of thumb nuts appertaining thereto.
After all the cocks and valves with the exception of the air cock at the top of
the boiler have been closed the steam valve is opened so that superheated steam.
generated in the evaporating vessel will pass into the chamber beneath the lower
partition and will pass through the material in the boiler from below. As soon as
the steam has passed through the materials contained in the boiler and fills up the
entire inner space, which is recognized by the air cock, the latter is closed. The
steam which further enters is conducted, after passing through and heating
the material, by the large pipe to the condensing vessel. When this steam has
penetrated into the condensing vessel to such an extent that it has heated the
water of the same so that cooling must take place, and when the heating of the
materials contained in the boiler and the exudation of the substances to be
extracted have progressed far enough the aforesaid steam valve is also closed,
whereas the second steam valve and the air cock at the top of the vessel provided
with the spy glass are opened. The steam now passes into the upper chamber of
the boiler and also penetrates into the partially lixiviated material which it keeps
boiling. For the most part it passes however through the large pipe to the con-
densing vessel where it is condensed in the lower cooling chamber and in the
intermediate pipes. The condensed water flows back through the large pipe to the
boiler, trickles through the boiling material and lixiviates the same and also
the substances, such as oils and the like, exuded from it by the superheated steam.
The extract thus obtained gradually fills the boiler and also passes into the rising
tube connected with it after being cleaned or filtered by the lower sieve. When
the extracted substance has risen to such a height that it flows from the overflow
pipe into the receptacle at the top, which may be observed through the spy glass,
the cock of the discharge pipe is opened, and the extract becoming gradually
weaker and weaker then flows into the collecting vessel. When, judging by the
overflow pipe, I consider the material to have been completely lixiviated I close
the air cock and the second steam valve again. The rising and discharge pipes in
combination with the said receptacle now form a siphon which draws all the
extract contained in the boiler into the collecting vessel. If however the whole
liquid is not to be drawn off, the air cock at the top of the receptacle must not be
closed.
When the material has not yet been completely lixiviated the operation may
be repeated one or more times in the before described manner, that is to say
until the overflow pipe indicates that the materials have been completely
. lixiviated.
All the liquid having been drawn off by the siphon and the remainder let off to
the testing or discharge cock the boiler, after the removal of the lid, is emptied
through its lower lateral opening and may now be cleaned, whereupon it is ready
to be filled again. During the lixiviation I may at any time take samples at the
testing or discharge cock.
With materials which can be extracted only by alcoholic or other vapours not
containing water, such vapours of course take the place of the water vapours.
Instead of the repeated steaming considered necessary with many materials for
preparing them, I may in the case of certain materials add some alcohol to the
water in the vaporizing apparatus, such alcohol being introduced through the
-before-mentioned funnel. The lighter alcoholic vapours then rise through the pipe

page_text: earlier than the water vapours and dissolve the oils and resins in the materials so
that these will combine subsequently with the continually decreasing alcoholic
vapours and finally with the following water vapours and enable a complete
lixiviation to take place. The alcoholic vapours which are first condensed not only
do not injure the extract but preserve the same. In the use of such extracts
which are added to a liquid, such as for instance the extract of hops in the
manufacture of beer, the two are boiled once; the alcohol has up to that time
preserved the extract well, and the alcoholic vapours volatilize rapidly and have
no deleterious action. In lieu of alcohol I may use ether, acetone or other
extractive substances for certain materials.
Dated this 1st day of May 1894.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.
Improvements relating to the Lixiviation of Dye-wood, Bark, Hops,
and other Materials, and to Apparatus therefor.
I, CHRISTOPH LUDWIG WILHELM ALBACII, of Höchst-on-the-Main, in the.
Empire of Germany, Copper-smith, 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 :-
My invention relates to the lixiviation of dye-wood, bark, hops and other
materials and to apparatus therefor.
In order to extract from dye wood, bark, hops and similar natural products the
valuable substances which they contain I use the apparatus represented in the
accompanying drawing which is also particularly adapted for lixiviating materials
containing ethereal oils, resins or the like.
In this apparatus the materials to be lixiviated are first strongly heated by
superheated steam which passes through them from below, so that they will exude
the substances to be obtained, such as ethereal oils or the like; while the heating
is continued by steam entering from above, the said materials are then lixiviated
by the water condensed from this steam and which is continually conducted away.
Of special importance in this case is that the vapours introduced are superheated,
for a portion of the substances to be obtained can be extracted or exuded from the
materials only by such vapours, but not by boiling water or by vapours at the
ordinary pressure. Only when this has taken place will lixiviation by condensed
water be possible.
The extract obtained is then drawn off through suitable pipes provided with an'
overflow pipe which is surrounded by a glass casing and by which the progress of
the lixiviation may at any time be ascertained.
My improved apparatus comprises an evaporating vessel A a boiler B and a
condensing vessel C placed above the latter connected with it by a large pipe B¹.
The evaporating vessel A is heated by a closed steam coil and is in connection
with the boiler B by a steam pipe g.
introduce the liquids necessary for the lixiviation of the materials, such as
alcohol, ether or the like, through a funnel a' while the water for the supply of
the steam generation is admitted through a cock d, for which purpose use is
preferably made of the cooling water which runs off and is therefore preliminarily
heated.
The boiler B is of the simple vertical type, closed by a cover provided with
an air cock . Near its bottom this boiler is provided with a discharge orifice
adapted to be closed by a lid c. In the lower part of the boiler is placed a

page_text: partition and a fine sieve e, and at its upper part another partition is provided.
The steam admission pipe terminates on the one hand in the chamber above the
upper partition f and on the other hand in the chamber beneath the lower
partition e. The admission of steam is regulated by two valves h and i. From
the chamber below the lower partition e a pipe k provided with a testing cock
leads upwards and terminates in an overflow pipe m. This overflow pipe terminates
in a vessel o furnished with the spy-glass or lantern n and having at the top an air
cock p. A pipe r extends from the said vessel o to the collecting vessel s. The
large pipe B leading to the condensing vessel C passes through the bottom of the
casing of this vessel and ends below a distributing cap in a lower cooling
chamber u which is connected by cooling pipes v with an upper cooling chamber 10.
On the said chamber is an air discharge cap which is provided at its lower side
with holes. These holes prevent the formation of pressure in the condensing
vessel and allow the admission of the air necessary for condensing the steam. The
two cooling chambers u and w and the intermediate pipes in the condensing
vessel are surrounded by the casing of this vessel, this casing being provided with
two cocks and y for regulating the inlet and outlet of the cooling water
circulating round the said cooling chambers and pipes.
When the apparatus is to be set in operation the material to be lixiviated
is introduced into the boiler B after removing the cover and the upper
partition so that it will entirely fill up the space between the upper and lower
partitions e and f. Then the upper partition is put in again and the cover b
is secured by means of screws fixed to turn on the boiler and of thumb nuts
appertaining thereto.
After all the cocks and valves with the exception of the air cock b' at the top
of the boiler have been closed the steam valve bis opened so that superheated
steam generated in the evaporating vessel will pass into the chamber beneath
the lower partition e and will pass through the material in the boiler from below.
As soon as the steam has passed through the materials contained in the boiler
and fills up the entire inner space which is recognized by means of the air cock 6'
the latter is closed. The steam which further enters is conducted, after passing
through and heating the material, by the large pipe B₁ to the condensing
vessel C'.
When this steam has penetrated into the condensing vessel to such an extent
that it has heated the water of the same, so that cooling must take place, and
when the heating of the materials contained in the boiler B and the exudation
of the substances to be extracted have progressed far enough the aforesaid steam
valve h is also closed, whereas the second steam valve i and the air cock p at the
top of the vessel n are opened. The steam now passes into the upper chamber
of the boiler B and also penetrates into the partially lixiviated material which it
keeps boiling. For the most part it passes however through the large pipe B₁ to
the condensing vessel C where it is condensed in the lower cooling chamber u and
in the intermediate pipes v. The condensed water flows back through the large
pipe B' to the boiler B trickles through the boiling material and lixiviates the
saine and also the substances, such as oils and the like, exuded from it by the
superheated steam. The extract thus obtained gradually fills the boiler B and
also passes into the rising tube connected with it after being cleaned or filtered by
the lower sieve, e. When the extracted substance has risen to such a height that
it flows from the overflow pipe m into the receptacle o which may be observed
through the spy glass n, the cock of the discharge pipe r is opened, and the extract
becoming gradually weaker and weaker then Hows into the collecting vessel 8.
When, judging by the overflow pipe, I consider the material to have been
completely lixiviated I close the air cock p and the steam valve i again. The
rising and discharge pipes and r in combination with the vessel o form a siphon
which draws all the extract coutained in the boiler B into the collecting vessel s.
If however the whole liquid is not to be drawn off the air cock p at the top of
the receptacle must not be closed.

page_text: When the material has not yet been completely lixiviated the operation may be
repeated one or more times in the before described manner, that is to say until
the overflow pipe indicates that the materials have been completely lixiviated.
All the liquid having been drawn off by the siphon k, o, and the remainder
let off to the testing or discharge cock the boiler, after the removal of the lid c
is emptied through its lower lateral opening and may now be cleaned, whereupon
it is ready to be filled again. During the lixiviation I may at any time take
samples at the testing or discharge cock 7.
With materials which can be extracted only by alcoholic or other vapours not
containing water, such vapours of course take the place of the water vapours.
Instead of the repeated steaming considered necessary with many materials for
preparing them, I may in the case of certain materials add some alcohol to the
water in the vaporizing apparatus, such alcohol being introduced through the
before-mentioned funnel a¹. The lighter alcoholic vapours then rise through
the pipe earlier than the water vapours and dissolve the oils and resins in the:
materials so that these will combine subsequently with the continually decreasing
alcoholic vapour and finally with the following water vapours and enable a
complete lixiviation to take place. The alcoholic vapours which are first.
condensed not only do not injure the extract but preserve the same.
In the
use of such extracts which are added to a liquid, such as for instance the extract.
of hops in the manufacture of beer, the two are boiled once; the alcohol has up.
to that time preserved the extract well, and the alcoholic vapours volatilize
rapidly and have no deleterious action. In lieu of alcohol I may use ether
acetone or other extractive substances for certain materials.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
First. A method of lixiviating materials by first preparing them by means of
vapours of alcohol, water, ether, acetone or other extractive substances, which are
conducted through the same, whereupon for the purpose of obtaining the extractive
substances the vapours are conducted over the mass while heating the latter and
into a condenser, from which the hot water of condensation flows back into the
mass in order to lead away the substances to be extracted.
Second. An apparatus designed for carrying out the method set forth in the
first claim, in which the materials to be lixiviated are placed between two.
sieves e, f, and in which the admission of steam takes place from above or from.
below through steam pipes 9 adapted to be closed, the space situated above the
upper sieve being connected with the condenser C, while the lower space is.
provided with devices for letting off the extract.
Third. In the apparatus characterized in the second claim the discharge of the
extract by means of a rising pipe & which for the purpose of continually observing
the condition of the extract terminates above as an overflow pipe in a lantern n,
from which the extract flows off through a pipe p, the lantern being moreover provided
with an air cock p for enabling the lixiviating vessel to be emptied at times by
siphon action after closing the cock, all substantially as described and represented
in the drawings.
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HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant