IMPROVED METHOD OF AND APPARATUS FOR LIXIVIATING VEGETABLE AND ANIMAL MATERIALS AND OBTAINING EXTRACTS THEREFROM
Year: 1882

page_text: LETTERS PATENT to Carl Heckmann and Eugen Hausbrand both of Berlin
Prussia, for an invention of "IMPROVED METHOD OF AND APPARATUS FOR
LIXIVIATING VEGETABLE AND ANIMAL MATERIALS AND OBTAINING EXTRACTS
THEREFROM
גן
PROVISIONAL SPECIFICATION left by the said Carl Heckmann and Eugen
Hausbrand at the Office of the Commissioners of Patents on the 18th April
1882.
CARL HECKMANN and EUGEN HAUSBRAND, both of Berlin, Prussia, " IMPROVED
METHOD OF AND APPARATUS FOR LIXIVIATING VEGETABLE AND ANIMAL MATERIALS
AND OBTAINING EXTRACTS THEREFROM
"
The object of our invention consists in the lixivation of vegetable and animal
materials by means of an improved method, either for the purpose of freeing such
materials from resinous, agglutinant and other substances, or for obtaining therefrom
valuable extracts. Besides, the invention comprises a special apparatus for carrying
out the process.
The materials to be treated and the lixivating liquid, for instance water, alkohol,
ether, sulphuret of carbon, &c., are put into a closed vessel in such a manner that
the former are supported or suspended above the latter. The liquid at the bottom
of the vessel is then heated in order that it may emit vapours, which, after having
passed through the materials, are condensed by being brought in contact with
refrigerating surfaces at the top of the vessel. The liquid of condensation thus
formed drips down on and percolates the materials, and thereby dissolves the
extractible substances softened by the vapours, and carries them down into the
bulk of the liquid. The lixivation having been completed, the liquid containing
the extracted substances is drawn off, while the residue of liquid in the treated
materials is evaporated and recovered by condensation in a special condenser.
The apparatus which we prefer to use for carrying out this process consists in a
horizontal cylinder or a vessel of other shape, having at one end a large opening,
which may be hermetically closed by a covor, and through which a perforated box
containing the materials to be treated, may be introduced. This box is supported
DC21

page_text: in a suitable manner about in the middle of the cylinder or vessel. Near the
bottom of the latter, a coil or series of pipes is arranged, into which steam can be
admitted for heating the lixivating liquid, while at the top there is a similar coil
or series of pipes, through which cold water circulates for condensing the vapours
generated by the steam. These heating and cooling surfaces may, however, be
formed in a different manner, and the materials, instead of being placed in a box,
may be spread out on a grate or a hurdle,
The apparatus is provided with sight-holes covered with glass, a tube for
inserting a thermometer, pressure-gauge, safely-valva, discharge-cock and other
requisite attachements. For distilling-purposes a condenser and also a dephlegmator
may be combined therewith. In some cases it is advantageous to connect the
apparatus with an air-pump in order to carry out the process in vacuum or alter-
nately in vacuum and under pressure, as for instance, when substances which
volatilize with difficulty are to be extracted and distilled. The dessication of the
materials treated may, under certain conditions, be accelerated by passing air
through the apparatus and thereby drawing off the vapours.
The described process is applied with advantage in the treatment of fibrous
plants, such as nettles, flax, hemp, &c., in order to disaggregate the fibres thereof.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said Carl Heckmann and Eugen Hausbrand in the Great Scal Patent Office
on the 16th October 1882.
CARL HECKMANN and EUGEN HAUSBRAND, both of Berlin, Prussia, " IMPROVED
METHOD OF AND APPARATUS FOR LIXIVATING VEGETABLE AND ANIMAL MATERIALS
AND OBTAINING EXTRACTS THEREFROM."
The object of our invention consists in the lixivation of vegetable and animal
materials by means of an improved method, either for the purpose of freeing such
materials from resinous, glutinous and other substances, or for obtaining therefrom
valuable extracts. Besides, the invention comprises a special apparatus for carrying
out the process.
The material to be treated and the lixivating liquid, for instance water, alkohol,
ether, sulphuret of carbon, &c., are put into a closed vessel in such a manner that
the former is supported or suspended above the latter. The liquid at the bottom
of the vessel is then heated in order that it may emit vapours, which, after having
passed through the material, are condensed by being brought in contact with
refrigerating-surfaces arranged in the upper part of the vessel. The liquid of con-
densation thus formed, drips down on and percolates the material, and thereby
dissolves the extractible substances softened by the vapours, and carries them
down into the bulk of the liquid. The lixivation having been completed, the liquid
containing the extracted substances is drawn off, while the residue of liquid in
the treated material is evaporated and recovered, when required, by condensation
in a special condenser.
The apparatus which we prefor to use for carrying out this process, is represented
on the annexed sheet of drawings. It consists in a horizontal cylinder A, or a
closed vessel of other shape, having at one end a large opening C, which may bo
hermetically closed by a cover, and through which a box E with perforated bottom,
containing the material to be treated, can be introduced. This box is supported in
a suitable manner about in the middle of the cylinder or vessel. According to the
drawing the supports consist in the bars D which serve at the same time as stays
for the plates B and B¹. Near the bottom of the vossel a coil or series of pipes S
is arranged, into which steam can be admitted for heating the lixivating liquid,
while at the top there is a similar coil or series of pipes S¹, through which cold
water circulates for condensing the vapours generated from the liquid. These
heating and cooling-surfaces may, however, be formed in a different manner, and
the material, instead of being placed in a box, may be spread out on a grate or a
hurdle. K and K' are sight-holes covered with glass, L is the discharge-cock, and
Ta tube for inserting a thermometer. Besides, the apparatus is provided with
two valves and a pressure-gauge attached to the respective branch-pipes H, T
and F. The pipe G, which may be closed by a cover, serves for pouring in the
liquid.
The box E with the material to be lixivated and the liquid having been intro-
duced into the apparatus, and all the openings closed, steam and cold water are
admitted. The liquid evaporated by its contact with the heated walls of the coil S,
passes in the state of vapour through the material in the box E, and having been
recondensed by the coil S¹ which is always kept cold, drips into the box, and
thence flows again to the bottom of the apparatus. By this circulation a complete
extraction of all the soluble substances contained in the material is brought about.
When the substances to be extracted, are volatile, such as essential oils (which
are extracted by alcohol) they may be separated from the non-volatile parts by a
distilling process carried out in the apparatus itself. In this case, the current of
cold water through the coil S' is stopped when the extraction is finished, and the
vapours are then conducted into a condenser put in communication with the
apparatus at T. Besides, the vapours may be passed through a dephlegmator in
order to cause the less volatile parts of the liquid to flow back into the apparatus.

page_text: The residue, which, in the manufacture of essential oils, generally consists of a
solution of resinous substances and of chloroform, is drawn off by the cock L.
Generally the lixivating or extracting operation will be carried out under n
certain pressure. If, however, this pressure, should become too high, it may be
reduced by causing a part of the vapours to pass off to the condenser by the valve
attached at T, or by accelerating the current of cold water in the coil S.
In case, substances which volatilizo with difficulty, are to be extracted, an air-
pump or other air-evacuating apparatus is combined with the condenser communi-
cating with the brauch-pipe T, and the process is performed in vacuum either from
the beginning or after the material in E is sufficiently softened, or the same is
carried out alternately in vacuum and under pressure. According to the special
requirements, this vacuum may bo partial or as complete as possible. While there
is a vacuum in the apparatus, the refrigerating coil S' will have no or but little
influence on the vapours.
The described process is applied with advantage in the treatment of fibrous
plants, such as nettles, flax, hemp, &c., in order to free them by means of alcohol
from resinous substances which cause their fibres to adhere together, and the
removal whereof is requisite before the latter can be separated from each other.
The extracting-liquid having been allowed to run off, the material is dried as
hereinbefore described. This drying-process may be accelerated by passing through
the apparatus air, which, in such case, enters by the branch-pipo H, and which,
after having become charged with vapour, is drawn off at T. When the air used
for this purpose is previously heated, the use of the heating coil S may bo dispensed
with.
Having thus described the nature and object of this invention, and the manner
in which it is performed or put in practico, we hereby claim as our invention.
1., The process of treating materials containing extractive substances by means
of evaporable liquids being dissolvents of the latter, and which are made to act on
the material at first in the state of vapour in order to produce a softening of the
extractive substances, and subsequently in condensed state for the purpose of
dissolving and extracting them, substantially as described.
2., The performance of the process claimed in claim No 1, in a vacuum which
may be either partial or as completo as possible, the evaporable dissolvents being
only employed intermittently in condensed state, as herein before specified.
3., An extracting-apparatus consisting of a closed vessel containing at the
bottom the heating-pipes or surfaces S, and at the top the refrigerating pipes or
surfacos S, and in which is placed a perforated receptacle E or a grate or hurdle
containing or carrying the material to be treated, substantially as and for the
purpose described.
4, The combination with the extracting apparatus consisting of a closed vessel
containing the heating-surface S and the refrigerating-surface S', and provided with
means for introducing the perforated receptacle E or a grate or hurdle, of a con-
densor, of a valvo inserted between the apparatus and the condeuser, and, if
preferred, of a dephlegmator, substantially as specified.
5., The combination with the extracting-apparatus and condensor, substantially
ns herein before set forth, of an air-evacuating apparatus as described.
In Witness whereof we, the said Carl Heckinann and Eugen Hausbrand,
have hereunto act our hands and seals this fifth day of October in the year
of our Lord One thousand eight hundred and eighty two.