Improvements relating to the Extraction from Grapes or Raisins of Various Substances, and to the Use or Application of the same for Colouring or other Purposes.
Year: 1884

page_text: Improvements relating to the Extraction from Grapes or Raisins
of Various Substances, and to the Use or Application of the
same for Colouring or other Purposes.
I EDWIN HENRY NEWBY, of 8 Bucklersbury, in the City of London, Merchant
do hereby declare the nature of my invention for "IMPROVEMENTS RELATING TO
"
THE EXTRACTION FROM GRAPES OR RAISINS OF VARIOUS SUBSTANCES AND TO THE
USE OR APPLICATION OF THE SAME FOR COLOURING OR OTHER PURPOSES
to be as
follows:-
My invention relates to the extraction of various substances from grapes or
raisins or from the residue in the manufacture of wine, spirits or alcohol therefrom,
and to the use or application of the said substances for colouring or other purposes.
After obtaining wine or spirits from grapes or raisins there remains a residue
from which the colouring matter and other substances which it contains cannot be
extracted by a simple lixiviation with hot or cold water.
Heretofore these colouring matters and other substances have not been utilized
in industry, and one object of my invention is to utilize them after having obtained
them by special processes.
°
The residue from grapes after they have been pressed contains about 50% of
water, I treat the said residue as hereinafter described that is to say :-I subject it
to a lixiviation with boiling water until I effect the complete extraction of the
matters which it still contains and which are capable of extraction. To this water
is added caustic soda or potash, the first alkalized bath shewing one degree (1°)
Baumè and the second bath four degrees (4°) Baumè. The succeeding baths are
not supplied with alkalies.
It is possible to vary the degrees of alkalization or even to alter the mode of
extraction of the matters contained in the aforesaid residue.
It is the custom when extracting the materials which are capable of extraction
from vegetable matters by lixiviation always to collect the strongest juices.
I filter these juices and add thereto hydrochloric acid (weakened to 10° Baumè) in
a sufficiently large quantity until all the precipitable substances are completely
precipitated

page_text: .
Any acid or acid salt, either vegetable or mineral, can be substituted for the
hydrochloric acid, but it is then necessary, previously to the operation which has
for its object to precipitate the colouring matter, to eliminate the lime which the
liquor contains. The liquid portion which remains above the precipitate contains,
besides a few extractive matters, a chloride of potash or of soda which can be
regenerated by again rendering it caustic, and I use this alkaline liquid again for
the succeeding operations.
I obtain a lacquer which is formed principally of the colouring matter of the
grapes; this lacquer is washed until the washing water no longer contains either
acid or chloride of calcium; the said washing water is very poor in alkali and can
be thrown away.
When the lacquer is well washed and drained I dilute it in an ammoniacal
solution composed of 10 kilograms of volatile alkali per 100 kilograms of distilled
water; this solution ought not to have a density of more than ten degrees (10°)
Baumè
The whole is placed in well closed vessels which should be only half filled and
placed in a stove heated to a temperature, as constant as possible, of about thirty
degrees (30°) centigrade and allowed to remain for at least ten days, or preferably
more.
After the liquor has thus remained in the stove, I filter it again, and then
evaporate it firstly in a distilling evaporator to collect the ammonia, and, when the
alkali is eliminated, I continue the evaporation in the open air.
This operation has for its object to drive out the ammonia from the liquor and
also to obtain an extract more or less concentrated, for example in the form of paste
or in a dry state.
The extraction of the colouring matters retained in the aforesaid residue can also
be effected by macerating the said residue, until the extraction is completed, in an
ammoniacal solution (volatile alkali) or even in pure ammonia and then evaporating
by distillation the whole of the residue and ammonia in order to collect the alkali.
Or, instead of operating by maceration, the extraction can be effected either by
infusion or by decoction, but, in such case, it is necessary to operate with closed
vessels provided with valves.
I afterwards add to the residue some distilled water to extract the colouring
matters therefrom either by lixiviation or otherwise, the liquor is filtered and then
'evaporated to the desired degree.
The alcohols and ethers can also be substituted for ammonia, the operation being
carried on as with volatile alkali, but the results obtained are not so good.
Moreover the colouring matters and other substances can be extracted from the
said residue by a lixiviation with boiling water to which is added caustic or
ordinary soda or potash exactly as in the first method above indicated, and then
eliminating the soda or potash by the treatment of the liquor by hydrofluosilicio
acid.
The elimination of the saline substances can also be effected by the use of
alcohol by the processes used in the manufacture of sugar.
There will still remain in the liquors a certain quantity of lime which it will be
necessary to eliminate. This elimination can be easily effected either by carbonic
acid gas or by ammoniacal phosphate of lime and also by any chemical agent
having the property of eliminating lime.
I may use other alkalies than those above named, either fixed or volatile, either
in their natural state or when rendered caustic, as well as any chemical agent or
any solvent having the property of extracting the extractive matters from the said
residue.
The colouring matters which I extract from the said residue may be employed
either for dyeing vegetable or mineral materials or for painting with water, size,
or oil colours, or for colouring liqueurs, wines, sweets, jellies, creams and articles of
confectionery. They can be advantageously used for dyeing cotton and woollen

page_text: fabrics. They possess, moreover, tanning properties and produce a colour which
does not fade and will not wash out. When made black the said colouring matters
can be used with advantage for painting horses harness or the leather hoods or
covers of carriages, as they make the leather dry and soft instead of sticky as it
becomes when blacking is used. They are moreover impermeable.
My invention is applicable not only to the extraction of the colouring matters
from the said residue but also to the extraction of colouring matters from grapes
or raisins from which neither wine nor alcohol has been extracted,
2004
HASELTINE, LAKE & Co.,
For the Applicant.

page_text: I, EDWIN HENRY NEWBY, of 8 Bucklersbury, in the City of London, Merchant,
do hereby declare the nature of my invention for "IMPROVEMENTS RELATING TO
"
THE EXTRACTION FROM GRAPES OR RAISINS OF VARIOUS SUBSTANCES, AND TO THE
USE OR APPLICATION OF THE SAME FOR COLOURING OR OTHER PURPOSES 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 the extraction of various substances from grapes or
raisins or from the residue in the manufacture of wine, spirits or alcohol there-
from, and to the use or application of the said substances for colouring or other
purposes.
After obtaining wine, spirits alcohol or other non-colouring matter from grapes
or raisins, there remains a residue from which the colouring matter and other sub-
stances which it contains cannot be extracted by a simple lixiviation with hot or
cold water. Heretofore these colouring matters and other substances have not been
utilized for industrial purposes, but have been destroyed, that is to say, converted
into a non-colouring product. The present invention is designed to provide for
the extraction and utilization of such substances.
The residue of grapes, after they have been pressed, contains about fifty per cent
(50%) of water. The said residue is, according to the present invention, treated
as hereinafter described, that is to say-It is subjected to lixiviation with boiling
water until the complete extraction of the matters which it still contains, and
- which are capable of extraction, is effected. To this water is added caustic soda or
potash, so that the first alkalized bath will shew one degree (1°) Baumé and the
second bath four degrees (4°) Baumé. The succeeding baths are not supplied with
alkalies.
The degrees of alkalization and the mode of extraction of the matters contained
in the aforesaid residue are varied according to circumstances.
It is the custom, when extracting the materials which are capable of extraction
from vegetable matters by lixiviation, to collect the strongest juices. These juices
obtained as above described are, according to the present invention filtered, and
hydrochloric acid (weakened to 10° Baume) is added thereto, in a sufficiently large
quantity, until all the precipitable substances are completely precipitated. Any
acid or acid salt, either vegetable or mineral, can be substituted for the hydrochloric
acid, but it is then necessary, previously to the operation which has for its object
the precipitation of the colouring matter, to eliminate the lime which the liquor
contains. The liquid portion which remains above the precipitate contains, more-
over, a few extractive matters, chloride of potash or of soda which can be

page_text: regenerated by again rendering it caustic, and I use this alkaline liquid again for
the succeeding operations.
I obtain a lac which is formed principally of the colouring matter of the grapes;
this lac is washed until the washing water no longer contains either acid or chloride
of calcium; the said washing water is very poor in alkali and can be thrown
away.
When the lac is well washed and drained, I dilute it in an ammoniacal solution
composed of ten (10) kilograms of volatile alkali per hundred (100) kilograms of
distilled water; this solution ought not to have a density of more than ten degrees
(10°) Baumé.
The whole is placed in well closed vessels, which should be only half filled, and
these vessels are placed in a stove heated to a temperature, as constant as possible,
of about thirty degrees (30°) Centigrade, and are allowed to remain therein for at
least ten days, but preferably for a longer period.
After the liquor has remained in the stove for the desired length of time, it is
again filtered and is then evaporated firstly in a distilling evaporator to collect the
ammonia, and, when the alkali is eliminated, the evaporation is continued in the
open air.
This operation has for its object to drive out the ammonia from the liquor, and
also to obtain an extract more or less concentrated, for example in the form of paste
or in a dry state.
"
The extraction of the colouring matter retained in the aforesaid residue can also.
be effected by macerating the said residue, until the extraction is completed, in an
ammoniacal solution (volatile alkali), or, if desired, in pure ammonia, and then
evaporating by distillation the whole of the residue and ammonia in order to collect
the alkali. Or, instead of effecting the extraction by maceration, it can be effected
either by infusion or by decoction, but, in such cases, it is necessary to use closed
vessels provided with valves.
Distilled water is afterwards added to the said residue to extract the colouring
matter therefrom, either by lixiviation or otherwise; the liquor is filtered and then
evaporated to the desired degree.
Alcohols and ethers can be substituted for ammonia, the operation being carried
on as with volatile alkali, but inferior results are thus obtained.
Moreover the colouring matter and other substances can be extracted from the
said residue by a lixiviation with boiling water, to which is added caustic or
ordinary soda or potash, exactly as in the first method above indicated, and the
subsequent elimination of the soda or potash by the treatment of the liquor by
bydrofluosilicic acid.
The elimination of the saline substances can, moreover, be effected by the use of
alcohol by the processes used in the manufacture of sugar.
There will still remain in the liquors a certain quantity of lime, which it will be
necessary to eliminate. This elimination can be easily effected either by carbonic
acid gas or by ammoniacal phosphate of lime or by any other chemical agent having
the property of eliminating lime.
I sometimes use other alkalies than those above named, either fixed or volatile,
and either in their natural state or after they have been rendered caustic; or I use
any chemical agent or solvent having the property of extracting the extractive
matters from the said residue.
The colouring matter which I extract from the said residue may be employed
either for dyeing vegetable or mineral substances or for painting with water, size,
or oil, or for colouring liqueurs, wines, sweets, jellies, creams and articles of
confectionery. It can also be advantageously used for dyeing cotton and woollen
fabrics. It possesses, moreover, tanning properties and produces a colour which
does not fade and will not wash out. When made black the said colouring matter
can be used with advantage for painting horses' harness or the leather hoods or
covers of carriages, as it renders the leather dry and soft instead of sticky, as is
the case when blacking is used. It is, moreover, water-proof.

page_text: The said invention is applicable not only to the extraction of the colouring
matter from the said residue but also to the extraction of colouring matter from
grapes or raisins from which neither wine nor alcohol has been extracted.
The extraction of the extractive matters from the grapes or raisins is sometimes
effected, either by maceration, infusion or decoction, by means of water to which
carbonate of soda or of potash has been added in the proportion of about five per
cent. of the weight of the residue of the grapes when dry.
The juices obtained are filtered and the colouring matter held in suspension in
the alkaline solution is precipitated by means of sulphuric, acetic or citric acid.
The lac, after being washed, is drained, and afterwards re-dissolved in water
alcoholized to thirty degrees (30°), more or less according to the difficulty with
which the lac is dissolved, whether it has been obtained by one acid or another.
The solution is distilled to collect the alcohol, and, when the distillation will no
longer yield alcohol, the operation is suspended, and the coloured water remaining
in the retort is filtered; the residue remaining on the filter is washed, and the
washing waters are added to the filtered solution to be concentrated to the desired
degree.
As above stated, I can employ other solvents than those above mentioned, such,
for example, as ethers, alcohols (sodaic or potassic), spirit of turpentine, wood
spirits, sulphide of carbon, alkalies and acids, alkaline or acid salts, glycerine, or
the wine itself. These solvents may be employed either for extracting the colouring
matter from the residue of the grapes or for re-dissolving the lac obtained by
precipitation.
Whatever solvents are employed for extracting the colouring matter from the
residue of the grapes, in order to utilize these solvents in the succeeding operations,
they can be regenerated by neutralizing them either by carbonate of lime, or lime
itself if they are alkaline solvents, or by distillation if they are alcohols, ethers or
spirits, and, in some cases, by distillation and afterwards by neutralization.
The filtration of the solutions is sometimes effected by the means employed in
the manufacture of sugar.
The reduction of the volume of the liquids can be effected either by. precipitation
or by evaporation at any temperature, in the open air or in a vacuum, or by
congelation.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what
I claim is
First. The improved product herein described extracted from grapes or raisins
and applicable for colouring or similar purposes.
Second. The improvements relating to processes of extracting from grapes or
raisins various substances to be used for colouring or other purposes, substantially
as above set forth.