A NEW OR IMPROVED COLOURING MATTER AND PROCESS FOR OBTAINING THE SAME
Year: 1884

page_text: I WILLIAM PHILLIPS THOMPSON of the Liverpool and London Agency for
Foreign Patent Solicitors, 6 Lord Street, Liverpool in the county of Lancaster
Civil Engineer do hereby declare the nature of the said invention for "A NEW
OR IMPROVED COLOURING MATTER AND PROCESS FOR OBTAINING THE SAME," 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 manufacture of coloring matter from the so-called
red-colored tannic woods and plants which possess the characteristics of the class
of coloring matters known as "Catechus" and because the woods or plants treated
for the production of these coloring matters is principally found in America, the
products obtained are designated "American Catechus." The invention however
is not confined to coloring matters produced from American woods or plants solely.
The following is a full, clear and exact description of the process.
The invention relates to the treatment of such plants and woods as contain
coloring matter in sufficient quantity to be practically useful in the arts for dyeing
woven fabrics, furs, skins, wood or other articles to which it is desired to give an
artificial color. These woods or plants contain also in addition to the coloring
Inatter the substance known as " tannin."
The woods and plants containing coloring matter combined with "tannin" may
be divided into tannic woods and plants colored red, and tannic woods and plants
colored yellow. The process as set forth in this specification relates to the
treatment of the tannic plants colored red.
When a wood or plant contains tannin" or in other words tannic or gallic
substances and little or no coloring matter; either red or yellow it is usually easy
to obtain therefrom all the extractive substances by simply treating it with
boiling water. But it is different when the wood or plant contains at the same
time a large proportion of tannin and also a large proportion of coloring matter.
In such case pure water even at a boiling temperature will dissolve only a portion.
of the "tannin" much of it remaining in the wood, and with it most and
sometimes all the coloring matter.

page_text: In order to obtain the coloring matter and the "tannin " from these woods and
plants that is those containing tannin" and coloring matter in large quantities,
various processes have heretofore been employed but in them all strong applications
of alkali or alkaline salts usually in solution bave been employed to act as solvents
on the coloring matter and the "tannin."
Now the use of alkali or alkaline salts seriously deteriorates the dyeing quality
of the extracts, especially those obtained from red colored tannic plants because
the coloring substance contained in them being less soluble than that of the
yellow colored tannic plants their manipulation requires the use of stronger
preparations of alkali or alkaline salts. And this deterioration of the dyeing
quality of the extracts cannot be wholly rectified; the degree of deterioration,
however varies somewhat with different plants.
This invention which as stated is especially applicable to the treatment of red
tannic woods and plants, consists in a process by which all the extractive coloring
substances contained in such woods or plants may be secured without the
deterioration stated incident to the use of alkalies or alkaline salts as heretofore
used.
It is a well known fact that the elements or constituent parts of natural tannin,
that is, tannin as it is found in plants in its normal state, do not separate or
decompose under the influence of fermentation, but fermentation, on the contrary,
does singularly affect the coloring matter combined with the tannin; under certain
conditions decomposing it rendering it worthless, and under different conditions,
giving it unexpected strength or vitality and stability. It is, therefore possible by
proper manipulation and treatment and without danger of altering the tannic
condition of the resulting extract or its coloring properties, to submit the plant to a
" and
process of fermentation which accomplishes the extraction of the "tannin
coloring matters contained in the plant, and which process being properly
conducted, will not only not injure the coloring substance, but, on the contrary
will increase its strength, vitality and stability. Such a process has been discovered
and forms a part of this invention.
After the wood or
It is also discovered that oxidation of the woods or plants by the use of certain
acids when diluted may be used as a substitute for the fermentation process and
that such oxidation is a more rapid method of practising the process, the effect both
of the fermentation and the acid oxidation as they are used in the process, being
to effect oxidation of the woods or plants which makes the coloring matters and
the tannin substances soluble in water. As stated the acids if very strong, should
be diluted so as not to destroy the coloring matter by altering or destroying the
ligneous portions in which the coloring matter is contained.
plant has been submitted to the fermentation or the oxidation by the use of the
diluted acids as the case may be, the first extract is obtained. The residues then
remaining may be further treated with alkaline bodies as heretofore, if desired, but
since such former use of alkaline substances is detrimental to the resulting extract
it is preferable to continue the process by treating the residues with a specially
prepared compound, consisting of an oily or fatty substance or substance of the
nature of carburretted hydrogen in combination with an alkaline substance
whereby saponification is effected.
The mode of carrying out and practising the process is as follows; beginning at
the commencement.
In suitable vats, barrels or other appropriate receptacles, adapted in any desired
manner to heat their contents is placed the woods or plants which it is desired to
treat having first crushed or bruised them or reduced them to a powder; shavings
or other finely divided parts. When the wood or plant is reduced to powder it has
preferably mixed with it finely powdered or comminuted charcoal, punice stone or
other like body capable by "catalytical" action of favoring the operation of the
leaven which is used to effect the fermentation, the proportion being about ten
pounds of charcoal or five pounds of pumice to one hundred pounds of the wood or
plant, but these proportions are not at all arbitrary but will be found to vary

page_text: according to the fermenting force that may be required, this will be determined by
the nature of the wood or plant being treated. The leaven used may be ordinary
brewers yeast or any other leaven capable of inducing or aiding fermentation.
To the mass thus obtained add enough tepid water to forin a pulpy mixture of
about the consistency of a stiff mush. If the wood or plant is bruised or crushed
or reduced to fragments simply and not to a powder, then add enough tepid water
to thoroughly soak the same and in such case do not use the charcoal, pumice stone
or similar substance. The harder or more dense the wood or plant the finer it
should be divided.
After the water has thoroughly saturated the pulp or the bruised, crushed or
finely divided fragments, as the case may be add the leaven, or the acid diluted
in water, as the case may be, to effect the oxidation. The proportion of leaven
is about one half pound, taking brewers yeast as the example, to one hundred
pounds of wood or plant and the proportion of the diluted acid is about five
hundred grammes to one hundred pounds of wood or plant, the acid being diluted
or dissolved in water to make a reduced solution, taking as the example, nitric
acid. The acids which it is preferable to use are chlorohydric and nitric acids,
because they are more easily eliminated from the resulting extract than most, if
not all the other acids, and this elimination of the acids from the extract is
desirable so that it may be as nearly neutral as possible. This elimination of
the acids is preferably effected by evaporation under the action of heat.
acids may however be used as hereinafter stated. After the admixture of the
leaven, or the acid as the case may be, with the wood or plant and the charcoal
or pumice stone when used, allow the mass to stand for about twenty four
(24) hours, for the purpose of effectually inducing the fermentation, or the
oxidation by the acids. At the end of that time add more water and raise the
temperature of the mass by steam or in any other desired manner to about 120 to
150 degrees Fahrenheit and stir the mass say every hour, repeat the stirring at
intervals of about an hour and maintain at about 120 or 150 Fahrenheit for a
period of about two days thus securing perfect oxidation.
Other
This is the practice whether the fermentation by the use of leaven is used or the
oxidation by the use of acids, with the difference only that the fermentation
process requires a longer time.
"
As a general rule the process when acid is employed requires about three days
and when leaven is used from a week to ten days. The proper time to discontinue
the process will be readily ascertained by the appearance of the scum on the top of
the mass which will have a deep orange color. When this takes place the
temperature of the mass is raised. until it reaches the boiling point and maintained
there for about an hour. The resulting liquor is then drawn off in any desired
manner. This liquor will be heavily charged with " tannin and with coloring
matter, and upon evaporation as usual results in the first product or extract, which
is as stated a strong decoction of the "tannin" and the coloring matter. It is
noticeable that when the liquor is first drawn off it appears to contain but little
coloring matter. The contrary, however is the fact. It rapidly grows darker
during evaporation, which is effected by heat. The liquor seems further to oxidize
by the action of the heat.
In addition to the acids named the following may be used, depending upon the
nature of the plant treated, tartaric, oxalic, malic, sulphuric, or there may even be
used oxygenated water, chlorine, certain metallic salts, chlorates of potash of
ammonia, of mercury, various nitrates, bi-oxide of barium, arsenous and arsenic
acids, antimonus and antimonic acids, staunic and chromic acids, peroxides of lead,
of manganese either alone or in conjunction with sulphuric acid, chromates and
manganates of potash and in general all substances capable of producing oxidation.
And it has been also found that for producing the oxidation certain alkalies which
by inhydration produce oxygen such as quicklime, caryta and strontian may be
used. But these bodies are used solely for the purpose of producing oxygen and in
no sense as alkalies, they being, when used for the purpose stated, insoluble in

page_text: '
water, and, therefore, have no effect on the extract. This process relates to the
treatment of all the red colored tinnic woods and plants such as hemlock, beech,
cedar, mahogany, elm, hazel or filbert, dividivi, quebracco, red cinchona, tamarind,
willow bark, brier root, the various coniferous plants, and in fact, all woods and
plants possessing the qualities and characteristics of those mentioned.
The first extracts obtained as above described compare very favorably with the
favorite brands of "Catechus" and more than the "Catechus" and more than any
other similar extract they incline to reddish brown under the influence of
michromates and manganates of potash or of alkaline sulphures, and to purple
gray under the influence of ferric salts, therefore,. the coloring matters thus
produced possess qualities and characteristics not found in any others known to
the said Michael Edmund Savigny and are therefore new articles of manufacture in
this art. And their color is of the kind known as "fast" color, which can be
destroyed only by the most violent agencies. When used to charge silk they do
not alter its touch as extracts having an alkaline basis do. They do not harden
cotton fabrics and they color wood without "packing," as it is called, that is
giving it a felty nature.
After the first product or extract above mentioned has been obtained, the
residues left in the bottom of the vat may, as already stated, be further treated
with alkaline bodies in the same manner as they have been heretofore treated for
the purpose of obtaining an additional quantity of extract from the residues. The
extract thus obtained, however, is of an inferior grade .or quality because it will
inevitably be effected more or less by the alkali when used as heretofore used.
But it has been discovered that the substances composing the residues with
which coloring matter is united and the coloring matter itself are as soluble in fatty
bodies and in the hydrogenated carbonets, as a class, as in the alkalies or alkaline
bodies heretofore used; instead therefore of using the alkalies-following further
the improved process, the proceeding is as follows:-first pour upon the residues
when still wet, a quantity of any animal or vegetable oil or equivalent fatty
substance preferably using only such substances as are soluble in water such as
glycerine or substances casily saponified by a small percentage of alkali. The
proportion of such fatty body to the residues will be determined by the quantity
of coloring matter which remains in the residue. For instance assuming that
one-third of the coloring matter remains in the residues, then use about a pound
of oil to one hundred pounds of residues,; from this the proportion of oil may be
estimated, the more color remaining the more oil should be used. Then add water,
to about one hundred pounds of the residue about one hundred and fifty quarts of
water, and bring the mass to a boiling point, meantime stirring it in order to
maintain the mixture as nearly as posible in a state of emulsion. When the
liquor is sufficiently colored gradually saturate the oil or the fatty substance by means
of a measured (titrée) alkaline liquor, using no more of it than just sufficient to
saponify the oil or tatty body upon which the decoction will become limpid. Then
continue the boiling until all the coloring matter is extracted which will be in the
neighborhood of one hour.
The liquor is then drawn off and evaporated as usual to obtain the desired
extract. This extract will be found much more valuable than that obtained by the
use of alkalies as herein before stated, because although a small percentage of alkali
has been used, still it is used not for the purpose of dissolving the coloring matter
but to saponify the oily or fatty matter and has no effect upon the coloring matter.
Instead of using the oily or tatty substance and the alkaline solution, thus effecting
saponification there can be used as a substitute therefor producing the same results,
a solution of ordinary soap either potash or soda. The percentage of alkali being
so small in it and it also being saponified that it does not act detrimentally on the
resulting extract.
It has also been found practical and advantageous when desiring to produce
cheaply a low grade of extract to combine the two operations, that is the fermenta-
tion or the oxidation with acids, as the case may be, and the treatment with soap

page_text: in one operation and at the same time. To do this first proceed with the oxidation
either by fermentation or the use of acids as above stated down to the boiling at
the end of the first operation, and then gradually add the soap compound preferably
in solution and then continue the boiling for a half hour or so, or in other words,
until all the coloring matter has been extracted. A few hours settling and one or
at most two filterings through filtering cloth will clarify the resulting extract.
All the extracts obtained by the practice of the above processes obey the same
reactives, produce the same shades, or at least shades of the same character with
the same chemical agents, these agents being used as now well understood by those
skilled in this art. That is to say, by means of chromates and manganates of
potash, sulphurs, alkalines and other agents which may be used for the same
purpose, these extracts produce all the reddish browns which may be required by
the dyer. In the same manner by using ferric salts the purplish grays may be
produced.
These extracts produce with zinc salts and salts of manganese pale grays; this
seems to be owing however to the fact that these salts always contain a greater or
less quantity of iron.
Finally, all the red tannic woods or plants containing colouring matter may be
treated by this process either separately or several together in order to obtain such
reddish browns as may be desired, all of them being capable of production by this
process. Also the extracts obtained by the red tannic plants can be combined with
the extracts from the yellow tannic plants or with other coloring matters to produce
such color or shade of color as may be desired.
It is to be distinctly understood that the fermentation, and the oxidation by the
use of the acids, are in this process the equivalent for each other because by both
of them, the wood or plant is oxidized thereby rendering the coloring matter
soluble and that when I use the word " oxidating in the claims I intend to cover
both the fermentation and the oxidation by use of acids.
"
I do not limit myself to the specific proportions mentioned because they can be
departed from depending on the character of the wood or plant being treated.
Having now described the invention as communicated to me and in what manner
the same is to be performed, I declare that what I claim in the art of extracting
coloring matter from red tannic woods or plants is :-
First: The described process consisting in first crushing bruising or finely
dividing the wood or plant and then "oxidating" the same under the influence
of heat substantially as described.
Second. The described process consisting in first crushing bruising or finely
dividing the wood or plant, then "oxidating" the same under the influence of
heat, then drawing off the first extract and then treating the residues with a soap
solution or with a fatty body saponified with an alkaline solution substantially as
set forth.
Third: The described process consisting in first crushing bruising or finely
dividing the wood or plant, then " oxidating" the same under the influence of
heat and then admixing with the mass before the withdrawal of the first extract
a soap solution or fatty body saponified with an alkaline solution substantially as
set forth.
Fourth The described process of treating the residues from which the first
extract has been drawn off consisting in mixing therewith a soap solution or a
fatty boly saponified with an alkaline solution substantially as set forth.
Fifth As a new article of manufacture the extract resulting from the described
process of treating red tannic woods or plants which process consists in "oxidating"
the same under the influence of heat, substantially as set forth, to wit, either by a
* process of fermentation or by oxidation by means of acids.
Sixth: As a new article of manufacture the extract resulting from the described
process of treating the residues of red tannic woods or plants from which part of
the coloring matter has been removed, consisting in treating the same with a soap

page_text: solution or with a fatty body saponified by the use of an alkaline solution,
substantially as set forth.
Seventh: As a new article of manufacture the extract resulting from the
described process of "oxidating" red tannic woods or plants consisting in first
subjecting the same to a process of fermentation or of oxidation by the use of
acids and after such process has been completed and before drawing off any extract
treating the ina-s with a soap solution substantially as set forth.