IMPROVEMENTS IN EXTRACTING THE COLORING MATTER OF MADDER ROOT FROM THE LIGNEOUS MATTER OF THE PLANT
Year: 1868

page_text: LETTERS PATENT to George Tomlinson Bousfield, of Loughborough
Park, Brixton, in the County of Surrey, for the Invention of
"IMPROVEMENTS IN EXTRACTING THE COLORING MATTER OF MADDER ROOT FROM
THE LIGNEOUS MATTER OF THE PLANT."--A communication from abroad
by Alfred Paraf, residing at New York, United States of America.
Sealed the 22nd June 1869, and dated the 29th December 1868.
PROVISIONAL SPECIFICATION left by the said George Tomlinson
Bousfield at the Office of the Commissioners of Patents, with his
Petition, on the 29th December 1868.
I, GEORGE TOMLINSON BOUSFIELD, of Loughborough Park, Brixton,
in the County of Surrey, do hereby declare the nature of the said In-
vention for "IMPROVEMENTS IN EXTRACTING THE COLORING MATTER OF MADDER
ROOT FROM THE LIGNEOUS MATTER OF THE PLANT," to be as follows:-
The Invention consists, first, of the process of extracting the coloring
matter of the madder root by treating it with water at a temperature of
about 305 degrees, and then precipitating the coloring matter from the
water while out of contact with the madder root.

page_text: The Invention consists further of the process of extracting the sugary
and coloring matters from the madder root by dissolving the sugary
matter in water at a moderate temperature, and extracting the coloring
matter by treatment with water at a high temperature (say about 305°
of Fahrenheit), and precipitating the coloring matter from the resulting
liquid out of contact with the ligneous matter of the root.
The Invention consists further of the process of extracting the resinous
and coloring matters from madder root by treating the material with
acid to remove the resinous matters, then treating it with water at a
high temperature (say 305° of Fahrenheit or thereabouts), and pre-
cipitating the coloring matter from the resulting liquid out of contact with
the ligneous matter of the root.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said George Tomlinson Bousfield in the Great Scal
Patent Office on the 23rd June 1869.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, GEORGE
TOMLINSON BOUSFIELD, of Loughborough Park, Brixton, in the County
of Surrey, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-ninth day of December, in the
year of our Lord One thousand eight hundred and sixty-eight, in the
thirty-second year of Her reign, did, for Herself, Her heirs and
successors, give and grant unto me, the said George Tomlinson Bousfield,
Her special licence that I, the said George Tomlinson Bousfield, my
executors, administrators, and assigns, or such others as I, the said
George Tomlinson Bousfield, 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 THE COLORING MATTER
OF MADDER ROOT FROM THE LIGNEOUS MATTER OF THE PLANT," & communica
tion to me from abroad by Alfred Paraf, a person resident at New York,
United States of America, upon the condition (amongst others), that I, the
said George Tomlinson Bousficld, my executors or administrators, by an

page_text: 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 Scal Patent Office within six.
calendar months next and immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said George Tomlinson Bousfield, do
hereby declare the nature of the said Invention, and in what manner
the same is to be performed, to be particularly described and ascertained
in and by the following statement thereof, that is to say :-
The coloring matter of madder has hitherto been found to be prac-
tically insoluble in water; the Invention which constitutes the subject
matter of this Patent is based upon the discovery that when the madder
root is subjected to a temperature of about 305° of Fahrenheit's thermo-
meter the coloring matter becomes soluble in pure water, and can be
removed from the woody fibre by successive washings with water of about
that temperature, and that the coloring matter carried off by the water
may be precipitated in a floculent state from the water, the precipitation
being effected by cooling down the solution from the said temperature.
The Invention consists, first, of the process of extracting the coloring
matter of the madder root by treating it with water at a temperature of
about 305 degrees, and then precipitating the coloring matter. from the
water while out of contact with the madder root.
The Invention consists further of the process of extracting tlie sugary
and coloring matters from the madder root by dissolving the sugary
matter in water at a moderate temperature and extracting the coloring
matter by treatment with water at a high temperature (say about 305° of
Fahrenheit, and precipitating the coloring matter from the resulting
liquid out of contact with the ligeneous matter of the root..
The Invention consists further of the process of extracting the resinous:
and coloring matters from madder root by treating the material with
acid to remove the resinous matters, then treating it with water at a high
temperature (say 305° of Fahrenheit or thereabouts) and precipitating
the coloring matter from the resulting liquid out of contact with the
ligneous matter of the root..
The Invention may be practised in several ways. That which is
deemed the best is effected by means of an apparatus such as is repre-
?

page_text: sented partly in section in the accompanying Drawing, but the Invention
is not restricted to any peculiar form or construction of apparatus. The
said apparatus consists substantially of a strong vessel or digester A,
fitted with trunnions b, b, on which it can be turned, and with perforated
pipes c, c', by which steam can be injected into its interior; of a second
vessel D, by means of which hot water under pressure may be introduced
into the first vessel A; and of the steam pipes and stop cocks by which
high-pressure steam from a suitable high-pressure boiler may be supplied
to the water vessel D and to the digester A. The digesting vessel A has
a domed head f, which is separated from the cylindrical portion of the
vessel by a diaphragm of wire cloth m.
The said Invention may be carried into effect as follows:-The dry
ground madder root is prepared for the extraction of the coloring matter
by washing it with water to free it from the sugary matter contained in
the root. To this end the root is steeped in about fifteen times its weight
of lukewarm water for about half an hour. The water is then removed
from the root by straining or otherwise, and the root is subjected to a
second steeping performed in the same manner as the first. The madder
root is freed from the second water by straining or otherwise. The water
employed in these oporations holds a large quantity of sugary matter in
solution, amounting generally to about forty per cent. of the weight of
the dry madder root, and the solution may be used for the manufacture
of alcohol or other purposes to which it is applicable.
The moist madder root is further prepared for the extracting process
by treating it with dilute sulphuric acid. For this purpose concentrated
commercial sulphuric acid is diluted with sufficient water to reduce its
specific gravity to 25° of Beaumé. The quantity of concentrated acid
of 66° Beaumé required for the purpose is about one quarter of the
original weight of the dry madder root. The moist madder root is
boiled in the dilute acid for two hours, after which the acid liquor is
drained off, the madder root is thoroughly washed to free it from the acid
liquor, and the surplus water is removed by pressure or by the action of
a centrifugal machine so as to leave the material in a damp condition.
The material in this condition is well prepared for the extracting process
and is substantially the same article as the garancine of commerce,
The extracting process is conducted by preference as follows:-A
quantity of the damp garancine is mixed with about four times its weight
of distilled water, and the mixture is introduced into the digesting

page_text: vessel A, which should be filled to the extent of two-thirds or three-
quarters its capacity; at the same time the water vessel D is filled with
distilled water, which is heated by letting into it the steam from the
steam boiler. Steam from the steam boiler at a pressure of from 50 to
60 lbs. per square inch above the atmospheric pressure is let into the
digester through the lower perforated pipe c', and the stop-cock g is left
open until the air in the vessel is blown out. The stop-cock is then closed,
and the temperature permitted to rise to the temperature of the steam,
say, from 302° to 315° Fahrenheit. As soon as this temperature is reached
(which may be ascertained by means of a thermometer, the bulb of
which is secured in the digester, or by means of a pressure gauge con-
nected with the digester,) the digester is reversed upon its trunnions so
as to place the stop-cock g at the lowest position, and this stop-cock is
opened to permit the liquid to escape. As the liquid escapes about an
equal quantity of water at the same temperature is permitted to enter
the digester from the hot-water vessel D along with steam through the
perforated pipe c, so that the material in the digester is uniformly or
thereabouts mixed with the liquid. The first liquor which escapes from
the digester is of a yellow color, and is charged with pectic acid. This
liquor may be permitted to run to waste. As the operation progresses
the liquor escaping at the stop-cock becomes charged with the coloring
matter of the garancine, and must be saved in a suitable tank. The
supply of hot water at the temperature of the steam or thereabouts and
the supply of steam to the digester are kept up as the liquor is drawn
off from the digester until the garancine is exhausted of colouring matter.
When this is effected the liquor running from the digester does not
precipitate colouring matter upon cooling nor upon the addition of a weak
acid. The supply of steam and water are then stopped, the digester is
blown off, the spent material is removed, and the apparatus is recharged.
In practice about two hours time is required for an operation, and a
quantity of water equal to about five and a half times the original
weight of the dry madder root are required to remove the coloring
matter. The temperature in the digester during the operation is main-
tained by keeping the steam at the requisite pressure in the steam boiler,
and the material is prevented from clogging upon the filtering diaphragm
by the constant agitation produced by the admission of steam through
the perforated pipe c, which is immersed in the mixture in the digester.
The liquor charged with the coloring matter is permitted to cool in a
suitable vat, whereby the greater part of the coloring matter is pre-

page_text: cipitated in a floculent state. The liquor is subsequently filtered to
separate all the coloring matter. The coloring matter is thoroughly
washed with water and drained, and is then in a suitable condition for
printing fabrics. The colouring matter of madder obtained by this process
is denominated tinctorine. In practice it has been found expedient to
make the digester of iron lined with sheet lead, so that the coloring
matter may not be soiled by the action of acid upon iron. In establish-
ments where power can be furnished it is expedient also to use a force
pump to supply water to the digester in place of the water vessel.
Another mode in which the Invention may be practised is as follows,
vizt. To add to the distilled water a sufficient quantity of some soluble
salt which will raise the boiling point to 302° Fahrenheit or more, and
to boil the garancine in the solution in an open vessel, the liquor being
progressively drawn off through a strainer, and fresh quantities of the
solution being introduced into the vessel until the coloring matter is
extracted. A salt which may be used for this purpose is chloride of
zinc.
But this mode of practising the Invention is not deemed as advan-
tageous as that first described, because it is difficult to free the pre-
cipitated tinctorine of the zinc or its salts.
The treatment of the madder root by washing and by sulphuric acid
is advantageous, as the effect is to remove the sugary, gummy, and
resinous matters from the material before tho coloring matter is
extracted; also to partially char the cellular tissue of the plant, and
thus facilitate the extraction of the coloring matter, but the coloring
matter may be extracted directly from the ground madder root without
such preparation by introducing it mixed with water into the digester,
and treating it with water at a high temperature, and a substantial
portion of the Invention may thus be used without the residue.
What is claimed as the Invention to be secured by Letters Patent is,
the process of extracting the coloring matter of madder root by treating
the material with water at a high temperature, and then precipitating
the coloring matter from the liquid, substantially as before described.
Also the compound process of separating the sugary and coloring
matters from inadder root, by first washing it with water to remove the
sugary matter, then treating the washed inadder root with water at a

page_text: high temperature, and precipitating the coloring matter from the resulting
liquid, substantially as before described.
Also the compound process of separating the resinous and coloring
matters from madder root by heating the madder root in the acid liquor
to remove the resinous matter, then treating the material with water at
a high temperature, and precipitating the coloring matter from the
resulting liquid, substantially as before set forth.
In witness whereof, I, the said George Tomlinson Bousfield, have
hereunto set my hand and seal, this Twenty-first day of June, in
the year of our Lord One thousand eight hundred and sixty-
ninc.
GEO. T. BOUSFIELD. (L.s.)