IM- PROVEMENTS IN TREATING MADDER OR PREPARATIONS OF MADDER SO AS TO OBTAIN A COLOURING SUBSTANCE THEREFROM
Year: 1855

page_text: LETTERS PATENT to James Higgin, of the City of Manchester, in the
County of Lancaster, Manufacturing Chemist, for the Invention of "IM-
PROVEMENTS IN TREATING MADDER OR PREPARATIONS OF MADDER SO AS TO
OBTAIN A COLOURING SUBSTANCE THEREFROM."
Sealed the 4th January 1856, and dated the 12th September 1855.
PROVISIONAL SPECIFICATION left by the said James Higgin at the
Office of the Commissioners of Patents, with his Petition, on the 12th
September 1855.
I, JAMES HIGGIN, of the City of Manchester, in the County of Lancaster,
Manufacturing Chemist, do hereby declare the nature of the said Invention
for IMPROVEMENTS IN TREATING MADDER OR PREPARATIONS OF MADDER SO AS TO
OBTAIN A COLOURING SUBSTANCE THEREFROM" to be as follows:-
I place madder or preparations of it in a tube or other convenient vessel, and
connect therewith a pipe from a steam boiler, and also a pipe from a retort
which is generating ammonia, and pass the mingled vapours through the madder
till the effect wanted is produced. I then blow steam alone through the
madder till all the ammonia is expelled; the madder is then removed, and is
used as garancine. In some cases I treat the prepared madder with dilute
acid after removing from the steam, then wash well with water till neutral,
and dry. This is also used in same manner as garancine.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said James Higgin in the Great Seal Patent Office on the 12th
March 1856.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JAMES
HIGGIN, of the City of Manchester, in the County of Lancaster, Manufac-
turing Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Royal
Letters Patent, bearing date the Twelfth day of September, in the year of our
Lord One thousand eight hundred and fifty-five, in the nineteenth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said James Higgin, Her special licence that I, the said James Higgin,
my executors, administrators, and assigns, or such others as I, the said James
Higgin, 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 TREATING
MADDER OR PREPARATIONS OF MADDER SO AS TO OBTAIN A COLOURING SUBSTANCE
THEREFROM," upon the condition (amongst others) that I, the said James
Higgin, by an instrument in writing under my hand and seal, should par-
ticularly 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 Seal Patent Office within six calendar months next and immediately
after the date of the said Royal Letters Patent.
NOW KNOW YE, that I, the said James Higgin, 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 (that is to say):-
My improvements consist in subjecting madder, muujeet, sooranjee, or any
plant of same family, or any preparation of madder, or of any plant of same
family, with the exception of those preparations known in commerce by the
names of garancine and garanceaux, to the action of ammonia in the state of
gas, either alone or mixed with steam, whereby I find that a change takes
place in the coloring matter or matters contained therein, so that when the
resulting product is used in dyeing or printing, a purer color is produced.
And in order that my Invention may be more clearly understood, I will
proceed to describe the mode in which I carry out my Invention.
When madder well "aged" is operated upon, the washing or fermentation

page_text: now to be described is unnecessary, and may be omitted; but as a general rule
I prefer to submit the madder to a preliminary operation, which I will now
describe:-I take madder, or any plant of same family, previously reduced to a
powder, for the sake of convenience, and mix it with water, in proportion of
one pound of madder to every gallon of water, and allow a fermentation to take
place, either without addition or with the aid of any suitable ferment. In
general the action of water is sufficient to produce the change required; and
though the ordinary temperature is sufficient, yet to shorten the process I
prefer to raise the temperature to about 120 Fahrenheit. As soon as the
required change is effected, which will take place in a time varying with dif-
ferent sorts of madder, but which in any case should not be less than two hours,
I strain off the liquor, and press as much moisture out of the madder as I can,
and then expose it to the action of ammoniacal gas, or mixture of ammonia and
steam, for as long a time as may be judged necessary for the particular sample
under operation; and though various forms of apparatus may be devised, the
method which I prefer is to place the madder substance in a cylinder, pre-
ferably of wood, provided with a false bottom perforated, on which is placed
the madder.
pump
The cylinder is provided also with a cover fitting tight, through which passes
a pipe, either communicating with the atmosphere, or connected to one of the
vessels, hereafter to be described. Under the false bottom of the cylinder
ammoniacal gas, or a mixture of ammonia and steam, is made to arrive and pass
through the madder substance for as long a time as may be judged necessary,
about an hour being frequently sufficient. The ammonia may be generated in a
retort or any suitable manner, and the gas conveyed by a pipe underneath the
false bottom; or when ammonia and steam are used, the mixture of ammonia
and steam may be obtained by injecting liquid ammonia by means of a force
into an ordinary low-pressure boiler, when amnionia will be given off
along with the steam, and may be conveyed in a pipe, as before stated, or
ammonia and steam may be made to arrive simultaneously in different pipes
under the false bottom; and it is better towards the end to cease the passage
of ammonia, and pass steam alone until no more ammonia remains in the
madder, when it may be removed from the cylinder and cooled. It may either
be used in this state, or it may be washed with cold water and dried; or it may
be mixed with water, and a small quantity of an acid added, such as sulphuric,
muriatic, acetic, or any acid capable of combining with the earthy or alkaline
bases existing in the madder, and which are left in a great measure combined
with the coloring matter; and when an acid reaction is obtained on adding the
acid, it may be considered that the compounds of coloring matter with alkaline

page_text: earths are decomposed; and the mixture may then be left to steep, either at the
ordinary temperature or at a slightly heated temperature, for about an hour, or
until the object proposed seems fully completed, when the mixture may be
cooled and filtered, and washed with cold water until the washings come away
neutral, when the madder preparation may be removed and used in this state,
or pressed and dried for use.
Another modification of my Invention is to be carried out as follows:-
Madder, or any plant of same species, is treated with water or fermented, as
above described, for madder not sufficiently "aged;" and as soon as the fer-
mentation is sufficiently performed, I add to the mixture sufficient acid, such as
sulphuric, muriatic, acetic, or any acid capable of combining with alkaline or
earthy bases, until an acid reaction is manifest to test paper. I then let the
mixture stand, preferring to heat it to about 120 degrees Fahrenheit, until I
consider the compounds of coloring matter with bases are decomposed. I then,
after cooling, throw the substance on a filter, and wash until the washings come
away neutral.
I then, after pressing it, subject it to the action of ammonia or
ammoniacal steam, as described above, And it is necessary here to remark,
that the preparation here described is not garancine, which is made by the
action of strong acids in excess, say, from 10 to 30 per cent. of the weight of
the madder, at a temperature at or near 212, either by boiling with water or
by steaming the mixture; whereas the preparation now described requires only
just sufficient acid to combine with the alkaline or earthy bases present in most
madders, and a temperature higher than the atmosphere, though convenient, is
not essential.
I will next describe the method or methods I adopt when I wish to condense
the ammonia after passing through the madder substance. I connect the pipe
passing through the cover of the cylinder, before described, with a close vessel
of any convenient shape, such as a long chest or wide tube, and near the end,
in which is inserted the pipe leading from the ammoniating vessel, I insert a
pipe connected with any convenient source of muriatic acid or acetic acid in
such a manner, that the ammonia meeting with the acid may combine with it,
and the resulting salt of ammonia will fall to the bottom, and may from time
to time be removed; or when a solution of such salt in water is wanted, the
pipe leading from the ammoniating vessel may dip into a vessel containing an
acid which will take up or combine with the ammonia; or in case of steam and
ammonia being used, I pass the mixture on issuing from the cylinder into a
worm or suitable refrigerator surrounded by cold water, when liquid ammonia
will be recovered.
Having now fully described the various ways of carrying out my Invention,

page_text: I do not confine myself to the particular details herein set forth, as they may be
easily modified without departing from the spirit of my Invention; but I claim
as new,
First, the use of ammonia in a gaseous state, either alone or mixed with
steam, for producing a beneficial change in the dyeing properties of madder, or
plants of same family, or any preparations therefrom, with the exception of
garancine and garanceux.
Second, the condensation of ammonia after acting on madder, or preparations
of madder, or any plants of same family, by any of the means described.
In witness whereof, I, the said James Higgin, have hereunto set my
hand and seal, this Tenth day of March, One thousand eight hundred
and fifty-six.
JAMES HIGGIN. (L.S.)
Signed, sealed, and delivered by the within-named
James Higgin, in the presence of
E. J. HUGHES, Patent Agent,
Manchester.