IMPROVEMENTS IN THE PREPARATION OF COLORING MATTERS FOR DYEING, STAINING, OR PRINTING FABRICS, STUFFS, AND YARNS OF COTTON, SILK, OR WOOL, OR SUCH LIKE SUBSTANCES
Year: 1861

page_text: LETTERS PATENT to Michael John Stark, of the City of Norwich,
Chemist, Merchant and Dyer, for the Invention of "IMPROVEMENTS IN
THE PREPARATION OF COLORING MATTERS FOR DYEING, STAINING, OR PRINTING
FABRICS, STUFFS, AND YARNS OF COTTON, SILK, OR WOOL, OR SUCH LIKE
SUBSTANCES."
Sealed the 4th June 1861, and dated the 8th February 1861.
PROVISIONAL SPECIFICATION left by the said Michael John Stark
at the Office of the Commissioners of Patents, with his Petition, on
the 8th February 1861.
I, MICHAEL JOHN STARK, of the City of Norwich, Chemist, Merchant, and
Dyer, do hereby declare the nature of the said Invention for "IMPROVEMENTS
IN THE PREPARATION OF COLORING MATTERS FOR DYEING, STAINING, OR PRINTING
FABRICS, STUPPS, AND YARNS OF COTTON, SILK, OR WOOL, OR BUCH LIKE SUBSTANCES,"
to be as follows:-
The said Invention consists in producing coloring matters by the action of
cyanides, ferricyanides, or ferrocyanides, or other combinations containing
cyanogen of different bases from aniline, toluidine, cumidine, or other analogous
substances, in the manner following:-I take aniline or a solution of a salt
of analine, or of such like substances, and also a solution of the ferricyanide of
potassium, or a solution of other cyanides. I then mix these two solutions
together and boil them for some time, and then allow them to cool, when I
separate by decantation or filtration a copious grayish-blue precipitate, which

page_text: when boiled with a strong solution of an organic or mineral acid produces
blue, violet, lilac, purple, or red shades of color according to the proportions in
which these substances above mentioned are used.
The dyes produced in this manner may be used with or without the usual
mordants, for cotton, silk, or wool, or such like substances.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Michael John Stark, in the Great Seal Patent Office on the
6th June 1861.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, MICHAEL
JOHN STARK, of the City of Norwich, Chemist, Merchant and Dyer, send
greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Eighth day of February, in the year of our Lord
One thousand eight hundred and sixty-one, in the twenty-fourth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me, the said
Michael John Stark, Her special licence that I, the said Michael John
Stark, my executors, administrators, and assigns, or such others as I, the said
Michael John Stark, 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
THE PREPARATIONS OF COLORING MATTERS FOR DYEING, STAINING, OR PRINTING
FABRICS, STUFFS, AND YARNS OF COTTON, SILK, OR WOOL, OR SUCH LIKE SUB-
STANCES," upon the condition (amongst others) that I, the said Michael John
Stark, my executors or administrators, by an 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
Seal Patent Office within a calcndar months next and immediat ly after
the date of the said Letters Patent.
NOW KNOW YE, that I, the said Michael John Stark, do hereby declare
the nature of my said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, that is to say :-
My said Invention consists in a mode of obtaining coloring matter from

page_text: aniline, xylidine, cumidine, toluidine, or any other analogous substance, as
follows: I take a salt of either of the above substances, or a mixture of the
salts of two or more of the above substances, or what is more simple, I take
either of the above substances themselves, or a mixture of the same, but I prefer
using aniline, it being at present the more easily obtainable of all these sub-
stances; and I add to the same an equal weight of hydrochloric, nitric,
sulphuric, acetic, tartaric, or other acid that will unite with it, or I use a
mixture of these acids; but I prefer using hydrochloric acid, or a mixture of
bydrochloric and nitric acid, both of the ordinary strength, and generally in
equal proportions. When I have well mixed these substances, namely, the
aniline and acid or acids together, I dilute this solution generally with about
an equal bulk of water, agitating it at the same time. I then mix it with a
ferricyanide or a ferrocyanide of any base, or a mixture of these cyanides, or
any other combination containing cyanogen; but I prefer using the ferri-
cyanide of potassium, and proceeding in the following manner :-I take about
an equal weight of ferricyanide of potassium to aniline, and dissolve it in about
ten times its weight of water, and to this solution I add the acid solution of
aniline, and then gradually heat up this mixture to boiling, and boil for two,
three, or more hours; the time of boiling depending somewhat upon the bulk
of the materials used and the proportions in which the materials may have
been mixed. When the whole has sufficiently boiled it is allowed to cool, and
I separate from it by subsidence and decantation, or by filtration, a copious
gray-blue precipitate, which I wash with one, two, or more waters. This
precipitate I prefer, while it is moist, to boil for about one or more hours with
a strong solution of an acid. Any acid will separate brilliant coloring matters,
but I prefer a solution of tartaric acid, and of about the strength of one of
acid to two of water, as it appears to me to give the best and most brilliant
colours. I filter the acid liquid having the color in solution, and I repeat
this treatment with acid upon the insoluble matter, if necessary.
This acid solution of coloring matter may be used for dyeing and other
purposes, but I generally treat it as follows:-When cold it is neutralized or
made slightly alkaline by an alkali or alkaline earth, but I prefer ammonia;
this precipitates the coloring matter from it, which I may wash by subsidenco
and decantation, or I may collect it on a filter at once and drain it. After
which I dissolve it, in preference, on account of its cheapness, in methylated
spirit, thus producing a dye of a very permanent character, and of a brilliant
purple colour, which I call, name, or style tyraline.
Although by using the substances in the proportions which I have given
above I produce the above purple dye, which as I have said before I have

page_text: named tyraline, still by altering the proportions in which these substances are
used above, the color will bo produced, but of a different shade, so that by
altering the proportions of aniline and acid to ferricyanide, in this way an
infinite variety of shades may be produced.
I sometimes add to the liquid decanted or filtered from the gray-blue pre-
cipitate obtained as stated above, on boiling the acid solution of aniline and
the ferricyanide of potassium, an additional quantity of ferricyanide, say, about
one-sixth of the original quantity used, and boil for some time, and in this way,
if the aniline has not been all decomposed in the first operation, I get a pre-
cipitate containing coloring matter, which I treat similarly to the original
gray-blue precipitate..
The boiling of the acid solution of aniline and ferricyanide of potassium I
have sometimes conducted in open vessels, sometimes in closed vessels, and
sometimes in retort-shaped vessels, when, as in the latter case, I have con-
densed the liquids coming from them, and used them in future operations and
otherwise.
The waste products obtained throughout this process may be turned to
account in the usual manner, well known to chemists when dealing with such
products; or they may be so far treated as is likewise well known and used in
future operations in obtaining the above colour, or the various shades of the
same; but this I do not consider to be part of my Invention, my Invention
being for the preparation of coloring matters for dyeing, staining, or printing
fabrics, stuffs, and yarns of cotton, silk, or wool, or such like substances, by the
action of cyanides, ferricyanides, or ferrocyanides, or other bodies containing
cyanogen, upon aniline, xylidine, cumidine, toluidine, or any other analogous
substance or substances.
In witness whereof, I, the said Michael John Stark, have hereunto set
my hand and seal, this Fifth day of June, in the year of our Lord
One thousand eight hundred and sixty-one.
Signed, sealed, and delivered
in the presence of
WILLIAM SKIPPER,
Solicitor, Norwich.
MICHAEL JOHN STARK. (L.S.)