IMPROVEMENTS IN OBTAINING COLORING MATTERS.
Year: 1864

page_text: LETTERS PATENT to Richard Smith and Christian Sieberg, both of
Glasgow, in the County of Lanark, North Britain, Chemists, for the
Invention of "IMPROVEMENTS IN OBTAINING COLORING MATTERS.".
Sealed the 16th December 1864, and dated the 20th June 1864.
PROVISIONAL SPECIFICATION left by the said Richard Smith and
Christian Sieberg at the Office of the Commissioners of Patents, with
their Petition, on the 20th June 1864.
We, RICHARD SMITH and CHRISTIAN SIEBERG, both of Glasgow, in the
County of Lanark, North Britain, Chemists, do hereby declare the nature of
the said Invention of "IMPROVEMENTS IN OBTAINING COLORING MATTERS," to be
as follows, that is to say :-
This Invention relates to various processes for obtaining coloring matters.
In one process a mixture of a salt of rosaniline, or the base rosaniline itself,
with hydriodic acid and an alcohol, is heated to a temperature of 212 to
250 degrees Fahrenheit for about four hours, or until a violet color is pro-
duced. A good result is obtainable with the following or approximate pro-
portions; namely, 75 parts hydrochlorate or acetate of rosaniline, or the base
rosaniline itself, with 160 parts strong methylated spirit, and 160 parts con-
centrated hydriodic acid. This mixture is heated to 250 degrees Fahrenheit
until the violet is produced. The product is mixed with 500 parts methy-
lated spirit and a solution of caustic soda, and is boiled until the spirit is

page_text: evaporated and the iodine is combined with the soda, from which it can be
easily recovered. The separated coloring matter is washed with water, and
combined with bydrochloric or other suitable acid, and is dissolved in spirit,
the solution being suitable for dyeing and printing. It is preferred to use
hydriodic acid prepared by concentrating until its boiling point is 250 degrees
Fahrenheit, the weak hydriodic acid obtained by the well-known process of
suspending iodine in water, and passing through it a stream of hydrosulphuric
acid.
In a second process alcohol is added to a salt of rosaniline containing more
than one equivalent of hydriodic acid, and the mixture is heated as before;
or to a very strong solution of a rosaniline salt in alcohol hydriodic acid is
added, and heat is applied until the violet is produced. A good result is
obtainable with the following or approximate proportions, namely, one part of
hydriodate of rosaniline containing three equivalents of hydriodic acid, and
two parts strong methylated spirit, which mixture is treated as in the example
herein-before detailed. Bromine may be substituted for iodine in the pro-
cesses herein-before described.
In a third process a mixture of one part oxanilide and three parts acetate of
rosaniline is heated to a temperature of about 400 degrees Fahrenheit for
about ten hours, when a violet coloring matter is produced. The product is
boiled repeatedly with acids to remove red, and the remaining matter is dis-
solved in methylated spirit to be used in dyeing and printing.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Smith and Christian Sieberg in the Great Seal
Patent Office on the 17th December 1864.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, RICHARD
SMITH and CHRISTIAN SIEBERG, both of Glasgow, in the County of Lanark,
North Britain, Chemists, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twentieth day of June, in the year of our Lord One
thousand eight hundred and sixty-four, in the twenty-eighth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto us,
the said Richard Smith and Christian Sieberg, Her special licence that we,
the said Richard Smith and Christian Sieberg, our executors, administrators,
and assigns, or such others as we, the said Richard Smith and Christian
Sieberg, our executors, administrators, or assigns, should at any time agree

page_text: 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
OBTAINING COLORING MATTERS," upon the condition (amongst others) that we,
the said Richard Smith and Christian Sieberg, our executors or adminis-
trators, by an instrument in writing under our, or one of our, 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 six calendar
months next and immediately after the date of the said Letters Patent.
NOW KNOW YE, that we, the said Richard Smith and Christian Sieberg,
do hereby declare the nature of our said Invention, and in what manner
the same is to be performed, to be particularly described and ascertained
in and by the following statement in writing, that is to say :-
Our said Invention relates to the obtaining of violet coloring matters by
improved processes.
In one process we mix rosaniline or a salt of rosaniline with bydriodic acid
and an alcoliol, and we heat the mixture to a temperature of 250 to 270
degrees Fahrenheit for about four hours, or until the violet color is produced.
We conduct the operation in a closed vessel, preferring an iron vessel lined
with lead. The violet may be rendered bluer or redder by varying the time
during which heat is applied. We find the following proportions of the
ingredients to answer well, namely, 75 parts by weight of rosaniline or salt of
rosaniline, with 160 parts by weight of methylated spirit, and 160 parts by
weight of concentrated hydriodic acid. We prefer in this process to use
hydriodic acid prepared by concentrating until its boiling point is about 250
degrees Fahrenheit, the weak hydriodic acid obtained by the well-known
process of suspending iodine in water, and passing through it a stream of
hydrosulphuric acid.
In another process chemically equivalent to that herein-before described,
but somewhat simplified, we mix 62 parts by weight of iodine with 200 parts
by weight of methylated spirit, and conduct through the mixture, which
should be continuously agitated, a stream of hydrosulphuric acid until a slight
excess is apparent. The requisite quantity may also be determined by the
solution becoming of a pale brown color, which does not get darker on further
agitation. If the hydrosulphuric acid is too much in excess the addition of a
little more iodine will correct it. We remove the precipitated sulphur from
the solution thus obtained, and then dissolve in the solution 75 parts by weight

page_text: of hydrochlorate or acetate of rosaniline, the dissolving action being accele-
rated by a slight heat. We then proceed as in the first process.
The product obtained by either process we dissolve in a considerable quantity
of methylated spirit, and then boil with caustic soda, with which last the
iodine combines, and from which it can be easily recovered. The separated
coloring matter we then combine with hydrochloric or other suitable acid,
and afterwards dissolve it in spirit or water, the solution being suitable for
dyeing and imparting to wool or silk a beautiful violet shade. A less proportion
of iodine than what is herein-before prescribed may be used, but in that case
the mixture must be heated for a longer time to produce a similar effect.
Bromine may also be substituted for the iodine.
In our Provisional Specification lodged on applying for the herein-before
in part recited Letters Patent, other processes or modifications of processes
were referred to besides what is herein-before described, but as we have not
found such processes to be of practical utility, we do not now make any claim
respecting them.
Having thus particularly described our said Invention, and in what
manner the same is or may be performed, we have to state that we do not
restrict ourselves to the precise details herein-before described, but that what
we believe to be novel, original, and useful, and claim as the Invention
secured to us by the herein-before in part recited Letters Patent is, the
obtaining of violet coloring matters by the action of hydriodic or hydro-
bromic acid on an alcohol, and on rosaniline or a salt of rosaniline.
In witness whereof, we, the said Richard Smith and Christian Sieberg,
have hereunto set our hands and seals, this Sixteenth day of
December, in the year of our Lord One thousand eight hundred and
sixty-four.
Witness,
EDMUND HUNT,
Patent Agent,
28, St. Enoch Square,
Glasgow.
(L.S.)
RICHARD SMITH.
CHRISTIAN SIEBERG. (L.S.)