IMPROVEMENTS IN PREPARING VIOLET, BLUE, AND RED COLORING MATTERS
Year: 1865

page_text: LETTERS PATENT to John Holliday, of Huddersfield, in the County of
York, Manufacturing Chemist, for the Invention of "IMPROVEMENTS IN
PREPARING VIOLET, BLUE, AND RED COLORING MATTERS."
PROVISIONAL SPECIFICATION left by the said John Holliday at the
Office of the Commissioners of Patents, with his Petition, on the 6th
October 1865.
I, JOHN HOLLIDAY, of Huddersfield, in the County of York, Manufacturing
Chemist, do hereby declare the nature of the said Invention for "IMPROVE.
MENTS IN PREPARING VIOLET, BLUE, AND RED COLORING MATTERS," to be as
follows:-
I produce a violet coloring matter by mixing, say, 70 parts by weight of
hydrochlorate of aniline with, say, 55 parts by weight of nitro-benzole, and
heating the mixture gradually up to a high temperature, say, 440° Fahrenheit
for 3 or 4 hours. The mass thus obtained I then put into about forty times
its bulk of water and boil it for about an hour, adding water as it boils away.
I afterwards filter this solution and precipitate the coloring matter from it
with a little alkali, by preference, ammonia or soda. I wash this precipitate
well with water and then dissolve it in methylated spirit and purify the color

page_text: obtained by distilling the spirit from the color. The residue is treated with
commercial hydrochloric acid, to which its bulk of water has been previously
added, and I reduce the residue thus dissolved to a dry body by evaporation.
In this form it is ready for sale as a violet dye, and may be rendered
ready for the dyer's vat by being dissolved in spirit, as is usual with aniline
colors.
To produce a blue coloring matter or dye I mix, say, 95 parts by weight
of nitro-benzole, by preference, at a low boiling point with, say, 200 parts by
weight of hydrochlorate of aniline. Other salts of aniline may be used.
The salt I prefer to be produced from aniline, boiling at a low temperature.
I heat this mixture for about three or four hours gradually up to a high
temperature, say, 440° Fahrenheit, when the color is formed. I then reduce
the product to a powder and wash it repeatedly in boiling water, to which I
have previously added a little bydrochloric acid, say, 10 per cent.
residue (the coloring matter) is again washed with water and then dried. To
purify further I dissolve this product in methylated spirit, filter the solution,
and distil the spirit to obtain the desired blue coloring matter ready for sale,
which may then be dissolved as is usual with other aniline colors ready for the
dyer's vat.
The
I produce a coloring matter of a red shade by mixing the proportions above
used for violet, say, twenty parts more nitro-benzole, and heating the mixture
for 3 or 4 hours gradually up to 440° Fahrenheit. I purify the coloring
matter so obtained by dissolving in water, filtering, and precipitating, as is
usual with ordinary aniline red.
I do not confine myself to the exact proportions and temperatures
SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said John Holliday in the Great Seal Patent Office on the 6th
April 1866.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JOHN
HOLLIDAY, of Huddersfield, in the County of York, Manufacturing Chemist,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Sixth day of October, in the year of our Lord One
thousand eight hundred and sixty-five, in the twenty-ninth year of Her reign,
did, for Herself, Her heirs and successors, give and grant unto me, the said

page_text: John Holliday, Her special licence that I, the said John Holliday, my
executors, administrators, and assigns, or such others as I, the said John
Holliday, 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
PREPARING VIOLET BLUE AND RED COLORING MATTERS," upon the condition
(amongst others) that I, the said John Holliday, my executors or adminis-
trators, 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
six calendar months next and immediately after the date of the said Letters
Patent.
•
:
NOW KNOW YE, that I, the said John Holliday, do hereby declare the
nature: of the said Invention, and in what manner the same is to bé
performed, to be particularly described and ascertained in and by the following
statement thereof, that is to say :-
. I produce a violet coloring matter by mixing, say, 56 pounds of hydro-
chlorate of aniline of commerce (the aniline of the above salt to be of a low
boiling point, say about 364° Fahrenheit) with about 44 lbs. of nitro-benzole of
commerce (I prefer the nitro-benzole of a low boiling point), and I heat the
mixture gradually up to a high temperature, say 440° Fahrenheit, for from 5
to 7 hours. As the operation progresses I take out samples to try its quality.
The colour is gradually formed in a somewhat bronzy mass, which when cold. I
put into about 40 times its bulk of water, and boil for about an hour, adding
water as it boils away; I afterwards filter this solution and precipitate the
coloring matter from it with a little alkali, by preference ammonia or soda,' I
wash this precipitate well with water, and afterwards, dissolve it in methylated
spirits, and I purify the color obtained by distilling the spirit from the color.
The residue (the coloring matter) I treat with commercial hydrochloric acid,
to which its bulk of water has been previously added, and I reduce the resi-
due thus dissolved to a dry body by evaporation, which may be dissolved as is
usual with aniline colors.
To produce a blue coloring matter or dye I mix about 34 lbs. of
nitro-benzole, by preference to be of a low boiling point, as free from
its homologues as possible, with, say, 66 lbs. of hydrochlorate of aniline,
the aniline of this salt I prefer as pure and as free from its homologues

page_text: as possible. I heat this mixture for about 5 to 7 hours gradually up to a high
temperature, say, 440° Fahrenheit, when the color is gradually formed; I test
for the colour by taking out samples from time to time. The coloring matter
when cold is a hard mass, I. then: reduce the product to a powder, and wash
repeatedly in boiling water to which I have previously added a little hydro-
chloric acid, say 10 per cent. The residue (the coloring matter). is again
washed with water and then dried. To purify further I dissolve this product
in methylated spirits, filter the solution and distil the spirit to obtain the
desired coloring matter which may, be then dissolved as is usual with other
aniline colors ready for the dyer's vat.
I produce a red colouring matter similar to ordinary magenta by mixing
with 75lbs. of hydrochlorate of aniline, 25 lbs. of nitro-benzole, İ
prefer the aniline used in the salt to be of a high boiling point, the. nitro-
benzole I prefer of a low boiling point;. this mixture I heat. gradually
up to 440° Fahrenheit or thereabouts, and maintain it till the colour
is gradually formed in a bronzy paste, which; when 'cold becomes hard and
brittle. I watch the formation of the color by taking samples from time to
time. I purify the mass thus obtained by methods adopted in purifying
ordinary magenta dye, other salts of aniline; may be used for producing those
colours, but I prefer the hydrochlorate of aniline. . When I use the; words
aniline and nitro-benzole I mean the commercial articles which usually contain
'more or less of their homologues as is indicated by the several boiling
points.
>
Having thus described my improvements and means which I adopt in
carrying the same into effect, I do not confine myself to the exact qualities,
quantities, or temperatures herein given as they may be varied without
materially effecting the results; but what I claim is the use of nitro-benzole
with a salt of aniline for making violet, blue, and red coloring matters or dyes,
substantially as explained.
In witness whereof, I, the said John Holliday, have hereunto set my
hand and seal, this Fifth day of April; in the year of our Lord One
thousand eight hundred and sixty-six.
JOHN HOLLIDAY. L.8.)