The Manufacture or Production of a New Blue Colouring Matter.
Year: 1893

page_text: Date of Application, 7th Apr., 1893
Complete Specification Left, 6th Jan., 1894-Accepted, 10th Feb., 1894
PROVISIONAL SPECIFICATION.
[Communicated from abroad by THE FARBENFABRIKEN vormals FRIEDRICH
BAYER & Co., of Elberfeld, in the Empire of Germany.]
The Manufacture or Production of a New Blue Colouring Matter.
I HENRY EDWARD NEWTON of The Office for Patents, 6 Bream's Buildings,
Chancery Lane, in the County of London, Patent Agent, do hereby declare the
nature of this invention to be as follows:-
It is known, that the bluish-violet dye-stuff resulting from nitrosodimethylaniline
hydrochlorate and gallamide, as described in the Letters Patent No. 2941, dated
19th February 1889, is technically valueless, on account of its insolubility in water,
and must be converted (by a subsequent treatment with sodium bi-sulphite) into a
soluble bisulphite compound (the so-called "gallamine-blue"), in order to render it
capable of being employed for dyeing or printing purposes.
There is no mention of the corresponding dye-stuff from nitrosodiethylaniline,
either in the aforesaid English Letters Patent, or in the corresponding foreign
Patents. Neither is it certain that the latter dye-stuff, if obtained by means of
the processes described in the above English Letters Patent, and in the corre-
sponding foreign Patents, would have any advantage in comparison with the
colouring matter from nitrosodimethylaniline and gallamide.
My foreign correspondents have, however, found, that the dye-stuffs obtained by
acting with nitrosodiethylaniline hydrochlorate, or other salts of nitrosodiethyl-
aniline, on gallamide, are technically very valuable products, and, compared with
the "gallamine-blue," possess such great advantages, that it would be difficult to
accept them as homologues, without knowledge of their composition.
""
Whilst the colouring-matter from nitrosodimethylaniline hydrochlorate is
insoluble in hot water the dye-stuff from nitrosodiethylaniline easily dissolves, and
need not be changed into its bisulphite compound as before mentioned. The
bisulphite compound of the former (the so-called "gallamine-blue") does not yield
"even shades on wool mordanted with chromium salts, whilst the dye-stuff from
nitrosodiethylaniline directly yields perfectly even "shades, and possesses the
property of dyeing equally throughout the thickest materials. "Gallamine-blue"
produces violet shades, but those obtained by means of the product from nitroso-
diethylaniline are a beautiful blue, and are superior by their beauty and purity to
those obtained by all the known oxazine colouring-matters. Besides, "gallamine-
blue" cannot, in dyeing and printing, be combined with all dye-stuffs (as it contains
bisulphite), especially with those which are reduced or destroyed by the action of
the bisulphite. The new colouring matter prepared by my foreign correspondents
can be used in any case, as it can be employed directly without the addition of
bisulphites. It possesses, likewise, a greater dyeing strength than the "gallamine-
blue," for its intensity is greater by about 30 per cent. than that of the latter.
The new dye-stuff derived from nitrosodiethylaniline possesses the same valuable
properties as the "gallamine-blue," viz., perfect fastness against fulling, without
any alteration in shade, great fastness against the action of light, and also the
property of not being altered by alkalies, dilute acids, or chlorine.
The production of the new dye-stuff is illustrated by the following example,
The parts are by weight.

page_text: EXAMPLE.
COLOURING MATTER FROM NITROSODIETHYLANILINE AND GALLAMIDE.
1 part of gallamide, and from one and a half to 2 parts of the hydrochlorate of
nitrosodiethylaniline, are stirred with 1 part of alcohol. The resulting mixture is
heated, until a test portion dissolves with a pure blue colour. The mass is then
poured into 10 parts of water, and the resulting liquid is mixed with a small
quantity of hydrochloric acid. After some time, the dye stuff separates in
crystalline state. It is isolated by filtering off and drying.
My foreign correspondents do not limit themselves to the above process of
producing this valuable dye stuff, as the directions given in the foregoing example
can be varied; for instance, in place of the hydrochlorate of nitrosudiethylaniline,
the corresponding quantities of the analogous salts can be used; the alcohol
employed in the above example can be replaced by other solvents or diluents. Of
course, such or similar modifications do not alter the nature of the invention
hereinbefore defined.
D: 1
"11000
NEWTON & SON,
Agents for the Applicant.
COMPLETE SPECIFICATION.
The Manufacture or Production of a New Blue Colouring Matter.
I, HENRY EDWARD NEWTON of The Office for Patents, 6 Bream's Buildings,
Chancery Lane in the County of London, Patent Agent, do hereby declare the
nature of this invention and in what manner the same is to be performed, to be
particularly described and ascertained in and by the following statement :-
It is known that the bluish-violet dye-stuff formed from_nitrosodimethylaniline
hydrochloride and gallamide, as described in the Letters Patent No. 2941, dated
19th February 1889, is technically valueless, on account of its insolubility in water,
and must be converted (by a subsequent treatment with sodium bisulphite) into a
soluble bisulphite compound (the so-called "gallamine blue"), in order to fit it
for dyeing or printing purposes.
There is no mention of the corresponding dyestuff from nitrosodiethylaniline
either in the aforesaid English Letters Patent or in the corresponding foreign
Patents. Nor is it certain that the latter dye-stuff, if obtained by means of the
processes described in the above English Letters Patent and in the corresponding
foreign Patents, would have any advantage over the coloring matter from nitroso
dimethylaniline and gallamide.
My foreign correspondents have found, however, that the dye-stuff obtained by
the interaction of nitrosodiethylaniline hydrochloride and gallamide, is technically
a very valuable product, which, in comparison with the "gallamine blue," possesses
such great advantages, that it would be difficult to regard them as homologues, if
their composition were unknown.
Whereas the coloring matter from nitrosodimethylaniline hydrochloride is
insoluble in hot water, the dye-stuff from nitrosodiethylaniline easily dissolves, and
need not therefore be converted into a bisulphite compound. The bisulphite
compound of the so-called "gallamine blue," does not yield "even" shades on wool
mordanted with chromium salts, but the dye-stuff from nitroso diethylaniline
directly yields perfectly even shades, and possesses the property of dyeing
equally throughout the thickest materials. Gallamine blue produces violet shades,
but those obtained by means of the product from nitrosodiethylaniline are a
beautiful blue, superior in beauty and purity to those obtained by means of all the
known oxazine coloring matters. Moreover, in dyeing and printing, gallamine blue
66
"

page_text: cannot be used together with all dye-stuffs, inasmuch as it contains bisulphite,
especially those which are reduced or destroyed by the action of a bisulphite.
The new coloring matter prepared by my foreign correspondents is generally
applicable, as it can be directly used without adding any bisulphite. It is also of
greater dyeing strength than gallamine blue, its intensity being greater than that
of the latter dye-stuff.
The new dye stuff derived from nitrosodiethylaniline has the same valuable
properties as gallamine blue, withstanding fulling without suffering any alteration
in shade, and exhibiting great fastness on exposure to light, and also being
unaltered by alkalies dilute acids, or chlorine.
The production of the new dye-stuff is illustrated by the following example.
The parts are by weight.
EXAMPLE.
COLORING MATTER FROM NITROSODIETHYLANILINE AND GALLAMIDE.
1 part of gallamide, and from one and a half to 2 parts of nitrosodiethylaniline
hydrochloride, are stirred up with 1 part of alcohol. The resulting mixture is
heated until a test portion dissolves in water, affording a pure colored solution.
The mass is then poured into 10 parts of water, and the resulting liquid is mixed
with a small quantity of muriatic acid. After a time, the dye-stuff separates in a
crystalline state. It is isolated by filtering off and drying. The dye-stuff' thus
produced is analogous to the so-called "gallocyanine," and if the latter product
has the formula suggested by R. Nietzki (in his manual entitled "Chemie der
Organischen Farbstoffe," of the year 1889, on page 141), the new coloring matter
herein described can be represented by the following formula :-
Cof
My foreign correspondents do not limit themselves to the above process of
producing this valuable dye-stuff, as the directions given in the foregoing example
can be varied; for instance, in place of the alcohol prescribed therein, other
solvents or diluents can be used. Of course, such or similar modifications do not
alter the nature of the invention herein before defined.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed, as communicated to me-
from abroad, I declare that what I claim is :—
1. The process of producing a blue coloring matter, which process consists in
acting with nitroso diethylaniline hydrochloride on gallamide in the presence of
suitable solvents or diluents.
2. As a new product of manufacture, the new dye-stuff produced by the process
hereinbefore defined, or by any other means affording the same result.
Dated this 2nd day of January 1894
NEWTON & SON,
Agents for the Applicant.