The Manufacture and Production of Black Colouring-matters of the Anthraquinone Series, suitable for. Directly Dyeing Cotton in the Cold Bath.
Year: 1895

page_text: Date of Application, 13th Aug., 1895
Complete Specification Left, 24th Apr., 1896-Accepted, 6th June, 1896
PROVISIONAL SPECIFICATION.
The Manufacture and Production of Black Colouring-matters of
the Anthraquinone Series, suitable for. Directly Dyeing Cotton
in the Cold Bath.
1, JAMES YATE JOHNSON, of 47 Lincoln's Inn Fields, in the County of
London, Patent Agent, do hereby declare the nature of this invention (which
has been communicated to me from abroad by The Badische Anilin & Soda
Fabrik of Ludwigshafen-on-Rhine, in the Empire of Germany) to be as
follows:-
In the Specification of Letters Patent No. 10996" granted to me there is
described that Troost in 1861 had found that on the action of alkaline reducing
agents (sulphides and polysulphides) on dinitro naphthalenes both red and violet,
or blue, dyestuffs may be obtained (Jahresberichte über die Fortschritte der
Chemie 1861, p. 958, Rep. chim. appl. 1861, 405).
Further my foreign correspondents in 1893 have manufactured valuable black
cotton-dyestuffs differing from the products of Troost, as described in the said
Specification of Letters Patent No. 10996".
Also nitro-derivatives of anthra-quinone have already been treated with alkaline
sulphides and converted into the corresponding amido-compounds (mono- and
diamido anthraquinone) by these agents (Böttger, Petersen Annalen 166, 150).
In this process intermediate products are obtained; that from di-ortho nitro-
anthraquinone has already been developed by Römer with potassium-stannite and
is described in the "Berichte der Deutschen Chemischen Gesellschaft, volume XVI,
p. 363. It is soluble in caustic soda solution with a blue colour..
My foreign correspondents have now found that by a stronger action of alkaline
sulphides (or poly-sulphides) on dinitro-anthraquinones or by further treating
the said diamido-anthraquinones or the above mentioned intermediate products
with the said agents, until they are perfectly soluble in water, compounds
are obtained quite different from those above mentioned. When diluted with
water bluish green or violet blue solutions are obtained, out of which the said
compounds are precipitated by the aid of acids; they are insoluble in acids but
are soluble in alkalies and alkaline sulphides and dye cotton directly in a solution
of sodium sulphide or in an alkaline solution.
°
As dinitro-anthraquinones, both the 1.4' di-ortho-nitro-anthraquinone and the
crude nitro-product, obtained by nitrating anthraquinone or the dinitro-anthra-
quinone contained in the latter, can be employed.
The following examples of the manner in which the new dyes can be obtained
will serve to further illustrate the nature of the invention and the manner in which
it can be carried into practical effect, but these are merely typical methods of
production and great variations can be made without departing froin the nature of
the invention. The parts are by weight.
'

page_text: and forty parts of dinitro-anthraquinone and heat until a test portion is quite
soluble in water. After cooling, a firm black crude product is obtained which
can be employed directly for dyeing or it can be transformed by appropriate
operations.
The product so obtained is readily soluble in cold water with a blue colour and
in concentrated sulphuric acid with a grayish-black colour. It is rather soluble
in alcohol with a green colour but is insoluble in acetone. The aqueous solution
can be precipitated with diluted mineral acids or with acetic acid; the precipitate
is very readily soluble in alkalies and alkaline sulphides and these solutions dye
cotton black.
EXAMPLE II.
Conformably with the process described in the foregoing example alpha-dinitro-
anthraquinone and the mixture of the crude nitrated anthraquinones can be
converted into the corresponding dyestuffs on employing fifty parts of alpha- or
crude dinitro-anthraquinone instead of the same quantity of 1.4' di-ortho-anthra-
quinone. The product obtained from alpha-dinitro-anthraquinone dissolves in
water with a violet-blue colour and also in alcohol, in acetone it dissolves with
bluish-green colour and in concentrated sulphuric acid with a brownish-red colour.
Cotton is dyed black.
Instead of the nitrated authraquinones of course also the corresponding amido-
compounds of anthraquinones, or the above said intermediate products, can be
employed and the corresponding dyestuffs are obtained.
The black shades obtained on cotton are very fast against the action of light,
acids, soap and chlorine.
Dated this 13th day of August. 1895.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.
COMPLETE SPECIFICATION.
The Manufacture and Production of Black Colouring-matters of
the Anthraquinone Series, suitable for Directly Dyeing Cotton
in the Cold Bath.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields, in the County of
London, Gentleman, do hereby declare the nature of this invention (which has
been communicated to me from abroad by The Badische Anilin & Soda Fabrik
of Ludwigshafen-on-Rhine, Germany) and in what manner the same is to he
performed to be particularly described and ascertained in and by the following
statement :-
:
In the Specification of Letters Patent No. 10996 granted to me it is explained
that Troost in 1861 had found that by the action of alkaline reducing agents
(sulphides and polysulphides), on dinitro-naphthalenes, both red and violet, or
blue, dyestuffs may be obtained (Tahresberichte über die Fortschritte der
Chemie 1861, p. 958; Rep. chim. appl. 1861, 405), and further in the said Specifi-
cation there is described the manufacture of valuable black cotton-dyestuffs
differing entirely from the products of Troost.
Nitro-derivatives of anthraquinone have also been treated with alkaline
sulphides and converted into the corresponding amido compounds (mono- and di-
amido-anthraquinone) by these agents (Böttger, Petersen, Annalen 166, 150).
In this process intermediate products are obtained; and that from di-ortho-nitro-
anthraquinone has also been obtained by Römer by the use of potassium-stapnite
(see Berichte der Deutschen Chemischen Gesellschaft, volume XVI, p. 363) it is
soluble in caustic soda solution with a blue colour.

page_text: 2. The manufacture of the new colouring-matters in the manners described in
each of the two examples bereinbefore given.
3. As new articles of manufacture the new colouring-matters (which dye cotton
directly from a cold alkaline bath) all such as can be obtained substantially in the
manner hereinbefore described.
Dated this 24th day of April 1896.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.