The Manufacture and Production of Greenish Blue Mordant Dyeing Colouring Matters.
Year: 1892

page_text: Date of Application, 24th Aug., 1892
Complete Specification Left, 3rd May, 1893-Accepted, 2nd June, 1893
PROVISIONAL SPECIFICATION.
The Manufacture and Production of Greenish Blue Mordant Dyeing
Colouring Matters.
I JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of Middlesex
Gentleman do hereby declare the nature of this invention which has been com-
municated to me from abroad by The Badische Aniline and Soda Fabrik of
Ludwigshafen on Rhine in the Empire of Germany to be as follows:-
It is known that certain soluble colouring matters can be produced by the action
of fuming sulphuric acid on certain di-nitro-anthraquinones and my foreign
correspondents have treated these soluble colouring matters which are intermediate
products with ordinary concentrated sulphuric acid for the production of mordant
dyeing colouring matters therefrom.
My foreign correspondents have also discovered that if the said soluble colouring
matters be suitably treated with an excess of strong ammonia, new and valuable
dyes are obtained. Similarly dyes are obtained on treating these intermediate
products with substituted ammonia compounds such as methylamines or aniline,
their homologues or analogues and the like.
The following examples will serve to illustrate the nature of this invention but I
do not bind myself to them as they are capable of considerable variation without
departing from the nature of this invention.
Mix about ten parts of the above mentioned soluble intermediate product with
about fifty to one hundred parts of aniline and heat the mixture at a temperature
of about one hundred and ninety to two hundred degrees centigrade for about five
or six hours or until the conversion into the dye difficultly soluble in acidified water
is complete. Then pour the melt into water heat to the boiling point acidify with
hydrochloric acid filter and wash with water to remove the excess of aniline salt.
In order to obtain the dye in a finely divided state dissolve it in caustic soda
precipitate with hydrochloric acid and wash.
As aforesaid analogous results can be obtained by the use of other ammonia
analogues besides aniline in a manner similar to that hereinbefore described.

page_text: Further the intermediate products obtained from other di-nitro-anthraquinones
besides the 14 dinitro-anthraquinone can be used such as for instance those from
alpha-dinitro-anthraquinone and from the crude mixture of dinitro-anthraquinones
resulting from the energetic nitration of anthraquinone. Also the intermediate
products obtainable from the reduction products of the dinitro-anthraquinones
yield analogous results.
Dated this 24th day of August 1892.
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, London, Agents.
COMPLETE SPECIFICATION.
The Manufacture and Production of Greenish Blue Mordant Dyeing
Colouring Matters.
I JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
Middlesex Gentleman do hereby declare the nature of this invention (which has
been communicated to me from abroad by The Badische Anilin and 'Soda Fabrik
of Ludwigshafen-on-Rhine in the Empire of Germany) and in what manner the
same is to be performed to be particularly described and ascertained in and by the
following statement :-
In the Specifications of Letters Patent No. 19588 and 19589 of 1891, granted to
me, on communications from my foreign correspondents, processes are described for
the production of mordant dyeing colouring matters from certain dinitro-anthra-
quinones. In the said processes, colouring-matters soluble in water are first
obtained as intermediate products. These soluble colouring matters constitute the
initial material which is used in this present invention.
The production of some similar soluble colouring matter from nitro-anthra-
quinones has been described in the lapsed German Patent No. 6526.
Now my foreign correspondents have discovered that if the intermediate soluble
colouring-matters of the aforesaid Letters Patent No. 19588 and 19589 of 1891
be suitably treated with an excess of strong ammonia, new and valuable dyes are
obtained. Similarly dyes are obtained on treating these intermediate products
with substituted ammonia compounds, such as methylamines, or aniline, their
homologues, or analogues and the like.
The following examples will serve to illustrate the nature of this invention and
the manner in which it can be carried into practical effect but I do not bind myself
to them as they are capable of considerable variation without departing from the
nature of the invention. The parts are by weight.
PREPARATION OF A NEW
GREENISH-BLUE MORDANT DYEING COLOURING
MATTER FROM THE AFORESAID SOLUBLE COLOURING MATTERS OR
INTERMEDIATE PRODUCT DESCRIBED IN THE SPECIFICATION OF LETTERS
PATENT NO. 19589º¹
Mix about ten parts of the above mentioned intermediate product readily soluble
in water with about fifty to one hundred parts of concentrated ammonia solution
containing about twenty two per cent. ammonia (NH2) and whilst the mixture is in
a closed vessel capable of withstanding pressure heat it at a temperature of from
about one hundred and seventy five to one hundred and eighty degrees centigrade
for about three to five hours or until no further conversion into the colouring
matter difficultly soluble in acidified water takes place. Then acidify the hot
solution with hydrochloric acid filter off the precipitated colouring matter, wash
and preserve for use in the form of paste. The colouring matter so obtained
closely resembles that described in the aforesaid application for Patent No. 19589.

page_text: It fixes itself on chrome mordanted wool giving a greener shade of blue than that
given by the said colouring matter of the Patent 19589º¹.
Instead of the concentrated ammonia solution in the above example methyl-
amines and ethylamines can be used in the same way.
EXAMPLE 2.
Mix about ten parts of the above mentioned soluble intermediate product with
about fifty to one hundred parts of aniline, and whilst the mixture is in a closed
vessel capable of withstanding pressure heat it at a temperature of from about
one hundred and ninety to two hundred degrees centigrade for about five or six
hours or until the conversion into the dye difficultly soluble in acidified water is
complete. Then pour the melt into water, heat to the boiling point, acidify with
hydrochloric acid, filter and wash with water to remove the excess of aniline salt.
In order to obtain the dye in a finely divided state dissolve it in caustic soda,
precipitate. with hydrochloric acid and wash.
As aforesaid analogous results can be obtained by the use of other ammonia
analogues besides aniline (for instance ortho-toluidine) in a manner similar to that
herein before described. Further the intermediate products obtained from other
dinitro-anthraquinones besides the 14' dinitro-anthra-quinone can be used such as,
for instance, those from alpha-dinitro-anthraquinone and from the crude mixture of
dinitro-anthra-quinones resulting from the energetic nitration of anthraquinone.
Also the intermediate products obtainable from the reduction products of the
dinitro-anthra-quinones (such as can be obtained in the manner described in the
Specification of the application for Letters Patent No. 13029 of 1892) yield
analogous results.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
1. The manufacture of greenish-blue mordant dyeing colouring-matters by
treating the soluble colouring matters hereinbefore defined with ammonia or sub-
stituted ammonia compounds, such as methylamines or aniline or their homologues
or analogues or the like substantially as hereinbefore described.
2. The manufacture of greenish-blue mordant dyeing colouring matters by
treating the soluble colouring matters herein before defined with concentrated
ammonia solution substantially as hereinbefore described in Example 1.
3. The manufacture of greenish-blue mordant dyeing-colouring matters by
treating the soluble colouring matters hereinbefore defined with aniline or ortho-
toluidine substantially as hereinbefore described in Example 2.
4. As new products the new greenish-blue mordant dyeing colouring-matters
such as can be obtained substantially as hereinbefore described.
Dated this 3rd day of May 1893.
J. H. JOHNSON & Co.,
Agents.