Improvements in the Manufacture of Mordant Dyeing Colouring Matters.
Year: 1892

page_text: Date of Application, 18th July, 1892
Complete Specification Left. 11th Apr., 1893-Accepted, 13th May, 1893
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Mordant Dyeing Colouring
Matters.
I JAMES YATE JOHNSON of 47 Lincolns 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 Anilin and Soda Fabrik of
Ludwigshafen on Rhine in the Empire of Germany) to be as follows:-
This invention relates to improvements in the process described under my appli-
cation for Letters Patent No. 19589 of A.D. 1891 and consists in a modification of
that process by means of which a somewhat different product is obtained.
In the example given the Provisional Specification of that application the treat-
ment of 14' dinitro-anthraquinone with fuming sulphuric acid containing about
forty per cent. free anhydride is described, followed by the isolation of a product'
soluble in water and its subsequent conversion by treatment with concentrated
sulphuric acid into a comparatively insoluble and valuable mordant dyeing colouring:
matter.
If in this example instead of using fuming acid containing about 40 per cent. of
free anhydride in the first stage of the reaction, a weaker fuming acid be used
(containing say about 12 per cent. free anhydride) then on proceeding as described
in the said example, that is on treating with concentrated sulphuric acid, after
isolation of the product of the first stage, a somewhat different product, as
hereinafter described, is obtained. The product obtained is different also to a
marked degree from that resulting from the process described in the first example
of the Application No. 19588 of 1891 wherein 14' dinitro-anthra quinone is treated
with fuming acid of the strength mentioned (twelve per cent. free anhydride) and
the soluble product obtained is, without isolation but after dilution to the required
strength, further treated with non-fuming acid.
The following example will further illustrate the nature of the invention but I
do not bind myself to details as many variations can be introduced without
essentially altering the result:
Example.--Mix about ten parts (the parts are by weight) of 1.41 dinitro-
anthraquinone with about one hundred parts of fuming sulphuric acid con-
taining about twelve per cent. free anhydride, heat the mixture to a temperature'
of about one hundred and sixty degrees centigrade and maintain the hea
for about one and a half to two hours. A soluble colouring matter
produced giving a violet solution in water. Dissolve the whole in water an
precipitate the colouring matter with common salt. Collect and dry. In the dry
form this' colouring matter is a black powder with metallic sheen giving a violet-
blue colour in sodium-carbonate solution, a blue colour in caustic soda, and a violet*
colour in concentrated sulphuric acid.
Mix the dry colouring matter with about ten times its weight of ordinary con-
centrated sulphuric acid (containing about ninety-five per cent. real acid H.SO.)
heat the mixture to about one hundred and thirty degrees centigrade and maintain
the heat for about five hours or until no further conversion into the insoluble
colouring matter takes place. Pour into water, filter and wash well with water.
The new dye fixes itself on métallic mordants giving for instauce a beautiful"
It dissolves in concentrated
violet-blue colour on chrome mordanted wool.
sulphuric acid giving a blue solution the solution in caustic soda is also blue. The
dye is not a single chemical compound but appears to be a mixture of two or more

page_text: compounds. It can however be used without any further purification or separation
of its components.
Dated this 18th day of July 1892.
J. H. JOHNSON & Co.,
47 Lincoln's Inn Fields, London, W.C., Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Mordant Dyeing Colouring
Matters.
I JAMES YATE JOHNSON of 47 Lincolns 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 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 :-
This invention relates to improvements in the process described in the Specifi-
cation of Letters Patent No. 19589 of 1891 granted to me on a communication of
my foreign correspondents and cousists in a modification within the scope of that
process by means of which a somewhat different product is obtained.
In the example given in the said Specification the treatment of 14' dinitroanthra-
quinone with fuming sulphuric acid containing about forty per cent. free anhydride
is described, followed by the isolation of a product soluble in water and its
subsequent conversion by treatment with concentrated sulphuric acid into a
comparatively insoluble and valuable mordant dyeing colouring matter.
40
If in this example instead of using fuming sulphuric acid containing about
per cent. of free anhydride in the first stage of the reaction a weaker fuming
acid be used, (containing say about 12 per cent. free anhydride), then on proceeding
as described in the said example, that is on treating with concentrated sulphuric
acid after isolation of the product. of the first stage a somewhat different product,
as hereinafter described, is obtained. The product obtained is also different to, a
marked degree from that resulting from the process described in the first example
of the Application No. 19588 of 1891, wherein 14 dinitroanthraquinone is treated
with fuming acid of the strength mentioned (twelve per cent. free anhydride) and
the soluble product obtained is without isolation but after, dilution. to, the required
strength further treated with nonfuming acid.
This present invention is not limited in its application to 1.4' dinitroanthra-
quinone as it can also be applied to the other dinitroanthraquinones mentioned in the.
Specification of Letters Patent No. 19589 of 1891,, namely alphadinitro-anthra-
quinone and the crude mixture of nitro-anthraquinones resulting from the energetic.
nitration of anthraquinone.
"
The following example will further illustrate the nature of the present invention
but I do not restriet myself to the precise details given in this example as they can
be varied without eseentially altering the result.
PAAMPLE.
(a.) Mix about ten parts (the parts are by weight) of 1:4! dinitroanthraquinone
with about one hundred parts of fuming sulphuric acid containing, about
twelve per cent. free anhydride; heat. the mixture to a temperature of about one
hundred and sixty degrees centigrade, and maintain the heat for about one and a half
to two hours. A soluble colouring-matter is produced giving a violet solution in
water. Dissolve the whole in water and precipitate the colouring, matter, with
common salt. Collect and dry., In the dry form this colouring-matter is a black
powder with a metallic sheen, giving a violet-blue colour in sodium carbonate

page_text: solution, a blue colour in caustic soda solution, and a violet colour in concentrated
sulphuric acid.
(b.) Mix the said dry colouring matter with about ten times its weight of
ordinary concentrated sulphuric acid (containing about ninety five per cent. real
acid H,SO), heat the mixture to about one hundred and thirty degrees centigrade,
and maintain the heat for about five hours or until no further conversion into the
insoluble colouring matter takes place. Pour into water, filter and wash well with
water.
.
The new dye so produced fixes itself on metallic mordants yielding for instance,
a beautiful violet-blue colour on chrome mordanted wool. It dissolves in concen-
trated sulphuric acid giving a blue solution, the solution in caustic soda is also
blue. The said dye is not a single chemical compound but appears to be a mixture
of two or more compounds. It can however be used without any further purification
or separation of its components.
Having now fully 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 :-
The improvement in the manufacture of mordant dyeing colouring matters by
first treating dinitroanthraquinones as herein explained with fuming sulphuric acid
containing about twelve per cent. free sulphuric anhydride, then isolating the
soluble colouring matters obtained and afterwards converting the said soluble
colouring matters into comparatively insoluble mordant dyeing colouring matters
by the action of ordinary concentrated sulphuric acid, all substantially as herein
before described.
Noted this 11th 1.
A
11000
J. H. JOHNSON & Co.,
Agents.