Manufacture of a Black Colouring Matter directly Dyeing Cotton.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
Manufacture of a Black Colouring Matter directly Dyeing Cotton.
I, CHARLES DENTON ABEL, of Birkbeck Bank Chambers, Southampton Buildings,
in the County of London, Consulting Engineer and Chartered l'atent Agent, do
hereby declare the nature of this invention (as communicated to ine from abroad by
Actien-Gesellschaft für Anilin-Fabrikation, of Berlin, in the Empire of Germany,
Chemical Manufacturers) to be as follows:-
My foreign correspondents have found that a valuable black dyestuff directly
dyeing cotton and distinguished by its great tinctorial power is obtained by heating
with sulphur and sodium sulphide a mixture of equinolecular proportions of dinitro-
laming
and dinitrophenol. (NU: NU₂?
the following example:
20 kilos. of dinitrooxydiphenylamine are mixed with 13-2 kilos. of dinitrophenol and
the mixture is introduced at about 100° C. into a melted mixture of 170 kilos. of
sodium sulphide, 60 kilos. of sulphur and 15 kilos. of water.
The formation of a dark black colouring matter begins almost at once.
The mass
is gradually heated up to 145° C. and this temperature is maintained during several
hours. In order to obtain the colouring matter produced in commercial form
several methods may be adopted. The mass is heated to a somewhat higher
temperature (160° to 170° C.) until it is dry and can be pulverized. Or the mass may
be dissolved in water, the aqueous solution caused to precipitate by means of common
salt and the precipitate dried. Or the dyestuff may be precipitated from the aqueous
solution of the mass by means of an acid, the precipitate thus produced re-dissolved
in an aqueous solution of sodium sulphide and the solution evaporated to dryness.
The colouring inatter obtained in any of these ways dissolves in water forming a
deep blue-black solution. It dyes cotton in a bath containing some salt deep greenish-

page_text: In the process above described ortho-amido-para-nitrophenol may be substituted
for dinitrophenol without altering the nature of the dyestuff produced..
Dated this 29th day of September 1899.
ABEL & IMRAY,
Agents for the Applicant.
COMPLETE SPECIFICATION.
Manufacture of a Black Colouring Matter directly Dyeing Cotton.
I, CHARES DENTON ABEL, of Birkbeck Bank Chambers, Southampton Buildings,
in the County of London, Consulting Engineer and Chartered Patent Agent, do
hereby declare the nature of this invention (as communicated to me from abroad by
Actien-Gesellschaft für Anilin-Fabrikation, of Berlin, in the Empire of Gerinany,
Chemical Manufacturers) and in what manner the same is to be performed, to
be particularly described and ascertained in and by the following statement :-
My foreign correspondents have found that a valuable black dyestuff directly dyeing
cotton and distinguished by its great tinctorial power is obtained by heating with
sulphur and sodium sulphide a mixture of equimolecular proportions of dinitro-
oxvdiphenylamine:
and dinitrophenol (NO, NO, OH
:
=
1:3:4).
The invention is illustrated by the following example:
20 kilos. of dinitrooxydiphenylamine are mixed with 132 kilos. of dinitrophenol
and the mixture is introduced at about 100° C. into a melted mixture of 170 kilos. of
sodium sulphide, 60 kilos. of sulphur and 15 kilos. of water.
The formation of a dark black colouring matter begins almost at once.
The mass
is gradually heated up to 145° C. and this temperature is maintained during several
hours. In order to obtain the colouring matter produced in commercial forın several
methods may be adopted. The mass is heated to a somewhat higher temperature
(160° to 170° C.) until it is dry and can be pulverised. Or the mass may be dissolved
in water, the aqueous solution caused to precipitate by means of common salt and
the precipitate dried. Or the dyestuff may be precipitated from the aqueous solution
of the mass by means of an acid, the precipitate thus produced re-dissolved in an
aqueous solution of sodium sulphide and the solution evaporated to dryness.
The colouring inatter obtained in any of these ways dissolves in water forming a
deep blue-black solution. It dyes cotton in a bath containing some salt deep-
greenish-black shades.
In the process above described ortho-amido-para-nitrophenol may be substituted
for dinitrophenol without altering the nature of the dyestuff produced.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is:-
1. The herein described manufacture of a black colouring matter directly dyeing

page_text: cotton by heating with sulphur and sulphides of alkali-metals a mixture of equi-
molecular, proportions of dinitrooxydiphenylamine:
and dinitrophenol (NO.: NO₂: OH=1: 3: 4) or ortho-amido-para-nitrophenol.
2. The colouring matter manufactured as above set forth.
ABEL & IMRAY,
Agents for the Applicant.