Manufacture of a Sulphurised Black Dyestuff.
Year: 1899

page_text: Date of Application, 7th Sept., 1899
Complete Specification Left. 5th June, 1900-Accented 7th July 1900
Date UIApplication, 7th Dept., 1899
Complete Specification Left. 5th June 1900-Accented 7th July 1900
PROVISIONAL SPECIFICATION.
Manufacture of a Sulphurised Black Dyestuff.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention, (as communicated to me from abroad by The Farbwerke vormals
Meister Lucius & Brüning, of Hoechst a/Main, in the Empire of Germany,
Chemical Manufacturers) to be as follows:-
My foreign correspondents, in their Specification No. 24,538 of 1898, have shewn
that, by heating the condensation product of para-amidophenol and nitrochloro-
benzenesulphonic acid with sulphur and a sulphide of an alkali metal, various
dyestuffs may be obtained according to the temperature, those obtained at a low
temperature being blue and those obtained at a higher temperature being black.
Similar results are obtained with the homologous condensation product from
para-amidocresol and nitrochlorobenzenesulphonic acid, as in this case also a
dyestuff is obtained at a low temperature different from that obtained at a high
temperature; that obtained at a low temperature is of a grey-violet and apparently
inferior, whilst that obtained at a high temperature is black and of considerable
importance on account of the beauty of its shade and its tinctorial power.
MANUFACTURE OF THE CONDENSATION PRODUCT PARA-OXY-META-METHYL-PARA-
NITRODIPHENYLAMINE-ORTHO SULPHONIC ACID OR PARA OXY-META-METHYL-
PARA AMIDODIPHENYLAMINE-ORTHO-SULPHONIC ACID.
1 molecular proportion of sodium nitrochlorobenzenesulphonate is heated with
1 molecular proportion of para-amidocresol, 1 molecular proportion of sodium
acetate and 4 litres of water in a closed vessel for 6 hours to 120° C. A red-
brown solution is obtained from which the nitro-compound is precipitated by
common salt in the form of reddish-brown crystalline needles. To obtain the
amido-compound the solution is at once further operated on, that is to say it is
reduced with iron and acetic acid. After reduction the iron is precipitated with
sodium carbonate the liquid is filtered and again acidified, when the amido-com-
pound is separated in the form of white needles; it is soluble with difficulty in
water.
MANUFACTURE OF THE DYESTUFF.
The nitro-compound as well as the amido-compound may be employed to manu
facture the black dyestuff.
As an example one part by weight of the amido-compound, for instance, is intro-
duced into a molten mixture of I part by weight of sulphur and 3 parts by weight
of sodium sulphide and the whole is heated for several hours to 180° C. and
afterwards for 3 or 4 hours to 240° C.
The product is a porous mass, being, when pulverised, a black powder, easily
soluble in water to a violet-black solution, and directly dyeing cotton a deep black.
Dated this 7th day of September 1899.
ABEL & IMRAY,
Agents for the Applicant.

page_text: COMPLETE
SPECIFICATION.
Manufacture of a Sulphurised Black Dyestuff.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention (as communicated to me from abroad by The Farbwerke vormals
Meister Lucius & Brüning, of Hoechst a/Main, in the Empire of Germany,
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 correspondents, in their Specification No. 24,538 of 1898, have shewn
that, by heating the condensation product of para-amidophenol and nitrochloro-
benzenesulphonic acid with sulphur and a sulphide of an alkali metal, various
dyestuffs may be obtained according to the temperature those obtained at a low
temperature being blue and those obtained at a higher temperature being black:
Similar results are obtained with the homologous condensation product from
para-amidocresol and nitrochlorobenzenesulphonic acid,, as in this case also a
yestuff is obtained at a low temperature different from that obtained at a high
temperature; that obtained at a low temperature is of a grey-violet and apparently
inferior, whilst that obtained at a high temperature is black and of considerable
importance on account of the beauty of its shade and its tinctorial power.
MANUFACTURE OF THE CONDENSATION PRODUCT PARA-OXY-META-METHYL-PARA-
NITRODIPHENYLAMINE-ORTHO-SULPHONIC ACID OR PARA-OXY-META-METHYL-
PARA-AMIDODIPHENYLAMINE-ORTHO-SULPHONIC ACID.
1 molecular proportion of sodium nitrochlorobenzenesulphonate is heated with
1 molecular proportion of para-amidocresol, 1 molecular proportion of sodium
acetate and 4 litres of water in a closed vessel for 6 hours to 120° C. A red-
brown solution is obtained from which the nitro-compound is precipitated by
common salt in the form of reddish-brown crystalline needles. To obtain the
amido-compound the solution is at once further operated on, that is to say it is
reduced with iron and acetic acid. After reduction the iron is precipitated with
sodium carbonate the liquid is filtered and again acidified, when the amido com-
pound is separated in the form of white needles; it is soluble with difficulty in
water.
MANUFACTURE OF THE DYESTUFF.
The nitro-compound as well as the amido-compound may be employed to manu-
facture the black dyestuff.
As an example one part by weight of the amido-compound, for instance, is intro-
duced into a molten mixture of 1 part by weight of sulphur and 3 parts by weight
of sodium sulphide and the whole is heated for several hours to 180° C. and
afterwards for 3 or 4 hours to 240° C.
The product is a porous mass, being, when pulverised, a black powder, easily
soluble in water to a violet-black solution, and directly dyeing cotton a deep black.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is:
The herein described manufacture of a sulphurised black dyestuff by heating at
a high temperature para-oxy-meta-methyl-para-amidodiphenylamine-ortho-sul-
phonic acid or para-oxy-meta-methyl-para-nitrodiphenylamine-ortho-sulphonic
acid with sulphur and sulphides of alkali metals.
Dated this 5th day of June 1900.
ABEL & IMRAY,
Agents for the Applicant.