Manufacture of Black, Substantive, Sulphurised Dyestuffs.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
Manufacture of Black, Substantive, Sulphurised Dyestuffs.
I, JOHN IMRAY, 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
La Société Anonyme des Matieres Colorantes et Produits Chimiques de St. Denis,
of 10, Rue Lafayette, Paris, France, Manufacturers) to be as follows:-
My foreign correspondents find that new, black, substantive dyestuffs, of much
importance in dyeing cotton are obtainable by melting with sulphur alone or with
sulphur and sodium sulphide, certain dyestuffs of the indophenol group or of the
indoaniline group. These dyestuffs, which form the raw material for the dye-
stuffs manufactured as herein set forth, are made in the known manner by
oxidising a mixture of paraphenylenediamine or paramidophenol on the one hand
with phenols or naphthols on the other hand; these easily prepared dyestuff's
are then treated in the known manner as in the following example.
EXAMPLE.
Into 15 kilos. of melted sulphur kept at a temperature of about 130° to 140° C.,
are introduced 10 kilos. of the dyestuff prepared from paraphenylenediamine
and a - naphthol, and the mass is heated for four hours, the temperature being
gradually raised to about 200° C.
There is thus obtained a friable, brittle mass which is pulverised and intro-
duced in small portions at a time into from 60 to 80 kilos. of crystallised sodium
sulphide previously fused and evaporated to a syrupy consistency.
Equally well, after having allowed the mass to cool, the sodium sulphide may
be added and heated gradually. When once melted, the sodium sulphide
dissolves little by little the product formed, and there is obtained a pasty mass
which is then heated to about 200° C. to 250° C.; energetic reaction ensues
and the mass then slowly dries becoming hard and brittle in which condition
it is suitable for use.
In this example for the dyestuff mentioned may be substituted any other
dyestuff's belonging to the indophenol group or indoaniline group, and the pro-
portion of sulphur and sodium sulphide. as well as the temperature and the
duration of heating may be varied without sensibly modifying the dyestuffs
obtained.
Dated thin 7th dor of April 1899
ABEL & IMRAY.
Agents for the Applicant.

page_text: Manufacture of Black, Substantive, Sulphurised Dyestuffs.
I, JOHN IMRAY, 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
La Société Anonyme des Matieres Colorantes et Produits Chimiques de St. Denis,
of 10, Rue Lafayette, Paris, France, 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 find that new, black, substantive dyestuffs, of much
importance in dyeing cotton are obtainable by melting with sulphur alone or with
sulphur and sodium sulphide, certain dyestuffs of the indophenol group or of the
indoaniline group. These dyestuffs, which form the raw material for the dye-
stuffs manufactured as herein set forth, are made in the known manner by
oxidising a mixture of paraphenylenediamine or paramidophenol on the one hand
with phenols or naphthols on the other hand; these easily prepared dyestuffs
are then treated in the known manner as in the following example.
EXAMPLE.
Into 15 kilos. of melted sulphur kept at a temperature of about 130° to 140° C.,
are introduced 10 kilos. of the dyestuff prepared from paraphenylenediamine
and a - naphthol, and the mass is heated for four hours, the temperature being
gradually raised to about 200° C.
There is thus obtained a friable, brittle mass which is pulverised and intro-
duced in small portions at a time into from 60 to 80 kilos. of crystallised sodium
sulphide previously fused and evaporated to a syrupy consistence.
Equally well, after having allowed the mass to cool, the sodium sulphide may
be added and heated gradually. When once melted the sodium sulphide
dissolves little by little the product formed, and there is obtained a pasty mass
which is then heated to about 200° to 250° C.; energetic reaction ensues
and the mass then slowly dries becoming hard and brittle in which condition
it is suitable for use.
In this example for the dyestuff mentioned may be substituted any other
dyestuffs belonging to the indophenol group or indoaniline group. and the pro-
portion of sulphur and sodium sulphide. as well as the temperature and the
duration of heating may be varied without sensibly modifying the dyestuffs
obtained.
Having now particularly described and ascertained the nature of this
invention, and in what manner the same is to be performed, I declare that what
I claim is:
-
1. The herein described manufacture of black substantive sulphurised dye-
stuffs by heating with sulphur and then with sodium sulphide colouring matters
of the indophenol or indoaniline group.
2. The dyestuffs manufactured as above set forth.