The Manufacture and Production of Colouring-matters for Cotton.
Year: 1898

page_text: Date of Application, 22nd Apr., 1898
Complete Specification Left, 19th Jan., 1899-Accepted, 25th Mar., 1899
PROVISIONAL SPECIFICATION.
The Manufacture and Production of Colouring-matters for Cotton.
1, BENJAMIN WILLCOX, of 47, Lincoln's Inn Fields, in the County of London,
Patent Agent, do hereby declare the nature of this invention, which has been com-
municated to me by the Badische Anilin and Soda Fabrik, of Ludwigshafen-on-
Rhine, in the Empire of Germany, to be as follows:-
My foreign correspondents have discovered that the violet and violet-black to
black colouring-matters, the manufacture of which is described in the Specifications
of Letters Patents N° 7766 and 20250 of the year 1896, and which are suitable for
dyeing wool, can, by heating with sodium sulphide, with or without the addition
of sulphur, be converted into violet, blue, greenish-blue and black colouring-matters,
which directly dye cotton in the cold bath.
The following examples will serve to further illustrate the nature of the inven-
tion but it is not confined to the details given in these examples. The parts are by
weight.
EXAMPLE 1-VIOLET DYESTUFF.
Heat about fifty parts of the dyestuff obtained from 11 dinitro-naphthalene, by
treating it in the manners described in the Specifications of Letters Patents
No 7766 and 20250 of the year 1896, and about five hundred parts of sodium
sulphide (containing about sixty per cent. real Na,S) for from one to two hours at
a temperature of about ninety to one hundred degrees centigrade. Then allow the
mass to cool, so that it solidifies. After breaking it up it can be directly used for
dyeing.
EXAMPLE 2 BLUE DYESTUFF.
Heat about fifty parts of the dyestuff obtained from 111 dinitro-naphthalene, by
treating it in the manners described in the Specifications of Letters Patents
N° 7766 and 20250 of the year 1896, and about five hundred parts of sodium
sulphide (containing about sixty per cent. real Na,S), and about twenty-five parts of
sulphur for from one to two hours, at a temperature of about ninety to one hundred
degrees Centigrade.
EXAMPLE 3.-GREENISH-BLUE DYESTUFF.
Heat about fifty parts of the dyestuff obtained from 11' dinitro-naphtbalene, by
treating it in the manners described in the Specifications of Letters Patents N° 7766
and 20250 of the year 1896, and about five hundred parts of sodium sulphide (con-
taining about sixty per cent. of real Na,S) and about fifty parts of sulphur for from
one to two hours at a temperature of about ninety to one hundred degrees Centi-
grade.
When in Examples 1, 2 and 3 the temperature is raised to about one hundred and
fifty to two hundred degrees Centigrade black colouring matters are obtained.....
Heat about fifty parts of the dyestuff obtained from 111 dinitro-naphthalene, by
treating it in the manners described in the Specifications of Letters Patents
N° 7766 and 20250 of the year 1896, and about five hundred parts of sodium
sulphide (containing about sixty per cent. real Na₂S), and about twenty-five parts of
sulphur for from one to two hours, at a temperature of about ninety to one hundred
degrees Centigrade.
EXAMPLE 3.-GREENISH-BLUE Dyestuff.
Heat about fifty parts of the dyestuff obtained from 11 dinitro-naphthalene, by
treating it in the manners described in the Specifications of Letters Patents N° 7766
and 20250 of the year 1896, and about five hundred parts of sodium sulphide (con-
taining about sixty per cent. of real Na,S) and about fifty parts of sulphur for from
one to two hours at a temperature of about ninety to one hundred degrees Centi-
grade.
When in Examples 1, 2 and 3 the temperature is raised to about one hundred and
fifty to two hundred degrees Centigrade black colouring matters are obtained.......

page_text: EXAMPLE 4 BLACK DYESTUFF.
Heat about fifty parts of the dyestuff obtained from a mixture of 1·11 and 1.41-
dinitro-naphthalene by treating it in the manners described in the Specifications of
Letters Patent No 20250 of the year 1896, and about five hundred parts of sodium
sulphide (containing about sixty per cent. real Na,S) and about fifty parts of sulphur 5
for from two to three hours at a temperature of about ninety to one hundred degrees
Centigrade.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.
The Manufacture and Production of Colouring-matters for Cotton.
I, BENJAMIN WILLCOX, of 47, Lincoln's Inn Fields, in the County of London,
Patent Agent, do hereby declare the nature of this invention (which has been
communicated to me from abroad by The Badische Anilin & Soda Fabrik, of
Ludwigshafen on Rhine, in the German Empire), and in what manner the same is
to be performed, to be particularly described and ascertained in and by the follow-
ing statement :-
In the Specification of Letters Patent No. 7766 of the year 1896 is described the

page_text: Heat about fifty parts of the dyestuff obtained from 1·11 dinitro-naphthalene (by
treating it in the manners described in the Specifications of Letters Patents Nos. 7766
and 20250 of the year 1896) and about five hundred parts of sodium sulphide (con-
taining about sixty per cent. of real Na,S) and about fifty parts of sulphur for from
one to two hours at a temperature of about ninety to one hundred degrees
Centigrade.
When, in Examples 1, 2 and 3, the temperature is raised to about one hundred
and fifty to two hundred degrees Centigrade, black colouring matters are obtained.
EXAMPLE 4-BLACK DYESTUFF.

page_text: Letters Patent No. 20250 of the year 1896) and about five hundred parts of sodium
sulphide (containing about sixty per cent. real Na,S) and about fifty parts of sulphur
for from two to three, hours at a temperature of about ninety to one hundred degrees
Centigrade.
The following table shews some of the characteristic reactions of these bodies :-
They separate out on the addition of hydrochloric acid to the aqueous solution, as
blue precipitates, and it is desirable to dissolve the crude melts, obtained according to
the foregoing examples, in water, and isolate the colouring matter by adding
hydrochloric acid and filtering, if it be required to preserve the product for any length
of time before use, because the colouring-matters are likely to detoriate if preserved
in the crude melt. In order to dye with the isolated colouring matters they are
dissolved in a solution of sodium sulphide.
Having now particularly described and ascertained the nature of this Inven-
tion and in what manner the same is to be performed I declare that what I
claim is
(1) The manufacture of colouring-matters (which dye cotton directly from a cold
bath) by treating the wool colouring matters hereinbefore defined with sodium
sulphide substantially as herein before described.
(2) The manufacture of colouring matters (which dye cotton directly from a cold
_bath) by treating the wool colouring matters hereinbefore defined with sodium sulphide
and sulphur substantially as hereinbefore described.
(3) The manufacture of colouring matter, substantially as hereinbefore described
in the several Examples.

page_text: (4) As new articles of manufacture, the violet-blue and greenish-blue and black
dye-stuffs, which dye cotton directly from a cold bath, such as can be obtained
substantially as hereinbefore described.
Dated this 10th day of January 1800
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London W.C., Agents.