Improvement in the Manufacture of Black Colouring Matters.
Year: 1899

page_text: Date of Application, 13th Dec., 1899
Complete Specification Left, 10th Jan., 1900-Accepted, 10th Feb.,
1900
PROVISIONAL SPECIFICATION.
Improvement in the Manufacture of Black Colouring Matters.
WILLIAM HENRY CLAUS and ALFRED REE, Chemical Manufacturers, both of
Clayton, Manchester, and LEON MARCHLEWSKI, Research Chemist, of Clayton,
Manchester, do hereby declare the nature of this invention to be as follows;-
In our British Patent Application 1070999 we described a colouring matter
obtained by heating o-hydroxydinitrodiphenylamine with sulphur and sodium
sulphide. We have now found that another black colouring matter is formed
if the said o-hydroxydinitrodiphenylamine is heated together with an equimole-
cular proportion of para-amidophenol with sulphur and sodium sulphide. In
order to illustrate the working of our invention, the following example is
given:-
27.5 parts of o-hydroxydinitrodiphenylamine (obtained by condensing o-amido-
phenol with 1.2.4. chlordinitrobenzene) and 11 parts of p-amidophenol are heated
with 77 parts of sulphur and 230 parts of crystallised sodium sulphide at first
to a temperature of about 110°, and then at 140-150°, or higher. There is
obtained a black mass, which may be used, after crushing, for dyeing cotton
without a mordant. The shades obtained may be made fast to washing and light
by an after-treatment with oxidising agents-such as bichromate of potash in
presence of sulphuric acid, or by a treatment with copper salts.
Dated this 11th day of December 1899.
WILLIAM HENRY CLAUS.
ALFRED REE.
LEON MARCHLEWSKI.
Improvement in the Manufacture of Black Colouring Matters.
WILLIAM HENRY CLAUS and ALFRED REE, both Chemical Manufacturers, of
Clayton, Manchester, and LEON MARCHLEWSKI, Chemist, of Clayton, Manchester,
do hereby declare the nature of this invention and in what manner the same is
to be performed, to be particularly described and ascertained in and by the
following statement;
In our British Patent Application 1070999, we described a colouring matter
obtained by heating o-hydroxydinitrodiphenylamine with sodium sulphide and
sulphur. We have now found that another black colouring matter is formed
if the said o-hydroxydinitrodiphenylamine is heated together with an equimole-
cular proportion of para-amidophenol with sulphur and sodium sulphide.

page_text: In order to illustrate the working of our invention, the following example is
given:
27.5 parts of o-hydroxydinitrodiphenylamine (obtained by condensing o-amido-
phenol with 1:2:4 chlordinitrobenzene) and 11 parts of p-amidophenol are heated
with 77 parts of sulphur and 230 parts of crystallised sodium sulphide for 3
hours at a temperature of about 80° C. gradually increasing the temperature
to 140° C. and maintaining the temperature at 1400 to 160° C. for 5 hours. The
resulting black mass is ready for use. It dissolves with a dark blue colouration
in water and dyes cotton in deep black shades in one bath.
Having now particularly described and ascertained the nature of our said
invention, and in what manner the same is to be performed, we declare that what
we claim is;
-
The manufacture of a black colouring matter by heating with sodium sulphide
and sulphur a mixture of equimolecular proportions of o-hydroxydinitrodiphenyl-
amine and p-amidophenol, substantially in the manner hereinbefore described.
Dated this 6th day of January 1900.
WILLIAM HENRY CLAUS,
ALFRED RÉE.
LEON MARCHLEWSKI.
WILLIAM HENRY CLAUS,
ALFRED RÉE.
LEON MARCHLEWSKI,