Production or Manufacture of Black Colouring Matters.
Year: 1899

page_text: Date of Application, 23rd May, 1899
Complete Specification Left, 10th Jan., 1900-Accepted, 10th Feb., 1969
Production or Manufacture of Black Colouring Matters.
WILLIAM HENRY CLAUS and ALFRED RÉE, Chemical Manufacturers, both of Clayton,
Manchester, and LEON MARCHLEWSKI, of Clayton aforesaid, Chemist, do hereby
declare the nature of this invention to be as follows:-
1
Our discovery relates to the production of black colouring matters by heating with
sulphur and sodium sulphide of certain diphenylaminederivatives, namely: 1, of
trinitro-p-bydroxydiphenylamine, obtained by condensing pierylchloride with
p-amidophenol, 2, of trinitro-o-hydroxydiphenylamine obtained by condensing
picrylchloride with o-amidophenol 3, of a mixture of the two above mentioned
trinitro-hydroxydiphenylamines 4, of dinitro-o-hydroxydiphenylamine, obtained by
condensing o-amidophenol with dinitro-chlorbenzol of the constition Cl: NO₂: NO₂
= 1:24. 5, of homologues of any one of the above mentioned diphenyl
aminederivatives. The following example will explain the carrying out of our
invention: trinitro-p-hydroxydiphenylamine is heated gradually with 2 parts of
sulphur and 5 parts of crystallised sodium sulphide to 150° C., when after some time a
colouring matter is obtained which dyes cotton jet black.
Dated this day the 23rd May 1800
Production or Manufacture of Black Colouring Matters.
WILLIAM HENRY CLAUS and ALFRED RÉE, 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:—
Our discovery relates to the production of black colouring matters, by heating with
sulphur and sodium sulphide certain diphenylamine derivatives, namely:
1. Trinitro-para-hydroxydiphenylamine, obtained by condensing picrylchloride
with p. amido phenol.
2. Trinitro-ortho-hydroxydiphenylamine, obtained by condensing picrylchloride
with o. amido-phenol.
3. A mixture of the two mentioned trinitro-hydroxydiphenylamine derivatives.
4. Dinitro-o-hydroxydiphenylamine, obtained by condensing o-amido-phenol with
dinitrochlorbenzol, of the constitution (Cl: NO₂: NO₁ = 1:2:4).

page_text: The following example will explain the carrying out of our invention:
One part of trinitro-para-hydroxydiphenylamine is heated with 6 parts of
crystallised sodium sulphide for 3 hours at 80° to 100° C.; two parts of sulphur are
now added and the temperature slowly raised to 140° C.; the temperature is
maintained at 140° to 150° C. for 4 to 5 hours. The resulting colour is a black
brittle mass, soluble in water with a bluish-black coloration, which dyes cotton deep
jet black in one bath. The shades thus obtained may be made more permanent by
an after-treatment with bichromate of soda or sulphate of copper.
Having now particularly described and ascertained the nature of our said inven-
tion, and in what manner the same is to be performed, we declare that what we
claim is
1. The production of black colouring matters by heating with sodium sulphide and
sulphur (a) trinitro-para-hydroxydiphenylamine; (b) trinitro-ortho-hydroxydiphenyl-
amine; (c) a mixture of these trinitro-hydroxydiphenylamines; (d) dinitro-ortho-
hydroxydiphenylamine, substantially as described.
2. The black colouring matters hereinbefore described.
WILLIAM HENRY CLAUS.
ALFRED RÉE.
LEON MARCHLEWSKI.