Tris-azo Dye-stuffs.
Year: 1894

page_text: Date of Application, 15th Feb., 1894
Complete Specification Left, 14th Nov., 1894-Accepted, 15th Dec., 1894
PROVISIONAL SPECIFICATION.
Tris-azo Dye-stuffs.
I, SYDNEY PITT, of Sutton, in the County of Surrey, Gentleman, (as
communication to me from abroad by Leopold Cassella & Co., of 19 Liebig-
strasse, Frankfort-on-Main, in the Empire of Germany,) do hereby declare the
nature of this invention to be as follows:
This invention relates to the preparation of tris-azo combinations such as are
referred to in the Specifications Nos. 19330%, 69729, and 14993"
The preparation of these tris-azo combinations is set forth in the following
examples:
Example I. 20 kilos. of para-diamido-diphenylamine are diazotised, the yellow
solution of the tetrazo compound is rapidly mixed with an alkaline solution of
24 kilos. y amidonaphtolsulpho acid. The intermediate compound which is
composed of equimolecular proportions of both substances, separates immediately
in the form of a black precipitate. It is then acidulated with muriatic acid and a
solution of 7 kilos. of sodium nitrite is added. This second diazotation is
completed within 3 to 6 hours. The tetrazo-azo compound is then introduced into
an alkaline solution of 22 kilos. m. phenylenediamine. After a lapse of 12 hours
the coloring matter which separates entirely is filtered off and dried. It dyes
unmordanted cotton a deep black.
Example II. 15 kilos. of acet-para-phenylene-diamine are diazotised and
combined in alkaline solution with 24 kilos. of y amidonaphtolsulpho acid. The
acetyl-group is then split off by heating the product in aqueous solution together
with caustic soda for several hours. To the cooled solution 14 kilos. of sodium
nitrite are added and the mixture is strongly acidulated. by means of muriatic
acid. The aqueous solution of the thus produced tetrazo-azo compound shows a
red shade. As soon as a clear solution is obtained, it is allowed to run into an
alkaline solution of 23 kilos. of resorcine. The coloring matter which is
instantaneously formed is precipitated by means of common
salt. It dyes
unmordanted cotton a deep black.
By replacing phenylenediamine or resorcine in these examples with meta-
toluylenediamine, meta-amidonaphtol or their products of substitution, coloring
matters of similar properties are obtained. As it has been generally stated in
the Specification of Patent No. 6972", also in the present analogous process
the 7 amido-naphtolsulpho acid can be replaced by other amidonaphtolsulpho
acids, such as for instance the amidonaphtoldisulpho acid which according to
Patent No. 1517589 is obtained by heating beta-naphtylamine-trisulpho acid
with caustic alkalies.
Dad thin 15th day of February 1901

page_text: COMPLETE SPECIFICATION.
Tris-azo Dye-stuffs.
I, SYDNEY PITT, of Sutton, in the County of Surrey, Gentleman, (a
communication to me from abroad by Leopold Cassella & Co., of 19 Liebigstrasse,
Frankfort-on-Main, in the Empire of Germany,) 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:-
This invention relates to the preparation of tris-azo combinations such as are
referred to in the Specifications Nos. 19330, 6972, and 14993".
The preparation of these tris-azo combinations is set forth in the following
examples:
Example I. 20 kilos. of para-diamido-diphenylamine are diazotised, the yellow
solution of the tetrazo compound is rapidly mixed with an alkaline solution of
24 kilos. y amidonaphtolsulpho acid. The intermediate compound which is
composed of equimolecular proportions of both substances, separates immediately
in the form of a black precipitate. It is then acidulated with muriatic acid and
a solution of 7 kilos. of sodium nitrite is added. This second diazotation is
completed within 3 to 6 hours. The tetrazo-azo compound is then introduced
into an alkaline solution of 22 kilos. m. phenylenediamine. After a lapse of
12 hours the coloring matter which separates entirely is filtered off and dried.
dyes unmordanted cotton a deep black.
It
Example II. 15 kilos. of acet-para-phenylene-diamine are diazotised and
combined in alkaline solution with 24 kilos. of y amidonaphtolsulpho acid. The
acetyl-group is then split off by heating the product in aqueous solution together
with caustic soda for several hours. To the cooled solution 14 kilos. of sodium
nitrite are added and the mixture is strongly acidulated by means of muriatic
acid. The aqueous solution of the thus produced tetrazo-azo compound shows a
red shade. As soon as a clear solution is obtained, it is allowed to run into an
alkaline solution of 23 kilos. of resorcine. The coloring matter which is
instantaneously formed is precipitated by means of common salt. It dyes
unmordanted cotton a deep black.
By replacing phenylenediamine or resorcine in these examples with meta-
toluylenediamine, meta-amidophenol or their products of substitution, coloring
matters of similar properties are obtained. As it has been generally stated in the
Specification of Patent No. 6972", also in the present analogous process the
yamidonaphtolsulpho acid can be replaced by other amidonaphtolsulpho_acids,
such as for instance the amidonaphtoldisulpho acid which according to Patent
No. 15175 is obtained by heating beta-naphtylamine-trisulpho acid with caustic
alkalies.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. The processes herein described for the production of tris-azo dye-stuffs.
2. Producing tris-azo dye-stuffs from the diazotised combination of equi-
molecular proportions of paradiamidodiphenylamine or paraphenylenediamine with
amidonaphtolsulpho acids such as gamma-amidonaphtolsulpho acid or beta-
amidonaphtoldisulpho acid substantially as described.
3. As new products of manufacture the new coloring matters herein described.
Dated this 6th day of November 1894.
SYDNEY PITT.