Manufacture of Colouring Matters of the Induline Series...
Year: 1894

page_text: Date of Application, 18th Oct., 1894
Complete Specification Left, 5th July, 1895-Accepted, 10th Aug., 1895
TRUVIDIONAL DIBUITUATION.
[Communicated from abroad by THE ACTIEN GESELLSCHAFT FÜR ANILIN
FABRIKATION, of Berlin, in the Empire of Germany, Chemical Manu-
facturers.]
Manufacture of Colouring Matters of the Induline Series...
J, CHARLES DENTON ABEL, of No. 28 Sonthampton Buildings, Chancery
Lane, in the County of London, Consulting Engineer and Chartered Patent Agent,
do hereby declare the nature of this invention to be as follows :—
This invention relates to the manufacture of colouring matters of the induline
series, which dye clear and fast tints on cotton mordanted with tannin and tartar
emetic. The production of the colouring matters is based on the following
reactions.
The unsymmetrical alkylised p-phenylendiamines or toluylendiamines, may with
diphenylamine, methyldiphenylamine and their homologues be combined to form
indamines by oxidation in acid solution. These indamines may be oxidised in
presence of a primary amine to blue violet colouring matters, easily soluble in
water and of great tinctorial power.
The following example illustrates the manufacture of these colouring matters.
19-2 kilos. of the hydrochlorate of nitroso-dimethylaniline are suspended in
750 litres of alcohol and, while actively stirring, 20 kilos. of zinc dust and 55 kilos.
of hydrochloric acid are added. When the reduction is complete, 17 kilos. of
diphenylamine and 4 kilos. of hydrochloric acid are added and the cold solution is
oxidised by a solution of 20 kilos. of crystallised sodium bichromate in 100 litres
of water.
The reaction product obtained is stirred for an hour, then heated to 70° C., and
mixed with a concentrated solution of 19 kilos. of chloride of aniline and 4 kilos. of
hydrochloric acid (20° Bé.); to this mixture is added a solution of 20 kilos. of
sodium bichromate in 150 litres of water. The blue reaction product thus prepared
is poured into about its equal volume of water and precipitated with common
salt.
The colouring matter and the chromium oxide precipitated are filtered off; the
colouring matter is dissolved in boiling water, filtered and precipitated by means of
common salt.
The dyestuff is easily soluble in water, it dyes tanned cotton in bright blue violet
tints, resisting the influence of alkalies acids and light.
In the above example for the p-amido dimethylaniline may be substituted other
unsymmetrical mono- or di-alkylised p-diamines or their sulpho acids; also for the
diphenylamine may be substituted methyl-diphenylamine or its homologues.
For the aniline may be substituted other primary amines of the aromatic series
or derivatives of such amines. For instance p-toluidine yields a dyestuff which
dyes nearly the same tints but the zinc chloride double salt of which is less soluble
and has greater tendency to crystallise.
Dated this 18th day of October 1894.
ABEL & IMRAY,
Agents for the Applicant.

page_text: CUMLELE
Manufacture of Colouring Matters of the Induline Series.
I, CHARLES DENTON ABEL, of No. 28 Southampton Buildings, in the County
of London, Consulting Engineer and Chartered Patent Agent, 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 manufacture of colouring matters of the induline
series which dye clear and fast tints on cotton mordanted with tannin and tartar
emetic. The production of the colouring matters is based on the following
-reactions.
By joint oxidation in acid solution the unsymmetrical alkylised p.-pheny-
lenediamines or toluylenediamines may be combined with secondary amines such as
diphenylamine to form so called "indamines"; on further oxidation in presence
of primary amines these indamines yield violet to blue colouring matters easily
soluble in water and of a great tinctorial power.
The following example illustrates the manufacture of these colouring matters.
19-2 kilos. of the hydrochlorate of nitrosodimethylaniline are suspended in
750 litres of alcohol, and while actively stirring, 20 kilos. of zinc dust and 55 kilos.
of hydrochloric acid are added. When the reduction is complete, 17 kilos. of
diphenylamine and 4 kilos. of hydrochloric acid are added and the cold solution
is oxidised by a solution of 20 kilos. of crystallised sodium bichromate in 100 litres
of water.
The reaction product obtained is stirred for an hour then heated to 70° C., and
mixed with a concentrated solution of 19 kilos. of chloride of aniline and 11 kilos.
of hydrochloric acid (20° Bé.); to this mixture is added a solution of 20 kilos. of
sodium bichromate in 150 litres of water. The blue reaction product thus
prepared is poured into about its equal volume of water and precipitated with
common salt.
The colouring matter and the chromium oxide precipitated are filtered off;
the colouring matter is dissolved in boiling water, filtered and precipitated by
means of common salt.
The dyestuff is easily soluble in water, it dyes tanned cotton in bright blue violet
tints, resisting the influence of alkalies acids and light.
In the above example for the p. amido dimethylaniline may be substituted other
uusyrametrical mono- or di-alkylised p-diamines or their sulpho acids; also for the
diphenylamine may be substituted its homologues.
For the aniline may be substituted other primary amines of the aromatic series
or derivatives of such amines. For instance p-toluidine yields a dyestuff which
dyes nearly the same tints but the zinc chloride double salt of which is less soluble
and has greater tendency to crystallise.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what I
claim is :-
1. The herein described manufacture of colouring matters of the induline series
by joint oxidation of primary amines and such indamines, as are formed by
oxidising unsymmetrical alkylised paraphenylenediamines or para-tuluylene-
diamines with diphenylamine or its homologues.
2. The colouring matters manufactured as above set forth.
Dated this 5th day of July 1805
ABEL & IMRAY,
Agents for Applicant.