Manufacture of New Violet 'Monoazo Dyestuffs for Wool, Dyeing a Fast Brown by Oxidation with Chrome.
Year: 1896

page_text: Date of Application, 19th Oct., 1896
Complete Specification Left 21st June, 1897--Accepted, 31st July, 1897
PROVISIONAL SPECIFICATION.
Manufacture of New Violet 'Monoazo Dyestuffs for Wool, Dyeing a
Fast Brown by Oxidation with Chrome.
I, OLIVER IMRAY, 6f No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention (as cominunicated to me from abroad by The Farbwerke vormals:
Meister Lucius and 'Brüning of Hoechst a/Main, in the Empire of Germany,
Chemical Manufacturers) to be as follows:-
Hitherto no azo dyestuffs of any technical, value have been obtained from diazotisęd
amido-naphthol sulphonic acids.
My foreign correspondents have found that such dyestuffs may be obtained
from 1:8 diazo naphthol sulphonic acids on the one hand and alpha-naphthylamine
or its alkyl- and alphyl-derivatives, respectively, on the other hand.
These dyestuffs are of great interest on account of their great fastness to light; on
treatment with chromates or chromic acid on the fibre they produce brown, powerful
tints of special fastness to milling and light and they dye evenly when applied. to
loose wool.
"The new dyestuffs may be obtained by employing diazotised amidonaphthol-
sulphonic acids such for instance as 'diazotised amido-naphthol disulphonic acid H,
diazotised amido naphthol monosulphonic acid S, diazotised ainidonaphthol
monosulphonic acid 18. 5, 'diazotised amidonnaphthol monosulphonic acid 1.8. 3,
diazotised amidonaphthol :monosulphonic acid 1-86.
Any of these is allowed to act upon the hydrochloride of alpha-naphthylamine.or
its derivatives, in the presence or absence of acetates, according as the combination
takes place more or less readily; or the amine is dissolved in a little alcohol and then
combined with the diazo compound.
EXAMPLE.
2.39.kilos of 1.8 amidonaphthol-4-sulphonic.acid.are, together, with 0-42 kilos. of
caustic soda, dissolved in about 90 litres of water; 0.69 kilos. sodium, nitrite, dissolved
in a little water are added and the solution.kept cold is allowed to run into 40 kilos. of
ice-cold diluted hydrochloric acid containing 0.92. kilos. of the acid, the solution being
well stirred.
The diazonaphtholsulphonic acid separates out, at once as a yellow', brown
precipitate; 1.43 kilos. alpha-naphthylamine are dissolved in 30 litres of hot, water and
the calculated quantity of hydrochloric acid, the solution is cooled down to about 25°C.
by the addition of ice and the diazo compound is allowed, to, run in ; 3' kilos of
crystallised sodium acetate are added, whereupon the formation of: the dyestuff,
soluble with difficulty, begins. After several hours stirring and, gradual heating up
to 80° C., the combination is complete.
By the addition of a solution of 2.2 kilos. of soda and subsequent heating, 'the
dyestuff is transformed into the sodium salt. "This, in dry condition, is a green black
powder of metallic lustre, soluble with difficulty in cold water,. more easily in hot
wator with a red violet colour.

page_text: By the addition of some common salt, a brown precipitate is obtained from this
solution.
The dyestuff dyes wool violet in an acid bath and on treatment with chromates or
chromic acid an even saturated brown of beautiful shade is obtained, which is fast to
milling and light.
ABEL & IMRAY,
Agents for the Applicant.
Manufacture of New Violet Monoazo Dyestuffs for Wool, Dyeing a
Fast Brown by Oxidation with Chrome.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention (as communicated to me from abroad by The Farbwerke vormals:
Meister Lucius and Brüning of Hoechst a/Main, in the Empire of Germany,
Chemical Manufactures,) and in what manner the same is to be performed to be
particularly described and ascertained in and by the following statement :-
Hitherto no azo dyestuffs of any technical value have been obtained from diazotised
amido-naphthol sulphonic acids.
My foreign correspondents have found that such dyestuffs may be obtained
from 1: 8 diazo naphthol sulphonic acids on the one hand and alpha-naphthylamine
or its alkyl-and alphyl-derivatives, respectively, on the other hand.
These dyestuffs are of great interest on account of their great fastness to light; on
- treatment with chromates or chromic acid on the fibre they produce brown, powerful
. tints of special fastness to milling and light and they dye evenly when applied to
loose wool.
The new dyestuffs may be obtained by employing diazotised amidonaphthol
sulphonic acids such for instance as diazotised amido naphthol disulphonic acid H,
diazotised amido naphthol monosulphonic acid S diazotised amido naphthol
monosulphonic acid 1. 8. 5, diazotised amido naphthol monosulphonic acid 1. 8. 3,
diazotised amidonaphthol monosulphonic acid 1. 8. 6, diazotised amido-naphthol
monosulphonic acid 1. 8. 7.
Any of these is allowed to act upon the hydrochloride of alpha-naphthylamine, in
the presence or absence of acetates, according as the combination takes place more or
less readily; or the amine is dissolved in a little alcohol and then combined with the
diazo compound.
EXAMPLE.
2.39 kilos. of 18 amidonaphthol-4-sulphonic acid are, together with 0.42 kilos. of
caustic soda, dissolved in about 90 litres of water; 0.69 kilos. sodium nitrite dissolved
in a little water are added and the solution kept cold is allowed to run into 40 kilos.
of ice-cold diluted hydrochloric acid containing 0.92 kilos. of the acid, the solution.
being well stirred.
The diazonaphthol sulphonic acid separates out at once as a yellow brown
precipitate; 1-43 kilos. alpha-naphthylamine are dissolved in 30 litres of hot water and
the calculated quantity of hydrochloric acid, the solution is cooled down to about 25° C.
by the addition of ice and the diazo compound is allowed to run in ; 3 kilos. of
crystallised sodium acetate are added, whereupon the formation of the dyestuff,
soluble with difficulty, begins. After several hours stirring and gradual heating up
to 80° C., the combination is complete.

page_text: By the addition of a solution of 2.2 kilos. of soda and subsequent heating, the
dyestuff is transformed into the sodium salt. This, in dry condition, is a green black
powder of metallic lustre, soluble with difficulty in cold water, more easily in hot
water, with a red violet colour.
By the addition of some common salt, a brown precipitate is obtained from this
solution.
.The dyestuff dyes wool violet in an acid bath and on treatment with chromates or
chromic acid an even saturated brown of beautiful shade is obtained, which is fast to
milling and light.
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 :-
The herein described manufacture of new violet monoazo dyestuffs by allowing
1:8 diazonaphthol sulphonic acids to act upon alpha-naphthylamine in an acid solution.
Dated this 21st day of June 1897.
ABEL & IMRAY,
Agents for the Applicant.