Improvements in the Manufacture of Mixed Azo Colours.
Year: 1889

page_text: Date of Application, 13th Aug., 1889
Complete Specification Left, 27th Sept., 1889-Accepted, 2nd Nov., 1839
PROVISIONAL SPECIFICATION.
[Communicated from abroad by RUPERT GREVILLE WILLIAMS, of Albany, in the
County of Albany, in the State of New York, one of the United States of
America, Manufacturer.]
Improvements in the Manufacture of Mixed Azo Colours.
I, HENRY HARINGTON LEIGH, Fel. Inst. P.A., Assoc. M. Inst. C.E., practising as
Phillips & Leigh, of 22, Southampton Buildings, Chancery Lane, W.C., in the County
of Middlesex, Engineer and Patent Agent, do hereby declare the nature of this
invention to be as follows
:-
It is well known that insoluble intermediate bodies formed by the combination of
one molecule of a tetrazo compound with one molecule of a napthylamine, or a
sulpho acid of a napthylamine, can be converted into soluble colouring matters
by reacting on them with another molecule of a different amine or with a phenol.
I have now found that a new class of intermediate bodies can be obtained by
combining one molecule of napthylene-azo-napthylamines, or sulpho acids of the
same, with one molecule of a tetrazo compound and that these intermediate bodies
can be converted into new and useful colouring matters by reacting on them with
another molecule of a phenol or amine.
of how I corzy out my process practically
Twenty-five pounds of Napthionate of Soda are dissolved in 50 gallons of water,
and 30 pounds of Muriatic Acid 22° Beaumé are added. The precipitated free
Napthionic Acid is cooled with ice and seven pounds of nitrite of soda dissolved
When the azotization is
in five times its weight of water are run slowly in.
complete, twenty-five pounds more naphthionate of soda, dissolved in 20 gallons of
water are added, and then fifteen pounds of acotate of soda. The mixture is stirred
until the molecule of free naphthionic acid is combined with the molecule of the azo-
naphthalene-sulpho acid. The reaction is complete when the whole product is trans-
formed into a clear bright scarlet solution.
The alpha-napthalene-sulpho-acid-azo-alpha-napthylamine-sulpho acid thus produced
(which is a wool dye stuff in itself) is allowed to react, in presence of acetate of soda,
on the tetrazo ditolyl formed in the usual manner by diazotizing thirty two pounds
of tolidene sulphate, or its equivalent of the base, with fourteen pounds of nitrite of
soda.
As soon as the tetrazo compound is all combined, twenty five pounds of naphthionate
of soda dissolved in about sixty gallons of water are added.
The colour is formed very slowly, and should be stirred for several days. The
completion of the reaction is ascertained when dye tests show no improvement.
The temperature is then raised to boiling point and enough soda lye added, to
convert the colour into its soda salt. It is then precipitated with common salt, filtered
off, pressed and dried.
The colour dyes unmordanted cotton a bright red in an alkaline or soap bath and
is fast to washing.

page_text: COMPLETE SPECIFICATION.
Improvements in the Manufacture of Mixed Azo Colours.
I, HENRY HARINGTON LEIGH, Fel. Inst. P.A., Assoc. M. Inst. C.E., practising as
Phillips & Leigh, of No. 22, Southampton Buildings, Chancery Lane, W.C., in the
County of Middlesex, Engineer and 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 :-.
It is well known that insoluble "intermediate" bodies formed by the combination

page_text: of one molecule of a tetrazo compound with one molecule of a naphthylamine, or a
ulpho acid of a naphthylamine, can be converted into soluble colouring matters by
eacting on them with another molecule of a different amine or with a phenol.
I have now found that a new class of intermediate bodies can be obtained by
combining one molecule of naphthalene-azo-naphthylamines, or sulpho acids of the
ame, with one molecule of a tetrazo compound, and that these intermediate bodies
can be converted into new and useful colouring matters by reacting on them with
another molecule of a phenol or amine.
nother molecule of a phenol or amine.
The following are examples
ΠΟ
entry out my process practically
EXAMPLE I.
Twenty five pounds of naphthionate of soda are dissolved in fifty gallons of water,
and thirty pounds of muriatic acid, 22° Beaumé, are added. The precipitated
free napthionic acid is cooled with ice and seven pounds of nitrite of soda dissolved
in five times its weight of water are run slowly in. When the azotization is complete,
twenty-five pounds more naphthionate of soda, dissolved in twenty gallons of water,
are added; and then fifteen pounds of acetate of soda. The mixture is stirred until
the molecule of free naphthionic acid is combined with the molecule of the azo-
naphthalene-sulpho acid. The reaction is complete when the whole. product is
transformed into a clear bright scarlet solution.
The alpha-naphthalene-sulpho-acid-azo-alpha-naphthylamine-sulpho acid thus pro-
duced (which is a wool dye-stuff in itself) is allowed to react, in presence of acetate
of soda, on the tetrazo ditolyl formed in the usual manner by diazotizing thirty two
pounds of tolidine sulphate, or its equivalent of the base, with fourteen pounds of
nitrite of soda.
As soon as the tetrazo compound is all combined, twenty five pounds of naphthionate
of soda dissolved in about sixty gallons of water are added.
The colour is formed very slowly, and the solution should be stirred for several
days.
The completion of the reaction is ascertained when dye-tests show no improvement.
The temperature is then raised to boiling point, and enough soda lye added to
convert the colour into its soda salt. It is then precipitated with common salt, filtered
off, pressed and dried.
The colour dyes unmordanted cotton a bright red in an alkaline or soap bath, and
is fast to washing.
The shade is similar to that of the colour commercially known as Benzo pur-
purine 4 B, and has the following formula :-
--

page_text: mono-sulpho-acid + orein.
The latter being combined with the intermediate in presence of an alkali. This
colour (unlike the product obtained with tetrazo ditolyl + naphthionic acid + orein)
is so soluble that it has to be precipitated out of its solution with an acid, drained off
and dried down with soda.
By tetrazo bodies I mean the following:
Tetrazo-diphenyl and its homologues.
Tetrazo-naphthalene.
Tetrazo-stilbene.
Tetrazo-fluorene.
Tetrazo-diphenolether.
Tetrazo-azo benzole and its homologues.
Tetrazo-oxy-diphenyl,
as well as the alkylized compounds or the carbo or sulpho acids of the same.
Having now particularly described and ascertained the nature of this said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is
1. The herein before described process for the production of new mixed azo colours
which process consists in combining one molecule of one of the hereinbefore
mentioned tetrazo compounds with one molecule of the hereinbefore described
naphthalene-azo-naphthylamines or sulpho acids of the same and afterwards acting
on the body thus produced with one molecule of an amine, or phenol, or sulpho acids
of an amine or phenol.
2. As a new colour-producing body, the intermediate product obtained by combining
one molecule of one of the herein before mentioned tetrazo bodies with one molecule
of naphthalene-azo-naphthylamine or its sulpho acids.
3. As new colouring matters, the dye-stuffs produced by the process herein
described.
Dated this 27th of September 1889
HENRY H. LEIGH.