Year: 1896

page_text: Date of Application, 10th Apr. 1890
Complete Specification Left, 7th Jan., 1897-Accepted, 10th Apr., 1897
vate
7050
Complete Specification Left, 7th Jan., 1897-Accepted, 10th Apr., 1897

page_text: Step 2. The solution of the mononitrosodioxy R salt from step 1, is made alkaline,
for example by the addition of 17 kilos. of sodium carbonate, and then a solution of
diazo benzene, obtained by diazotising 9-3 kilos. of aniline in the usual manner, is
allowed to run in while stirring. The new nitroso-azo colouring matter is formed
after a few hours, and may be salted out, filtered and pressed.
It dyes wool, in an acid bath, brown; chrome mordanted fibres, a dark brown.
These colours are fast to light and to milling and possess other valuable properties.
If, for the diazo-benzene in Example II, step 2, the diazo compound of
a naphthylamine, ß naphthylamine, or amido naphthol sulpho acid y is substituted,
the following colouring matters result:-
We do not confine ourselves to the shades or to the materials and processes herein-
before described and we may, by way of example, substitute for the paranitraniline
or a naphthylamine, other suitable amido compounds, and in place of the dioxy
acid R, other suitable dioxynaphthalene sulpho acids or dioxynaphthalenes may be
used, as for example, dioxynaphthalene mono-sulpho acid G, a, a, dioxynaphthalene-
ag-monosulpho acid, or a₁ a dioxynaphthalene-ß, Ba-disulpho acid, and the like.
Dated this 9th day of April A.D. 1896.
W. E. HEYS & SON,
Agents for the Applicants.
Manufacture or Production of New Colouring Matters.
We, LEVINSTEIN LIMITED and IVAN LEVINSTEIN both of Minshull Street
Manchester in the County of Lancaster, Chemical Manufacturers, 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 :-
Nitroso-azo colouring matters of the dioxy bodies of the benzene series only, are
so far known and have hitherto been obtained by the action of nitrous acid on
resorcinol azo colours. (See the Specification of German Letters Patent No. 46479.)
We have however succeeded in producing corresponding nitroso-azo colouring
matters of dioxy bodies and dioxy sulphonic acids of the naphthalene series.
In the production of these new colouring matters according to our present
invention, we may proceed either by way of treating the mono-azo colours of the
dioxy bodies with nitrous acid, as hereinafter described under Example I, or by
treating the dioxy bodies first with nitrous acid and then by combining the thus
obtained mononitroso-oxy bodies with diazo bodies as described hereinafter under
Example II. The resulting nitroso-azo dye-stuffs possess the advantage that they

page_text: are capable of not only dyeing animal fibres in an acid bath, but also the further
valuable property of forming lakes with metallic salts, which lakes are fast to light.
and to milling. They are therefore valuable and applicable to the arts of dyeing and!
of printing.
The shades of colour produced may be varied by employing different mordants
and different amines.
EXAMPLE I.
140 kilos. of paranitraniline are diazotised in the well known manner and combined,.
in a bath consisting of a weak acetic acid solution, with 26-2 kilos. of the sodium.
salt of dioxynaphthalene monosulpho acid R. When the combination is completed,
a red colouring matter is found to have been formed. A solution of 7-5. kilos. of
sodium nitrite is then added, and the whole mixture is allowed to flow slowly into:
30 kilos. of hydrochloric acid 20° Bé., diluted with water, taking care to cool the acid
solution by ice or otherwise. The mixture is well stirred for about 12 hours, at the
end of which time the reaction is completed.
The new nitroso-azo colour thus produced and which to a large extent is in
solution, is precipitated by common salt. It dyes chrome mordanted fibres in shades.
varying from yellow to brown, which are fast to light and to milling. It possesses:
also other valuable properties.
EXAMPLE II.
Step 1. Production of the nitroso-dioxy R salt.
26-2 kilos. of the sodium salt of dioxynaphthalene mono-sulpho acid R, are
dissolved in about 500 litres of water. This solution is acidified with 30 kilos. of
commercial hydrochloric acid 18° Bé., is well cooled with ice, and has then added to
it a solution of 7.2 kilos. of sodium nitrite. The whole is stirred and the reaction is
completed within a short time, the resulting product being the mono-nitroso-dioxy R
salt, which remains in solution.
Step 2. The solution of the mononitroso-dioxy R salt from step 1, is made
alkaline, for instance by the addition of 17-0 kilos. of sodium carbonate, and then a
solution of diazobenzene obtained by diazotising 9-3 kilos. of aniline in the usual
manner, is allowed to run in whilst stirring. The new nitroso-azo colouring matter
is formed after a few hours and may be salted out, filtered and pressed. It dyes wool,
in an acid bath, brown; chrome mordanted fibres, a dark brown. These colours
are fast to light and to milling and possess other valuable properties.
If, for the diazobenzene in Example II, step 2, the diazo compound of alpha-
naphthylamine, heta-naphthylamine, or amidonaphthol sulpho acid gamma, is
substituted, the following colouring matters result:-

page_text: the alpha-naphthylamine, other suitable amido compounds; and, in place of the
dioxy acid R, other suitable dioxy-naphthalene sulpho acids or dioxynaphthalenes
may be used, as for example, dioxynaphthalene mono-sulpho acid G, alpha,-alpba-
dioxypaphthalene alpha,-mono-sulpbo acid, or alpha,-alpha,-dioxynaphthalene beta
betag-disulphonic acid, and the like.
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 hereinbefore described process for the manufacture or production of
nitroso-azo colouring matters of the naphthalene series which consists in treating
monazo colours of the dioxy bodies of the naphthalene series with nitrous acid,
substantially as set forth.
2. The hereinbefore described process for the manufacture or production of
nitroso-azo colouring matters of the naphthalene series which consists in treating
monazo colours of the dioxy bodies of the naphthalene series with nitrous acid and
in combining the product with diazo colours, substantially as set forth.
3. As new substances, the new nitroso-azo colouring matters of the naphthalene
series produced substantially as and by the processes herein before described."
Dated this 6th day of January A.D. 1897.
W. E. HEYS & SON,
Agents for the Applicants.