Improvements in the Manufacture of Colouring Matters.
Year: 1895

page_text: Date of Application, 10th Jan., 1895
Complete Specification Left, 16th Sept., 1895-Accepted, 19th Oct., 1895
[Communicated from abroad by K. JOEHLER, of Offenbach-on-the-Maine, in the
Empire of Germany, Manufacturer.]
Improvements in the Manufacture of Colouring Matters.
1, HENRY HARRIS LAKE, of the Firm of Haseltine, Lake & Co., Patent Agents,
do hereby declare the nature of this invention to be as follows:-
My invention consists in the production of new brown azo dye stuffs dyeing
N N. at least 8 times in a
unmordanted cotton and containing the azo group
-
-
molecule.
The communicator has found that 2 molecules of the Bismarck brown-sulpho-
acids obtained by the process described in the Specification of former Letters
Patent No. 11000 can be combined with 1 molecule diazotized diamido-naphthaline-
disulpho-acid to form an intermediate dye stuff which can be further combined with
2 molecules of a diazotized aromatic-amido-sulpho-acid.
The before named Bismarck brown-sulpho-acids are the intermediate compounds
from toluylene-diamine-sulpho-acid and two molecules meta-phenylene-diamine or
meta-toluylene-diamine. And the above mentioned diamido-ẞ naphthaline-
disulpho-acid is that acid, which is obtained by dinitrizing or reducing ẞ₁ ẞ3
naphthaline-disulpho-acid.
As example of the method of proceeding I describe the production of the dye
stuff from diamido-ẞ-naphthaline-disulpho-acid-Bismarck-brown-sulpho-acid and
naphtionic-acid :
8 parts by weight of diamido-ẞ-naphthaline-disulpho-acid are suspended in
200 parts of water, mixed with 11 parts of hydrochloric acid of 20° B. and
diazotized by pouring in a solution of 3.5 parts of nitrite of soda in 8 parts of
water. The tetrazo compound thus obtained is poured, while stirring, into a
solution of 23.1 parts of the dye stuff obtained by the method described in the said
former Patent No. 1100089 Example II, from i molecule tetrazotized toluylene-
diamine-sulpho-acid of Schwanert and 2 molecules of meta-phenylene-diamine
dissolved in 500 parts of water and 20 parts of soda.
The formation of the intermediate dye stuff begins at once and is finished after
24 hours. The diazo-naphthaline-sulpho-acid obtained from 12.3 parts of naphtionate
of soda, 20 parts of hydrochloric acid of 20° B., 3.5 parts of nitrite of soda and
the necessary quantity of water, is allowed to run into the former solution and is
boiled after 24 hours standing; the final dye stuff is precipitated by salt, pressed
and dried.
This dye stuff forms a black-brown powder, 'soluble in concentrated sulphuric acid
with a violet-brown colour, which turns into yellow brown by the addition of water.
It dyes unmordanted cotton in an alkaline soap-bath deep chestnut-brown, which
shows a remarkable resistance against soaping. In the above process, the meta-
phenylene-ẞ diamine can be replaced by meta-toluylene diamine and the naphtionic
acid by amido-sulpho-acids for example: sulphonil-acid, ß naphthylamine-sulpho-
acid or others.

page_text: The colouring matters thus obtained dye cotton as follows:
Diamido acid + 2BBS + 2 diazo-sulphonil-acid == chestnut-brown.
+2 diazo-ß-naphthylamine-sulpho acid =
"
"
+
"
"
+
"
وو
brown.
+ 2 diazo-amidoazobenzol-sulpho acid
Diamido-acid + 2BBST + 2 diazo-naphtionic acid
(BB S
=
BBST
=
-
yellow-
= red-brown.
yellow-brown.
combination of toluylene-diamine-sulpho-acid + 2 mol. meta-
phenylene-diamine."
toluylene-diamine-sulpho-acid + 2 mol, meta-toluylene-diamine.)
Dated this 10th day of Januar 100%
improvements in the Manufacture of Colouring Matters.
I, HENRY HARRIS LAKE, of the Firm of Haseltine, Lake & Co. Patent Agents,
45 Southampton Buildings, in the County of Middlesex, 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:-
The invention consists in the production of new brown azo-dyestuffs dyeing
unmordanted cotton and containing the azo-group - NN at least eight times
in a molecule.
-
The communicator has found that two molecules of the Bismarck-brown-sulpho-
acids, obtained by the process described in the Specification of former Letters
Patent No. 11000 of 1889 can be combined with one molecule diazotized diamido-
beta-naphthalene-disulpho-acid to form an intermediate dyestuff which can be
further combined with two molecules of a diazotized aromatic amido-sulpho-acid.
The before mentioned Bismarck-brown-sulpho-acids, are the intermediate com-
pounds from toluylene-diamine-sulpho-acid and two molecules meta-phenylene-
diamine or meta-toluylene-diamine. And the mentioned diamido-ẞ-naphthalene-
di-sulpho-acid is that acid which is obtained by dinitrizing or reducing B₁-ß-
naphthalene-di-sulpho-acid.
As example of the method of proceeding I describe the production of the
dye-stuff from di-amido-6-naphthalene-disulpho-acid, Bismarck brown-sulpho-acid
and naphthionic acid; the parts being by weight. Eight parts of diamido-ẞ-
naphthalene-di-sulpho-acid are suspended in 200 litres of water mixed with 11 parts
of hydrochloric-acid of 20° Bé. and diazotized by pouring in a solution of 3-5 parts
of nitrite of soda in 8 parts of water. The tetrazo-compound thus obtained is
poured, while stirring, into a solution of 23.1 parts of the dyestuff obtained by the
method described in the said former Patent No. 11000 of 1889. Example II from
1 molecule of tetrazotized toluylene-diamine-sulpho-acid of Schwanert and
2 molecules of meta-phenylene-di-amine dissolved in 500 parts of water and 20 parts
of soda.
The formation of the intermediate dye-stuff begins at once and is finished
after 24 hours. The diazo-naphthalene-sulpho-acid obtained from 12.3 parts of
napthionate of soda, 20 parts of hydrochloric acid of 20° Bé., 3.5 parts nitrite of
soda and the necessary quantity of water, is allowed to run into the former solution
and is boiled after 24 hours standing; the final dyestuff is precipitated by salt
pressed and dried.
This dyestuff forms a black brown powder, soluble in concentrated sulphuric acid
with a violet-brown colour, which turns into yellow brown by the addition of water.
It dyes unmordanted cotton in an alkaline soap bath deep chestnut-brown which

page_text: phenylene-diamine can be replaced by meta-toluylene-diamine and the naphthionic
cid by amido-sulpho-acids for example: sulphanil-acid, ẞ-naphthylamine-sulpho-
acid or others.
The colouring matters thus obtained dye cotton as follows:
Diamido-acid + 2 B BS + 2 diazo-sulphanil-acid
"
"3
"
وو
دو
== chestnut-brown.
=
+2 diazo-ß-naphthylamine-sulpho-acid: yellow-
brown.
==
+ 2 diazo-amido-benzol-sulpho-acid = red-brown.
+ 2BBST + 2 diazo-naphthionic-acid = yellow-brown.
BBS combination of toluylene-diamine-sulpho-acid + 2 mol. of meta.
phenylene-diamine."
=====
BBST
=
toluylene-diamine-sulpho-acid + 2 mol. of meta-toluylene-diamine.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, as communicated to me by my
foreign correspondent, I declare that what I claim is :-
1. The method of producing new brown azo dye-stuffs dyeing unmordanted
cotton and consisting in the subsequent combination of the Bismarck-brown-sulpho-
acids (obtained by the method described in the Specification of former Patent
No. 11000 of 1889) with one molecule diazotized diamido-ß-naphthalene-di-sulpho-
acid and then with two molecules of an aromatic diazo-sulpho-acid as for instance:
diazotized sulphanil acid, naphthionic acid, B-naphthylamine-sulpho-acid, amido-
azo-benzol-sulpho-acid and others.
2. As new articles of manufacture the new brown azo dye stuffs obtained by the
process described in the first claim and having the properties described.
Dad: 10th of Contember 1805
HASELTINE, LAKE & Co.,
45 Southampton Buildings, London, W.C., Agents for the Applicant.