The Production of Dioxynaphthaline-mono-sulpho Acid and of Disazo Dyestuffs from the same.
Year: 1890

page_text: Date of Application, 15th Jan., 1890
Complete Specification Left, 10th Oct., 1890-Accepted, 15th Nov., 1890
PROVISIONAL SPECIFICATION.
[Communicated from abroad by Messrs. DAHL AND Co., of Barmen, in the Kingdom
of Prussia, Dye Manufacturers.]
The Production of Dioxynaphthaline-mono-sulpho Acid and of
Disazo Dyestuffs from the same.
I ADOLF BANG of Park Row Leeds in the County of York, Dye Merchant,, do
hereby declare the nature of this invention to be as follows:-
If a naphthylaminedisulpho acid, whose lime salt is soluble in alcohol of 80 per cent.
absolute strength, is melted for eight to ten hours with three to four times its quantity
of caustic soda at 200° to 220° Celsius, the composition then dissolved in water and
the soda salt neutralized with hydrochloric acid until an acid reaction sets in, a dioxy-
naphthaline-mono-sulpho acid is precipitated as crystals on cooling. This acid is..
pretty difficultly soluble in water, and crystallizes out from the same in small
plates or leaves. In a solution of common sait, the soda salt is very difficultly
soluble.
With the tetrazo- compounds of benzedine, tolidine, diamido stilbene, diamido,
carbozol, dianisidin, this acid forms violet to blue disazo dyestuffs, which dye
unmordanted cotton very strongly in a weak alkaline bath.
The following example is given to illustrate the method of producing the dioxy-
naphthaline-mono-sulpho acid.
30 kilogrammes (66 lbs.) of the soda salt of a naphthylaminedisulpho acid are
introduced into a hot (about 180° C.) solution of 110 kilogrammes (242 lbs.) of
caustic soda and 20 kilogrammes (44 lbs.) of water, and the composition heated for
eight to ten hours to 200-220° (. The composition is then dissolved in about
400 litres of water, and 300 kilogrammes (660 lbs.) of hydrochloric acid of 30%
strength are gradually added. After filtering and cooling nearly all the dioxy-
naphthaline-mono-sulpho acid separates out in crystals.
The next example is given to illustrate the method of producing disazo- dye stuffs
from the above mentioned dioxynaphthaline-mono-sulpho acid.
105 kilogrammes (23 lbs.) of tolidin (or an equivalent quantity of benzedine,.
diamido-stilbene, diamido-carbozol, or dianisiin) are diazodized with 30 kilogrammes
(66 lbs.) of hydrochloric acid and 7 kilogrammes (15.4 lbs.) of sodic-nitrite, and
slowly introduced into a solution of 26 kilogrammes (57.2 lbs.) of dioxy naphthaline-
mono-sulpho acid and 40 kilogrammes (88 lbs.) of soda. After 24 hours time the
dye-stuff is completely formed, and is then filtered off, pressed and dried.
Dated this 14th day of January 1890.
J. CLARK JEFFERSON,
2, East Parade, Leeds, Agent for Applicant.
COMPLETE SPECIFICATION.
The Production of Dioxynaphthaline-mono-sulpho Acid and of
Disazo Dyestuffs from the same.
I, ADOLF BANG of Park Row Leeds in the County of York Dye Merchant, 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:
per cent.
If a naphthylamine- disulpho acid, whose lime salt is soluble in alcohol of SO
absolute strength, is melted for 8 to 10 hours with three to four times its quantity of
caustic soda at 200° to 220° Celsius, the composition theu dissolved in water and the

page_text: soda salt nextralized with hydrochloric acid until an acid reaction sets in, a dioxy-
naphthaline-mono-sulpho acid is precipitated as crystals on cooling. This acid is
pretty difficultly soluble in water, and crystallizes out from the same in small
plates or leaves. In a solution of common salt, the soda salt is very difficultly
soluble.
With the tetrazo- compounds of benzedine, tolidine, diamido-stilbene, diamido-
carbozol, dianisidin, this acid forms violet to blue disazo- lyestuffs, which dye
unmordanted cotton very strongly in a weak alkaline bath.
The following example is given to illustrate the method of producing the dioxy
naphthaline-mono-sulpho acid.
30 kilogrammes (66 lbs.) of the soda salt of a naphthylamine-disulpho acid are
introduced into a hot (abcut 180° C.) solution of 110 kilogrammes (242 lbs.) of
caustic soda and 20 kilogrammes of water, and the composition heated for 8 to 10 hours
to 200 to 220° C. The composition is then dissolved in about 400 litres of water, and
300 kilogrammes of hydrochloric acid of 30% strength are gradually added.
After filtering and cooling nearly all the dioxynaphthalins-mono-sulpho acid separates
out in crystals.
The next example is given to illustrate the method of producing disazo-dyestuffs
from the above mentioned dioxynaphthaline-mono-sulpho acid.
.10.5 kilogrammes (23 lbs.) of tolidin (or an equivalent quantity of benzidine,
diamido-stilbene diamido-carbozol or dianisidin) are diazodized with 30 kilogrammes
(66 lbs.) of hydrochloric acid and 7 kilogrammes (15.4 lbs.) of sodic nitrite, and
slowly introduced into a solution of 26 kilogrammes (57.2 lbs.) of dioxynaphthaline-
mono-sulpho acid and 40 kilogrammes (88 lbs.) of soda. After 24 hours time the
dye-stuff is completely formed, and is then filtered off, pressed and dried.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1° The production of dioxynaphthaline-mono-sulpho acid, by melting a naphtha-
line-disulpho acid with caustic soda, dissolving the composition in water, and
precipitating by means of hydrochloric acid, all substantially as herein set forth.
2° The production of disazo dyestuffs by the action of dioxynaphthaline-mono-
sulpho acid on tetrazo- compounds of benzidine, tolidine, diamido-stilbene, diamido-
carbozol, and dianisidine.
3° The use of disazo- dyestuffs, obtained according to claim 2°, for dyeing
purposes.
Dated this 9th day of Ontaban 1800