Manufacture of Blue Mordant, Dyestuffs of the Anthraquinone Series.
Year: 1899

page_text: Date of Application, 15th Dec., 1899
Complete Specification Left, 12th Sept., 1900-Accepted, 24th Nov., 1900
PROVISIONAL SPECIFICATION.
Manufacture of Blue Mordant, Dyestuffs of the Anthraquinone Series.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, 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 & Brüning, of Hoechst /Main, in the Empire of Germany,
Chemical Manufacturers,) to be as follows:-
It is known that the practically valueless products of the void German Patent
No. 6526 are transformed according to the process of the German Patent
No. 75,490 by heating them with dilute alkalies or with the hydroxides of
alkaline earths under moderate pressure into blue-dyeing mordant dyestuffs
soluble in water, which possess colouring properties essentially superior to those
of the raw materials.
My foreign correspondents have found that pure mordant dyestuffs, similar to
anthracene blue, may be obtained, if the products obtained according to the void
German Patent No. 6526 be heated under pressure according to the method
described in the said patent, with dilute alkalies or alkaline earths, or still better
in form of their lime-lakes, with aqueous alkalies, with or without addition of a
suitable oxidising agent, such, for instance, as saltpetre, till they become in-
soluble in water. Besides the elimination of sulphonic groups a substitution of
amido-groups by the hydroxyl takes place, ammonia being formed.
EXAMPLE.
In a closed vessel provided with an agitator 100 grams of the product obtained
according to the void German Patent No. 6526 are introduced into 3. litres of
water to which are added 50 grams of burnt lime, best in the form of milk of
lime, and 100 grams of sodium hydroxide, and the whole is heated for about
20 hours to about 180° C.
To this mass about 20 grams of saltpetre may be added.
The insoluble lime-lake thus formed after being washed is treated in a boiling
state with dilute hydrochloric acid and the eliminated hexa-oxyanthraquinones
are freed by filtration and washing from the small portion of sulphonic acid
remaining unattacked, they are identical with the sulphonic acids obtained
according to the German Patent No. 104,750.
ABEL & IMRAY,
Agents for the Applicant.

page_text: Manufacture of Blue Mordant Dyestuffe of the Anthraquinone Series.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, in the
County of London, Chartered l'atent Agent, do hereby declare the nature of
this invention (as communicated to me from abroad by The Farbwerke vormals
Meister Lucius & Brüning, of Hoechst /Main, in the Empire of Germany,
Chemical Manufacturers) and in what manner the same is to be performed to
be particularly described and ascertained in and by the following statement:-
It is known that the practically valueless products obtained according to
German Patent No. 6526 are transformed according to the process of the German
Patent No. 75490 by heating them with dilute alkalies or with the hydroxides of
alkaline earths under moderate pressure into blue-dyeing mordant dyestuffs
soluble in water, which possess colouring properties essentially superior to those
of the raw materials.
My foreign correspondents have found that pure mordant dyestuffs, similar to
anthracene blue, may be obtained, if the products obtained according to the
German Patent No. 6526 be heated under pressure according to the method
described in the said Patent No. 75490, with dilute alkalies or alkaline earths, or
still better in form of their lime lakes with aqueous alkalies, with or without
addition of a suitable oxidising agent, such, for instance, as saltpetre, till they
become insoluble in water. Besides the elimination of sulphonic groups a
substitution of amido-groups by the hydroxyl occurs, ammonia being formed.
EXAMPLE.
In a closed vessel provided with an agitator 100 grams of the product
obtained according to the German Patent No. 6526 are introduced into 3 litres
of water to which are added 50 grams of lime, best in the form of milk of lime,
and 100 grams of sodium hydroxide, and the whole is heated for about 20 hours
to about 180° C.
To this mass about 20 grams of saltpetre may be added before the heating
operation.
Test portions are taken from time to time and heated with hydrochloric acid
to see whether the insoluble dyestuff is formed. In this the process differs from
that described in German Patent No. 104,750 according to which an insoluble
lime-lake is likewise formed, but which when decomposed with hydrochloric
acid produces a soluble dyestuff.
The insoluble lime-like thus formed after being washed is treated in a boiling
state with dilute hydrochloric acid and the eliminated hexa-oxyanthraquinones
are freed by filtration and washing from the small portion of sulphonic acids
remaining unattacked; these sulphonic acids are identical with the sulphonic
acids obtained according to the German Patent No. 104,750.
By dissolving, for instance, these hexa-oxyanthraquinones in the usual manner
in a solution of dilute sodium carbonate or alkali or by washing them with
sulphuric acid, a pure blue-dyeing mordant dyestuff is obtained having the
properties of the known hexaoxyanthraquinones.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is
1. The herein described manufacture of a blue mordant dyestuff by heating
sulphonic acids, obtained as described in German Patent No. 6526 by the action

page_text: of fuming sulphuric acid on dinitroanthraquinone or its products of reduction,
with aqueous alkalies or alkaline earths, with or without addition of an oxidising
agent and under pressure or not, till a test portion of the insoluble lime-lake
obtained yields when decomposed with hydrochloric acid the insoluble dyestuff.
2. The blue dyestuff manufactured as above set forth.
Dated this 12th day of September 1900.
ABEL & IMRAY,
Agents for the Applicant.