Manufacture of Colouring Matters Dyeing Blue with Mordants.
Year: 1893

page_text: Date of Application, 4th Dec., 1893
Complete Specification Left, 4th Sept., 1894-Accepted, 6th Oct., 1894
PROVISIONAL SPECIFICATION.
[Communicated from abroad by THE ACTIEN GESELLSCHAFT FÜR ANILIN
FABRIKATION, of Berlin, in the Empire of Germany, Chemical Manu-
facturers.]
Manufacture of Colouring Matters Dyeing Blue with Mordants.
I, CHARLES DENTON ABEL of No. 28 Southampton Buildings in the County
of London, Consulting Engineer and Chartered Patent Agent, do hereby declare
the nature of this invention to be as follows:-
This invention is based on the observation that orthochinones or their sulpho-
acids and alkyl-para phenylin-diamines form condensation products, which, when
afterwards treated with sulphur and fuming sulphuric acid, yield valuable blue
colouring matters capable of forming with metallic mordants lakes which dye
beautiful fast blue tints and are especially well suited for dyeing and printing wool
and cotton, previously mordanted with chromium.
The following is given as an example of the manufacture of these colouring
matters.
13.6 kilos. dimethylparaphenylindiamine, as hydrochloric-salt, are dissolved in
100 litres of water, and while agitating 276 kilos. potassium salt of the
B, naphthachinone ẞ mono-sulpho-acid are added.
a1
The solution is rendered alkaline by means of carbonate of soda and then heated
whilst a current of air is blown through the liquid for two hours. The condensation
product formed in this way separates partly during the reaction in the form of a
dark-blue precipitate. The precipitation is completed by addition of common salt.
The product, thus obtained, is filtered off and dried. It forms a blue powder which
dissolves in water with a grey-violet colour, which is not altered by alkalies, but
changes into yellow on addition of hydrochloric-acid. Concentrated sulphuric-
acid dissolves the product forming a solution of brown yellow colour.
dyed grey.
Wool is
The transformation of this intermediate product into the blue dye-stuff may be
carried out in the following manner.
25 kilos. of the intermediate product and 12 kilos. of flowers of sulphur are
dissolved in 250 kilos. of fuming sulphuric-acid, containing about 30 per cent. of
anhydride. The mixture is well stirred for 12 hours. In order to complete the
production of the colouring matter, the sulphuric-solution is finally gently heated.
The reaction is completed as soon as a test-sample of the mixture, poured into
water and boiled, yields a bright blue liquid. The whole liquid is poured into
water and ice and the solution is heated to boiling. The precipitate is separated
by filtration and afterwards dissolved in diluted soda-solution. The solution
obtained is filtered in order to remove the sulphur and the colouring matter is then
precipitated by means of hydrochloric-acid or with common salt.
In the above described process, for the sulphur may be substituted substances
capable of forming sulphur sesquioxide when used along with fuming sulphuric-
acid.
Dated this 4th dor of December 1893
ABEL & IMRAY,
Agents for the Applicant.

page_text: Manufacture of Colouring Matters Dyeing Blue with Mordants.
I, CHARLES DENTON ABEL, of No. 28 Southampton Buildings, in the County
of London, Consulting Engineer and Chartered 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:-
This invention is based on the observation that orthoquinones or their sulpho-
acids and alkyl-paraphenylen-diamines form condensation products, which, when
afterwards heated with sulphur and fuming sulphuric acid, yield valuable blue
colouring matters, capable of forming with metallic mordants lakes, which dye
beautiful fast blue tints and are especially well suited for dyeing and printing wool
and cotton previously mordanted with chromium.
The following is given as an example of the manufacture of these colouring
matters.
13.6 kilos. dimethylparaphenylendiamine, as hydrochloric salt, are dissolved in
100 litres of water, and while agitating 27-6 kilos. potassium salt of the a ẞ, naphtho-
quinone mono-sulpho-acid are added.
The solution is kept slightly alkaline by means of carbonate of alkalies.
The condensation product formed begins to separate partly in the form of a dark
blue precipitate; and may be entirely precipitated by the addition of common salt;
in order to complete the reaction and to obtain a better yield it is suitable either to
heat the mixture slightly in the presence of air or still better to blow a current of
air through the liquid for some time.
The product, thus obtained, is filtered off and dried. It forms a blue powder
which dissolves in water with a grey violet colour, which is not altered by alkalies,
but changes into yellow on addition of hydrochloric acid. Concentrated sulphuric
acid dissolves the product forming a solution of brown yellow colour. Wool is
.dyed grey.
The transformation of this intermediate product into the blue dye-stuff may be
carried out in the following manner.
25 kilos. of the intermediate product and 12 kilos. of flowers of sulphur are
dissolved in 250 kilos. of fuming sulphuric acid, containing about 30 per cent. of
anhydride. The mixture is well stirred for about 12 hours. In order to complete
the production of the colouring matter, the sulphuric solution is finally gently
heated. The reaction is completed as soon as a test sample of the mixture, poured
into water and boiled, yields a bright blue liquid. The whole liquid is poured into
water and ice and the solution is heated to boiling. The precipitate is separated
by filtration and afterwards dissolved in diluted soda solution. The solution
obtained is filtered in order to remove the sulphur, and the colouring matter is then
precipitated by means of. hydrochloric acid or with common salt.
It produces on goods, previously mordanted with chromium, fine blue shades.
In an analogous manner the other colouring matters appertaining to this group
may be prepared.
When employing instead of quinonmonosulpho acids the quinones themselves,
practically the same result is obtained, because in these cases a sulphonation takes
place by the treatment with fuming sulphuric acid; on the other hand when
employing such quinone sulpho acids (mono- or di-) in which a sulpho group stands
in the a, position, this sulpho group is split off when the condensation to the
so called intermediate product is effected.
For the dimethyl-paraphenylendiamine in the above example may be substituted
other mono or dialkylized derivatives of paraphenylendiamine or its homologues
provided these products contain one free amido group.

page_text: Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
1. The hereinbefore described process for production of condensation products
by the action of ortho-naphthoquinone or the sulpho acids thereof upon the mono-
or dialkylised derivatives of paraphenylendiamine or its homologues containing one
free amido group.
2. The hereinbefore described process for the transformation of the products
obtained as set forth in the preceding claim into blue mordant dyeing colouring
matters by heating these products with sulphur in the presence of fuming sulphuric
acid.
3. The condensation products manufactured as set forth in Claim 1.
4. The colouring matters manufactured as set forth in Claims 1 and 2.
Dated this 4th day of September 1891
ABEL & IMRAY,
Agents for the Applicant.