Manufacture of Blue Basic Dyestuffs Soluble in Water.
Year: 1899

page_text: Date of Application, 25th Jan., 1899
Complete Specification Left, 21st Sept., 1899-Accepted, 21st Oct.,
1899
PROVISIONAL SPECIFICATION.
Manufacture of Blue Basic Dyestuffs Soluble in Water.
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 and Brüning, of Hoechst a/Main, in the Empire of Germany, Chemical
Manufacturers,) to be as follows:―
In the German Patents Nos. 85932, 91721, 92015 and 95483 has been described a
series of peculiar blue dyestuffs more or less soluble in water, which are obtained by
combining a diazotised safranine with naphthol, molecular quantities of both com-
ponents being employed.
My foreign correspondents have found, that, by combining diazotised safranine
with B-naphthol, valuable blue dyestuffs soluble in water may be obtained, if 2 mole-
cules of a diazotised safranine and 1 molecule of ẞ-naphthol are employed in a
neutral, slightly acid or ammoniacal solution. The products thus obtained are
distinguished from those of the patents above mentioned by their ready solubility
and superior pureness of tint.
The safranines here referred to are phenosafranine and its homologues, known in
the market under various names, such as, safranine "G extra," safranine "H N extra,"
safranine concentrated, safranine "G G S," safranine "B" safranine "T" etc.
The following examples illustrates the process:-
14 kilos. of safranine "G extra" (0.04 mol.) are dissolved in water and diazotised
with 9 kilos. of hydrochloric acid (20° Bé.) and 2.76 kilos. of sodium nitrite (100%)
in the usual manner while being cooled with ice. On completion of the diazotation
there is run into the diazosolution while stirring rapidly a solution of 3 kilos.
of B-naphthol (0.02 mol.) in 4 kilos. of soda-lye (specific gravity 1.437) and
50 to 100 litres of water. After 12 to 24 hours the formation of the dyestuff is
complete; the solution is heated to 70° or 80° C. and filtered if necessary. The
dyestuff is then salted out with common salt, collected on a filter, washed with a
solution of common salt, pressed and dried.
In this case the formation of the dyestuff takes place in a neutral solution ;
the following example illustrates the process employing an acid solution.
14 kilos. of safranine "G extra" (0.04 mol.) are diazotised in the manner above
described. On completion of the diazotation, a solution of 7.5 kilos. of sodium acetate
is added and while stirring rapidly a solution of 3 kilos. of ẞ-naphthol (0.02 mol.) in
2 kilos. of soda-lye (specific gravity 1.437) and 50 to 100 litres of water is run in.
The process is completed as in the first example.
If the reaction is to take place in an ammoniacal solution, there is added to the
excess of sal-ammoniac or
alkaline B-naphthol solution in the first example an
ammonia sulphate.
The dyestuff obtained by the above examples is readily and completely soluble in
water with a blue violet colour and dyes cotton, unmordanted and mordanted with
tarter emetic, as well as wool and half wool a fast blue.

page_text: Instead of safranine "G extra," equivalent quantities of others of the safranines
mentioned above may be employed and the dyestuffs thus obtained differ little from
those produced as above described.
ABEL & IMRAY,
Agents for the Applicant,
Manufacture of Blue Basic Dyestuffs Soluble in Water.
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 and Brüning, of Hoechst a/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:-
In the Gerinan Patents Nos. 85932, 91721, 92015 and 95483 has been described a
series of peculiar blue dyestuffs more or less soluble in water, which are obtained by
combining a diazotised safranine with naphthol, molecular quantities of both com-
ponents being employed.
My foreign correspondents have found, that, by combining diazotised safranine with
B-naphthol, valuable blue dyestuffs soluble in water may be obtained, if 2 molecular
proportions of a diazotised safranine and 1 molecular proportion of B-naphthol are
employed in a neutral, slightly acid or ammoniacal solution. The products thus
obtained are distinguished from those of the patents above mentioned by their
ready solubility and superior pureness of tint.
The safranines here referred to are phenosafranine and its homologues, known in
the market under various names, such as, safranine "G extra," safranine "HN extra,"
safranine concentrated, safranine "GGS," safranine "B," safranine "T" etc.
The following example illustrates the process.
14 kilos. of safranine "G extra" (0.04 mol.) are dissolved in water and diazotised
with 9 kilos. of hydrochloric acid (20 Bé. specific gravity) and 2.76 kilos. of sodium
nitrite (100 per cent. strength) in the usual manner while being cooled with ice. On
completion of the diazotisation there is run into the diazo-solution while stirring
rapidly a solution of 3 kilos. of B-naphthol (0.02 mol.) in 4 kilos. of soda-lye (specific
gravity 1.437) and 50 to 100 litres of water. After 12 to 24 hours the formation of
the dyestuff is complete; the solution is heated to 70° or 80° C. and filtered if
necessary. The dyestuff is then salted out with common salt collected on a filter,
washed with a solution of common salt, pressed and dried.
In this case the formation of the dyestuff takes place in a neutral solution; the
following example illustrates the process employing an acid solution.
14 kilos. of safrauine "G extra" (0.04 mol.) are diazotised in the manner above
described. On completion of the diazotisation, a solution of 7.5 kilos. of sodium
acetate is added and while stirring rapidly a solution of 3 kilos. of ẞ-naphthol
(0.02 mol.) in 2 kilos. of soda-lye (specific gravity 1.437) and 50 to 100 litres of water
is run in. The process completed as in the first example.
If the reaction is to take place in an ammoniacal solution, there is added to the
B-naphthol solution in an excess of alkali an excess of sal-ammoniac or ammonium
sulphate.
The dyestuff obtained by the above examples is readily and completely soluble in
water to a blue violet solution and dyes cotton, unmordanted and mordanted with
tartar emetic as well as wool and half wool a fast blue.

page_text: Instead of safranine "G extra," equivalent quantities of others of the safranines
mentioned above may be employed and the dyestuffs thus obtained differ little from
those produced as above described.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, declare that what I
claim is:-
1. The herein described manufacture of blue, basic dyestuffs soluble in water by
combining 1 molecular proportion of beta-naphthol with 2 molecular proportions of
a diazotised safranine in neutral acid or ammoniacal solution.
2. The dyestuffs manufactured as above set forth.