The Manufacture or Production of New Dyestuffs of the Diphenylnaphthylmethane Series.
Year: 1899

page_text: ABRIKEN VOTH
TRIEDRICH DAYER
& Co., of Elberfeld, Germany.]
The Manufacture or Production of New Dyestuffs of the
Diphenylnaphthylmethane Series.
I, HENRY EDWARD NEWTON, of The Office for Patents, 6, Bream's Buildings,
Chancery Lane, in the County of London, Patent Agent, do hereby declare the nature
of this invention to be as follows :-
My foreign correspondents have found that valuable new dye-stuffs, capable of
5 dyeing wool, in acid baths, blue shades, are obtained if basic dye-stuffs of the so-
called "Victoria blue" series, having the general formula-

page_text: pulverised, and stirred into 120 kilos. of fuming sulphuric acid (containing 7.3 per
cent. of SO3), the temperature being kept at about zero. To the solution thus
produced, 165 kilos. of fuming sulphuric acid (containing 70 per cent. of SO,) are
added at the same temperature. The mixture thus obtained is allowed to stand for
some time (during which time the temperature may rise to about 15° Centigrade),
until a diluted test portion of the reaction mixture is found to be completely soluble
in alkalies. The mixture is then immediately poured on ice, and is neutralized with
sodium carbonate, by means of which operation the dyestuff is precipitated. Finally,
the dyestuff is isolated by filtration. It can be further purified in the known manner
by dissolving the same in hot water, and precipitating again from the resulting
solution, by the addition of common salt.
EXAMPLE B.
20 kilos. of the dyestuff obtainable by condensing tetra methyl diamido benzo-
phenone with para tolyl alphanaphthylamine, are dissolved in 100 kilos. of sulphuric
acid mono hydrate, whilst being cooled and stirred. To the solution thus produced,
30 kilos. of fuming sulphuric acid (containing 70 per cent. of SO,) are added while
continuously stirring, the temperature being kept below zero. The mixture thus
obtained is allowed to stand for some time at from 0° to 5° Centigrade, until a test
portion poured into water dissolves completely in hot dilute alkalies. Subsequently
the reaction mixture is poured on ice, and the dye-stuff sulphonic acid is isolated
therefrom in the manner described in the foregoing example.
EXAMPLE C.
25 kilos. of the dyestuff obtainable by condensing tetra methyl diamido benzophe-
none with ethyl-alphanaphthylamine, are stirred into 75 kilos. offfuming sulphuric
acid (containing 22 per cent. of SO3), the temperature being kept below zero.
Subsequently, to this mixture 25 kilos. of fuming sulphuric acid (containing 75 per
cent. of SO,) are slowly added at the same temperature. The reaction inass is
allowed to stand until the sulphonation is finished, whilst the temperature may rise
up to 15° Centigrade. The separation of the dye-stuff sulphonic acid is performed
in a manner analogous to that described in the above Example A.
The colouring matters obtainable according to the above examples represent brown
powders.
They are easily soluble in water with a blue color, and dye wool, in acid baths,
very clear and even blue shades.
My foreign correspondents do not intend to confine themselves to the particulars
given in these examples, as these are merely typical, and can be varied within wide
limits.
Dated this 20th day of I... 1000
NEWTON & SON,
Agents for the Applicant.
The Manufacture or Production of New Dyestuffs of the
Diphenyluaphthylmethane Series.
I, HENRY EDWARD NEWTON, of the Office for Patents, 6, Bream's Buildings,
Chancery Lane, in the County of London, Patent Agent, do hereby declare the 45
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 :-
My foreign correspondents have found that valuable new dye-stuffs, capable of

page_text: dyeing wool, in acid baths, blue shades, are obtained, if basic dyestuffs of the so-called
"Victoria blue" series, having the general formula-
20 kilos. of the carefully dried dye-stuff obtainable by condensing tetramethyl-
diamidobenzophenone with phenylalphanaphthylamine ("Victoria blue B") are well
pulverized and stirred into 125 kilos. sulphuric acid monohydrate, at the ordinary
temperature. To the solution thus produced, which is previously cooled down to
about 4 degrees below zero, Centigrade, from 32 to 36 kilos. of fuming sulphuric acid
(containing 70 per cent. of SO,) are added. The mixture thus obtained is allowed to
stand (while standing, the temperature must not be allowed to rise above zero) until
a diluted test portion of the reaction mixture is found to be completely soluble in
water and in alkalies. The mixture is then immediately poured on ice, and is neutralized
with sodium carbonate, by means of which operation the dye-stuff is precipitated.
Finally, the dye-stuff is isolated by filtration. It can be further purified in the known
manner, by dissolving the same in hot water, and precipitating again from the
resulting solution, by the addition of common salt.
EXAMPLE B.
20 kilos. of the carefully dried and pulverized dye-stuff obtainable by condensing
tetramethyl diamidobenzophenone with paratolylalphanaphthylamine, are dissolved
in 100 kilos. of sulphuric acid monohydrate, whilst being cooled and stirred. To the
solution thus produced, 36 kilos. of fuming sulphuric acid (containing 70 per cent.
of SO,) are added, with continuous stirring, the temperature being kept below zero.
The mixture thus obtained is allowed to stand for some time, at from 0° to 5º Centi-
grade, until a test portion poured into water, dissolves completely in hot dilute
alkalies. Subsequently, the reaction mixture is poured on ice, and the dye-stuff
sulphonic acid is isolated therefrom in the manner described in the foregoing
example.

page_text: (containing 22 per cent. of SO₁), the temperature being kept below zero
Subsequently, to this mixture 25 kilos. of fuming sulphuric acid (containing
75 per cent. of SO3) are slowly added at the same temperature. The reaction mass is
allowed to stand until the sulphonation is finished, whilst the temperature may rise
up to 15° Centigrade. The separation of the dye-stuff sulphonic acid is performed in
a manner analogous to that described in the above Example A.
The coloring matters obtainable according to the above examples, represent brown
powders.
They are easily soluble in water, with a blue color, and dye wool, in acid baths,
very clear and even blue shades.
My foreign correspondents do not intend to confine themselves to the particulars
given in the above examples, as these are merely typical, and can be varied within
wide limits.
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
ine from abroad, I declare that what I claim is :---
1. The process for the production of new blue acid dye-stuffs, which process
consists in treating with sulphonating agents, the basic dye-stuffs of the so-called
"Victoria blue" series, having the general formula-