The Manufacture or Production of New Dye-stuffs of the Diphenylnaphthylmethane Series.
Year: 1899

page_text: Date of Application, 12th Apr., 1099
Complete Specification Left, 11th Jan., 1900-Accepted, 17th Feb., 1900
Date of Application, 12th Apr.
Complete Specification Left, 11th Jan., 1900-Accepted, 17th Feb., 1900
[Communicated from abroad by THE FARBENFABRIKEN vormals FRIEDRICH
BAYER & Co., of Elberfeld, Germany.]
The Manufacture or Production of New Dye-stuffs 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:-
In the Specification of Letters Patent No. 23392 93, my foreign correspondents
described the production of basic dye-stuffs which are obtained, for instance, by
condensing tetraalkylated diamidobenzo-phenones with para-alky-loxy-phenyl-
alphanaphylamines in the presence of phosphorus oxychloride.
My foreign correspondents have now found that, by treating these basic dye-
stuffs with sulphonating agents, very valuable pure blue coloring matters are
obtained, which dye unmordanted wool, in acid baths, very clear and even shades
fast to alkalies.
:
In order to illustrate the production of these new dye-stuffs, the following
example is given, the parts being by weight.
EXAMPLE.
20 parts of the dyestuff obtainable by condensing tetramethyl-diamido benzo-
phenone with para-ethoxy-phenyl-alpha-naphtylamine, in the presence of phos-
phorus oxychloride, are carefully dried and pulverized, and then stirred into
140 parts of fuming sulphuric acid (containing 13 per cent. of SO₁), the tem-
perature being kept between zero and 10 degrees Centigrade. Stirring is continued
at the ordinary temperature, until a diluted test portion of the reaction mixture is
found to be soluble in ammonia. When this stage is reached, the reaction liquid
is poured on ice. The resulting mixture is heated to about 50 to 60 degrees
Centigrade, and then neutralized with sodium carbonate, by means of which
operation the sodium salt of the new sulphonic acid is separated in the shape of a
resinous precipitate, which soon becomes transformed into a crystalline mass.
The new dyestuff thus obtained is isolated by filtration. If necessary, it can be
further purified in the manner known and in use for the purification of such
dye-stuffs.
The new coloring matter, when dry and pulverized, is a dark powder having
a bronze-like lustre. It is easily soluble in water, and dyes wool, in acid baths,
beautiful clear and level blue shades.
Similar dye-stuffs are obtained if, instead of the condensation product prepared
from tetramethyl-diamido-benzophenone and para-ethoxy-phenyl-alphanaphtyl-
amine, other of the above mentioned basic dye-stuffs are used in the foregoing
example.
My foreign correspondents do not intend to confine themselves to the particulars

page_text: given in this example, which is merely, typical, as they can be varied within
wide limits.
NEWTON & SON,
Agents for the Applicant,
The Manufacture or Production of New Dye-stuffs 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 and in what manner the same is to be performed to be
particularly described and ascertained in and by the following statement:-
-
In the Specification of Letters Patent No. 2339293, my foreign correspondents
described the production of basic dye-stuffs which are obtained, for instance, by
condensing tetraalkylated diamido benzo-phenones with para-alkyloxy-phenyl-
alpha-naphthylamines in the presence of phosphorus oxychloride.
My foreign correspondents have now found that, by treating these basic dye-
stuffs with sulphonating agents, very valuable pure blue coloring matters are
obtained, which dye unmordanted wool, in acid baths, very clear and even shades
fast to alkalies.
In order to illustrate the production of these new dye-stuffs, the following
example is given, the parts being by weight,
EXAMPLE.
20 parts of the dyestuff obtainable by condensing tetramethyl-diamido-benzo-
phenone with para-ethoxy-phenyl-alpha-naphthylamine, in the presence of phos
phorus oxychloride, are carefully dried and pulverized, and then stirred into
140 parts of fuming sulphuric acid (containing 13 per cent. of SO), the tem-
perature being kept between zero and 10 degrees Centigrade. Stirring is continued
at the ordinary temperature, until a diluted test portion of the reaction mixture is
found to be soluble in ammonia. When this stage is reached, the reaction liquid
is poured on ice. The resulting mixture is heated to about 50 to 60 degrees
Centigrade, and then neutralized with sodium carbonate, by means of which
operation the sodium salt of the new sulphonic acid is separated in the shape of a
resinous precipitate, which soon beconies transformed into a crystalline mass.
The new dyestuff thus obtained is isolated by filtration. If necessary, it can be
further purified in the mauner known and in use for the purification of such
dye-stuffs.
The new coloring matter, when dry and pulverized, is a dark powder having
a bronze-like lustre. It is soluble in water, and dyes wool, in acid baths,
beautifully clear and even blue shades.
Similar dye-stuffs are obtained if, instead of the condensation product prepared
from tetramethyl-diamido benzophenone and para-ethoxyphenylalphanaphthyl-
amine, other of the above mentioned basic dye-stuffs are used in the foregoing
example.
My foreign correspondents do not intend to confine themselves to the particulars
given in this example, which is merely typical, as they can be varied within
wide limits.
Having now particularly described and ascertained the nature of the said

page_text: invention and in what manner the same is to be performed, as communicated to
me from abroad, I declare that what I claim is:-
1. The production of blue dye-stuff sulphonic acids from coloring matters
obtainable by condensing paraalky-loxy-phenyl-alpha-naphthylamine (such as
para-methoxyphenyl-alpha-naphthylamine,
para-ethoxyphenyl-alpha-naphthyl-
amine, or the like) with tetra-alkylated diamido-benzophenones, in the presence
of phosphorus oxychloride, which process consists in treating the above defined
products with sulphonating agents, substantially as hereinbefore described.
2. As new articles of manufacture, the new blue dye-stuffs for wool obtainable
by the process hereinbefore defined.
NEWTON & SON,
Agents for the Applicant.