IMPROVEMENTS IN TREATING QUINONS TO OBTAIN CERTAIN PRODUCTS." PROVISIONAL SPECIFICATION
Year: 1878

page_text: LETTERS PATENT to Eduard Ullrich, of the Firm Oesterreichische Alizarin-
Fabriks Gesellschaft, Przibram and Co., of Vienna, Austria, but temporarily
residing at the Cannon Street Hotel, in the City of London, for the Invention
of "IMPROVEMENTS IN TREATING QUINONS TO OBTAIN CERTAIN PRODUCTS."
PROVISIONAL SPECIFICATION left by the said Eduard Ullrich at the Office
of the Commissioners of Patents on the 31st May 1878.
EDUARD ULLRICH, of the Firm Oesterreichische Alizarin-Fabriks Gesellschaft,
Przibram and Co., of Vienna, Austria, but temporarily residing at the Cannon
Street Hotel, in the City of London. "IMPROVEMENTS IN TREATING QUINONS TO
OBTAIN CERTAIN PRODUCTS."
My Invention has for its object improvements in treating quinons to obtain
certain products.
I take a dry quinon, add to it strong sulphuric acid and saltpetre, or nitric acid;
in sufficient quantity to produce the desired degree of nitration.
'
This mixture I heat under pressure in a closed vessel until nitro-quinon is pro-.
duced. By continuing the heating process under pressure to a temperature of from
Fahrenheit dye or colouring matter is produced.
100 to 300 degrees Celsius
212
572
"
The shades of colour produced will vary according to the quantity of saltpetre or
nitric acid, the duration of the heating process, and the temperature.
In lieu of producing the dye or colouring matter direct by continuation of the
heating process, as described, the application of heat may be discontinued when'
nitro-quinon of the required strength or order is obtained. Such nitro-quinon may
Dries 71

page_text: then be precipitated, washed, and dried, and by treatment with reducing agents
corresponding amido compounds may be produced.
"
"
Fahrenheit
If these amido compounds, or the different orders or strengths of nitro-quinon,
100 to 250 degrees Celsius
be heated with strong sulphuric acid at a temperature of from 212 482
and then precipitated in water, with or without the addition of salt, the dye or
colouring matter will be isolated; or if the amido compounds or nitro-quinon be
treated with an alkali the dye or colouring matter will be neutralized.
According to the nature of the base with which the dye or colouring matter so
obtained is mixed, or the mordant with which it is brought into contact, different
colours will be produced.
By treating the dye or colouring matter with aniline, toluidine, methylaniline,
or other secondary monamines, or by infusions of radicals, such as aethyl, methyl,
acetyl, et cætera, other colour combinations will result.
SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Eduard Ullrich in the Great Seal Patent Office on the 25th
November 1878.
EDUARD ULLRICH, of the Firm Oesterreichische Alizarin-Fabriks Gesellschaft,
Przibram and Co., of Vienna, Austria, late temporarily residing at the Cannon
Street Hotel, in the City of London. "IMPROVEMENTS IN TREATING QUINONS TO
OBTAIN CERTAIN PRODUCTS."
My Invention has for its object improvements in treating quinons to obtain
certain products.
I take a dry quinon, for instance, anthra-quinon, add to it 5 to 10 parts by
weight of commercial strong sulphuric acid, and 1 to 2 parts by weight of com-
mercial saltpetre or commercial nitric acid.
This mixture I heat under pressure of 1 to 5 atmospheres in a closed vessel until
nitro anthra-quinon is produced; this will take about five hours. By continuing
the heating process for about five hours more under pressure to a temperature of
100 to 300 degrees Celsius
from
212 to 572 degrees Fahrenheit dye of colouring matter is produced.
It is not peremptory to operate under pressure; it is also possible to operate in
open caldrons, in which case the temperature is raised from 10 to 20 degrees C.
The shades of colour produced will vary according to
or nitric acid, the duration of the heating process, and
enlarging the proportions of nitric acid, on prolonging
50 to 68 degrees F.
the quantity of saltpetre
the temperature, viz., on
the time of the heating

page_text: process, and on raising the temperature, bluer tints are produced, and in the reverse
case redder tints.
In lieu of producing the dye or colouring matter direct by continuation of the
heating process, as described, the application of heat may be discontinued when
nitro anthra-quinon of the required strength or order (mono or binitro quinon) is
obtained. Such nitro anthra-quinon may then be precipitated, washed, and dried,
and by adding the reducing agents and heating, corresponding amido compounds
may be produced.
Or I prepare a solution of quinon, for instance, anthra-quinon, in strong sulphuric
acid (say to one part by weight of anthra-quinon about ten parts by weight of
sulphuric acid of 66 degrees Beaume), and add a mixture of sulphuric and nitric
acid, by preference red, forming nitric acid.
This latter mixture is to be as follows:-To one part by weight of anthra-quinon
take one part by weight of red fuming nitric acid, soluted in about double its
volume of sulphuric acid of 66 degrees Beaumé. The well-agitated mass is poured
into water, filtered, washed, and dried.
In order to amidize the nitro-product of the quinon, id est, to transform the same
into an amidine combination, it is mixed with about three to five parts by weight
of spirits of sal ammoniac, of the strongest quality to be had in commerce, in a
closed caldron, heated for about four or five hours under pressure, until an essay
taken from the caldron shews that transformation has taken place.
Another way of amidizing is as follows:-Nitro anthra-quinon or other nitro-
combinations are boiled with diluted spirits of sal ammoniac and a reducing agent,
for instance, zinc dust, in closed vessels. Care must be taken that a surplus of the
two agents be always present, the generated vapours are conducted into cold water,
so as to regain the escaping spirits of sal ammoniac.
A hydro-combination of the amido-product soluble in water is formed, which is
by preference filtered under pressure. Air is blown into the filtrated substance,
and the separated mass is filtered, washed, and dried.
122 to 482
F.'
If these amido compounds, or the different orders or strengths of nitro-anthra-
quinon, be heated with eight to ten or more parts by weight of strong sulphuric
acid at a temperature of from 50 to 250 degrees C., and then precipitated in water, with
or without the addition of salt, the dye or colouring matter will be isolated; or if
the amido compounds or nitro anthra-quinon be treated with an alkali, the dye or
colouring matter will be neutralized,
"
According to the nature of the base with which the dye or colouring matter,
obtained as herein-before described is mixed, or the mordant with which it is
brought into contact, different colours will be produced.
By treating the dye or colouring matter with aniline, toluidine, methylaniline,
or other secundary monamines, by infusions of radicals, such as aethyl, methyl,
acetyl, or by condensation by means of glycerine, or an oxalic acid, or naphtalic
acid, and sulphuric acid, et cætera, other colour combinations will result, as will be
readily understood by chemists.
Having described the nature of any said Invention, and explained the manner of
carrying it into practical effect, I hereby declare that what I consider to be novel
and original, and therefore claim as secured to me under the Letters Patent herein-
before in part recited is,―
Firstly. Producing nitro anthra-quinons in the manner and for the purposes
specified.
Secondly. Producing colouring matter by exposing nitro anthra-quinons to the
influence of heat under pressure in the manner herein-before specified.
Thirdly. Producing amido compounds of nitro anthra-quinons by means of
reducing agents, in the manner and for the purpose specified.
Fourthly. Producing colouring matter by treating amido compounds of nitro
anthra-quinons, in the manner and for the purposes described.

page_text: :
Fifthly. Producing the different shades of colouring matters by varying the base
in the treatment of amido compounds of nitro anthra-quinons in the manner above
described.
In witness whereof, I, the said Eduard Ullrich, have hereunto set my hand
and seal, this Sixteenth day of November, in the year of our Lord One 5
thousand eight hundred and seventy-eight.
EDUARD ÜLLRICH. (L.S.)