The Manufacture of a Blueish Red Dye belonging to the Rosinduline Series.
Year: 1894

page_text: Date of Application, 5th Feb.. 1894
Complete Specification Left, 5th Nov., 1894-4ccepted, 8th Dec.. 1894
PROVISIONAL SPECIFICATION.
The Manufacture of a Blueish Red Dye belonging to the
Rosinduline Series.
We READ HOLLIDAY & SONS LIMITED of Upperhead Row, Huddersfield, in
the County of York, Manufacturing Chemists, and KARL BERNHARD ELBEL,
Ph. D. of Huddersfield aforesaid, Chemist in the employment of the said Read
Holliday & Sons Limited do hereby declare the nature of this invention to be as
follows:-
This invention relates to the manufacture of a blueish red dye belonging to the
rosinduline series.
The alpha naphtoldisulphonate of soda of the Specification of Letters Patent
granted to the said Read Holliday & Sons, Thomas Holliday and Paul Robert
Emmanuel Seidler, dated the 21st of March 1891, No. 5103, forms on treatment
with nitrite and acetic acid at various temperatures a nitroso-alpha-naphtol-
disulphonate of soda of characteristic properties. It forms fine orange red needles
or leaflets which are difficultly soluble in water. It yields when treated with
ammonia under pressure the corresponding nitrosonaphtylamine derivative.
On heating either the nitroso-alpha-naphtoldisulphonate or the nitroso-alpha-
naphtylaminedisulphonate with three times their weight of aniline and the equal
weight of aniline salt to a temperature between 140° and 160° Centigrade for
6 to 8 hours a red melt is formed, from which the excess of aniline is removed
either by distillation with an excess of caustic soda or by extraction with hydro-
chloric acid. In the first case the colour separates out of the remaining liquor
after all the aniline is driven off. In the other case the residue of the extraction
is dissolved in hot water and caustic soda, after having been filtered and washed
with water. From this solution the new compound is precipitated by an excess of
caustic soda or by addition of common salt. It forms red leaflets with a yellow
metallic lustre. Being too insoluble in water it cannot be very well employed as a
dye without resulphonating. For this purpose the recrystallized sulphonate is
decomposed by hydrochloric acid in a solution or fine suspension in hot water.
It is then
The precipitated free sulpho acid is filtered, washed, pressed and dried.
ground finely and dissolved in twice its weight of sulphuric acid of 66° Bé. The
sulphonation is complete after 12 hours standing at ordinary temperature or after
an hour's heating up to 50°. The sulphonation melt is then run into cold water.
The new sulpho acid separates from the red acid liquor, is filtered and washed with
some salt water. It is then dissolved in hot water and caustic soda.
temperature of about 80° to 90° a small quantity of common salt or an excess of
caustic soda precipitates the sodium salt as crystalline powder, which is filtered,
pressed and dried. The new body dyes wool in an acid bath a blueish red shade
of great fastness to light and milling.
Dated the 5th day of February 1894.
At a

page_text: i
The Manufacture of a Blueish Red Dye belonging to the
Rosinduline Series.
We READ HOLLIDAY & SONS LIMITED, of Upperhead Row, Huddersfield, in
the County of York, Manufacturing Chemists, and KARL BERNHARD ELBEL,
Ph. D. of Huddersfield aforesaid, Chemist in the employment of the said Read
Holliday & Sons Limited 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 relates to the manufacture of a blueisli red dye belonging to the
rosinduline series.
The alpha naphtoldisulphonate of soda of the Specification of Letters Patent
granted to the said Read Holliday & Sons, Thomas Holliday and Paul: Robert
Emmanuel Seidler dated the 21st of March 1891 No. 5103 forms on treatment with
nitrite and acetic acid at various temperatures a nitroso-alpha-naphtoldisulphonate
of soda of characteristic properties. It forms fine orange red needles or leaflets
which are difficultly soluble in water. It. yields when treated with ammonia under
pressure the corresponding. nitrosonaphtylamine derivative.
On. heating either the nitroso-alpha-naphtoldisulphonate or the nitroso-alpha-
naphtylaminedisulphonate with three times their weight of aniline. and the equal
weight, of aniline salt, to a temperature between 140° and. 160° Centigrade for
6 to 8 hours. a red melt is formed; from which the, excess, of aniline, is removed
either by distillation, with an excess of caustic soda, or by extraction with hydro-
chloric acid. In the first case the colour separates out of the remaining. liquor
after all the aniline is driven off. In the other case the residue of the extraction
is dissolved in hot water and caustic soda, after having been filtered and washed
with water. From this solution the new compound is precipitated by an excess of
caustic soda or by addition of common salt. It forms red leaflets with a yellow
metallic lustre. Being too insoluble in water it cannot be very well employed as a
dye without resulphonating. For this purpose the recrystallized sulphonate is
decomposed by hydrochloric acid in a solution or fine suspension in hot water.
The precipitated free sulpho acid is filtered, washed, pressed and dried. It is then
ground finely and dissolved in twice its weight of sulphuric acid of 66° Bé. The
sulphonation is complote after 12 hours standing at ordinary temperature or after
an hour's heating up to 10%. The sulphonation melt is then run into cold water.
The new sulpho acid separates from the red acid liquor, is filtered and washed with
some salt water. It is then dissolved in hot water and caustic soda. At a
temperature of about 80° to 90° a small quantity of common salt or an excess of
caustic soda precipitates the sodium salt as crystalline powder, which is filtered,
pressed and dried. The new body dyes wool in an acid bath a blueish red shade
of great fastness to light and milling.
Having now particularly described and ascertained the nature of our said
invention,, and in what manner the same is to be performed, we declare that we
are aware of the Specification of Johnson's Patent No. 6875, A.D. 1890, and we wish
it to be understood that we make no claim to anything described and claimed therein
what we claim is :
The manufacture of a blueish red dye by heating the nitroso napthol and
napthylamine disulpho acids made from the disulnho acid of manthol described in

page_text: the Specification of Letters Patent dated the 21st of March 1891 No. 5103 with
aniline and aniline salts and sulphonating the resulting colour, substantially as
described.
Dated the 2nd day of November 1894.
WM. BROOKES & SON,
55 & 56, Chancery Lane, London, Agents for the Applicants.