The Manufacture and Production of New Colouring-matters of the Anthracene Series.
Year: 1899

page_text: Date of Application, 13th July, 1899
Complete Specification Left, 27th Mar., 1900-Accepted, 28th Apr., 1900
PROVISIONAL SPECIFICATION.
The Manufacture and Production of New Colouring-matters of the
Anthracene Series.
I, JAMES YATE JOHNSON, of 47, Lincoln's Inn Fields, in the County of London,
Gentleman, do hereby declare the nature of this invention (which has been
communicated to me from abroad by The Badische Anilin & Soda Fabrik, of
Ludwigshafen-on-Rhine, in the German Empire) to be as follows: —
It is known that diamido-anthraquinone can be readily converted into
sulphoacids, which are wool-colouring matters, yielding red to violet-red shades
in an acid bath. On account of their poor qualities in certain respects these
colouring matters have not hitherto been used practically in the dyeing
industry.
The present invention consists in the conversion of these diamido-anthra-
quinone sulphoacids into valuable colouring-matters by nitrating them. The
nitro colouring-matters thus obtained dye chrome mordanted wool giving blue-
violet to brown-violet shades which are very fast to light.
The following example will serve to further illustrate the nature of the inven-
tion, and the manner in which the new colouring-matters may be obtained but
the invention is not limited to the details given."
EXAMPLE.
Mix together about 10 parts of 1.4' (or 1.5) diamido-anthraquinone and
10 parts of dried boracic acid. Add this mixture to about 200 parts of sulphuric
acid monohydrate. Add to the melt 200 parts of fuming sulphuric acid (con-
taining about 40% SO%). Heat the mixture to about 115° Centigrade and
maintain it at this temperature until a test portion is completely soluble in
water. Allow the melt to cool. Prepare 6 parts of a cold mixture of nitric
and sulphuric acids containing 85% HNO₂.” Run the cold melt into this cold
mixture, stir thoroughly and cool continuously, so that the temperature of the
mixture constantly remains below 10° Centigrade. When the mixture has
been effected, stir for about 12 hours at the ordinary temperature, then pour
the melt into ice water, and salt out the nitro product obtained with potassium
chloride or common salt. Filter and dry.
The colouring-matter so obtained is a dark coloured powder, readily soluble
in water, giving a red-violet solution. The sulphoacids of 1.3. (alpha) and
1.1 (1.8 or delta) diamido-anthraquinones can similarly be converted into nitro
derivatives soluble in water.
The foregoing example may be varied in many ways. For instance, instead
of taking the melt containing diamido-anthraquinone sulphoacids, isolated
diamido anthraquinone-sulphoacid can be dissolved in sulphuric acid and
nitrated.
Doind thi 102
S TL 1800

page_text: The Manufacture and Production of New Colouring-matters of the
Anthracene Series.
I, JAMES YATE JOHNSON, of 47, Lincoln's Inn Fields, in the County of London,
Gentleman, do hereby declare the nature of this invention (which has been
communicated to me from abroad by The Badische Anilin & Soda Fabrik, of
Ludwigshafen-on-Rhine, in the German Empire) and in what manner the
same is to be performed to be particularly described and ascertained in and
by the following statement:-
It is known that diamido-anthraquinone can be readily converted into
sulphoacids which are wool colouring matters yielding red to violet-red shades
in an acid bath. On account of their poor qualities in certain respects, these
colouring matters have not hitherto been used practically in the dyeing
industry.
The
The present invention consists in the conversion of these diamido-anthra-
quinone sulphoacids into valuable colouring matters by nitrating them.
nitro colouring matters thus obtained dye chrome mordanted wool blue-violet
to brown-violet shades which are very fast to light.
The following example will serve to further illustrate the nature of the inven-
tion, and the manner in which the new colouring matters may be obtained but
the invention is not limited to the details given in this example. The parts
are by weight.
EXAMPLE.
Mix together about ten parts of 1.41 (or 1.5) diamido-anthraquinone and ten
parts of dried boracic acid. Add this mixture to about two hundred parts of
sulphuric acid monohydrate. Add to the melt two hundred parts of fuming
sulphuric acid (containing about forty per cent. SO3). Heat the mixture to about
one hundred and fifteen degrees Centigrade and maintain it at this temperature
until a test portion is completely soluble in water. Allow the melt to cool.
Prepare six and a half parts of a cold mixture of nitric and sulphuric acids
containing eighty five per cent. HNO3. Run the cold melt into this cold
mixture, stir thoroughly, and cool continuously so that the temperature of the
mixture constantly remains below ten degrees Centigrade. When the mixture
has been effected stir for about twelve hours at the ordinary temperature, then
pour the melt into ice water and salt out with potassium chloride, or common
salt the nitro product obtained. Filter and dry.
The colouring matter so obtained is a dark coloured powder, readily soluble
in water, giving a red-violet solution. The sulphoacids of 1.3 (alpha) and
1.1, (1.8 or delta) diamido anthraquinones can similarly be converted into nitro
derivatives soluble in water.
The foregoing example may be varied in many ways. For instance instead
of taking the melt containing diamido-anthraquinone sulphoacids, isolated
diamido-anthraquinone sulphoacid can be dissolved in sulphuric acid and
nitrated.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed I declare that what
I claim is:
1. The manufacture of new colouring matter of the anthracene series by con-
verting diamido-anthraquinones into sulphoacids and treating the same with

page_text: nitric acid in concentrated sulphuric acid solution substantially as herein before
described.
2. The manufacture of new colouring matters of the anthracene series, by
treating a solution of diamido-anthraquinone sulphoacid in sulphuric acid with
nitric acid substantially as herein before described.
3. The manufacture of new colouring matters of the anthracene series by
treating diamido anthraquinone sulpho acid with nitric acid.
4. The manufacture of new colouring matters of the anthracene series sub-
stantially as described in the Example hereinbefore given.
5. As new products of manufacture the new colouring matters of the anthra-
cene series such as can be obtained substantially as herein before described.
Dated this 27th day of March 1900.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.