Improvements in the Manufacture of Tetra-nitro-anthrachrysone.
Year: 1892

page_text: Date of Application, 7th Dec., 1892
Complete Specification Left, 2nd Sept., 1893-Accepted, 14th Oct., 1893
PROVISIONAL SPECIFICATION.
[Communicated from abroad by THE FARBWERKE vormals MEISTER LUCIUS
AND BRUNING, of Hoechst on Maine, in the German Empire, Chemical
Manufacturers].
Improvements in the Manufacture of Tetra-nitro-anthrachrysone.
I, OLIVER IMRAY of No. 28 Southampton Buildings, Chancery Lane in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention to be as follows:-
Anthrachrysone can be easily and quantitatively converted into a tetra-nitro-
compound.
For nitrating the anthrachrysone, it is dissolved in about twelve times its weight
of concentrated sulphuric acid and while cooling it is caused to flow slowly into
the quantity of nitric acid calculated, for 4 nitro groups in the form of nitrating-
acid. As the nitration proceeds the nitro-product separates in the form of a yellow
crystalline mass. To ensure that the entire quantity of anthrachrysone is con-
verted into the nitro-compound, near the end of the operation the entire mass is
heated to about 80° C.
After having cooled down it is poured upon ice and diluted with such a quantity
of water that the separated nitro-anthrachrysone remains undissolved in the diluted
acid; it is separated from the acid by filtration.
In order to purify the crude product it is precipitated from its aqueous solution
by means of concentrated hydrochloric acid and washed with somewhat diluted
hydrochloric acid. The purified product has been found to contain 12.1 per cent.
of nitrogen; the calculated quantity of nitrogen for the tetra-nitro-anthrachrysone
being 12-4 per cent.
The tetra-nitro-anthrachrysone is easily soluble in the usual solvents, except in
benzene, ligroine and chloroform. From its solution in pure glacial acetic acid it
can be obtained by precipitation by means of chloroform in the form of very small
crystals, which heated to from 280° to 300° C. decompose with detonation. With
potassium, sodium and ammonium it forms a salt insoluble in alcohol. The salts of
the nitro-anthrachrysone detonate on being heated.
The tetra anthrachrysone dyes chromed wool strong brown shades, alumned
wool strong claret-brown shades, which excel by great fastness in fulling and in
lustre. In these respects the tetra-anthrachrysone is superior to all the coloring
matters of similar shade at present known.
Din 7th dox of December 1800
ABEL & IMRAY,
Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Tetra-nitro-anthrachrysone.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered 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 :-
Anthrachrysone can be easily and quantitatively converted into a tetra-nitro-
compound.
For nitrating the anthrachrysone, it is dissolved in about twelve times its weight
of concentrated sulphuric acid and, while cooling, it is caused to flow slowly into

page_text: the quantity of nitric acid calculated, for 4 nitro groups in the form of nitrating
acid. As the nitration proceeds the nitro product separates in the form of a yellow
crystalline mass. To ensure that the entire quantity of anthrachrysone is con-
verted into the nitro compound, near the end of the operation the entire mass is
heated to about 80° C.
After having cooled down it is poured upon ice and diluted with such a quantity
of water that the separated nitro anthrachrysone remains undissolved in the dilute
acid; it is separated from the acid by filtration.
In order to purify the crude product it is precipitated from its aqueous solution
by means of concentrated hydrochloric acid and washed with somewhat diluted
hydrochloric acid. The purified product has been found to contain 12.1 per cent.
of nitrogen; the calculated quantity of nitrogen for the tetra-nitro-anthrachrysone
being 12.4 per cent.
The tetra-nitro-anthrachrysone is easily soluble in the usual solvents, except in
benzene, ligroine and chloroform. From its solution in pure glacial acetic acid it
can be obtained by precipitation by means of chloroform in the form of very small
crystals, which when heated to 280° to 300° C. decompose with detonation.
With potassium, sodium and ammonium it forms a salt insoluble in alcohol. The
salts of the tetra-nitro-anthrachrysone detonate on being heated.
The tetra nitro anthrachrysone dyes chromed wool strong brown shades, alumned
wool strong claret-brown shades, which excel by great brilliancy and fastness in
fulling. In these respects the tetra-nitro anthrachrysone is superior to all the
coloring matters of similar shade at present known.
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 herein described manufacture of tetra-nitro-anthrachrysone by treating
anthrachrysone with suitable proportion of nitric acid.
2. The tetra-nitro-anthrachrysone manufactured as above set forth.
Dated this 2nd day of September 1893.
ABEL & IMRAY,
Agents for the Applicant.