AN IMPROVED MANUFACTURE OF CERTAIN SULPHO-ACIDS AND OF COLORING MATTERS THEREFROM
Year: 1882

page_text: LETTERS PATENT to Frank Wirth of the firm of Wirth and Company
Patent Solicitors at Frankfort on the Main in the Empire of Germany for
an Invention of "AN IMPROVED MANUFACTURE OF CERTAIN SULPHO-ACIDS
an Invention of "AN IMPROVED MANUFACTURE OF CERTAIN SULPHO-ACIDS
AND OF
COLORING MATTERS THEREFROM
A communication to aim
the "Farbfabrick vormals Brönner" at Frankfort-on-the Main Germany
Irom
PROVISIONAL SPECIFICATION left by the said Frank Wirth at the Office of
the Commissioners of Patents on the 4th August 1882.
FRANK WIRTH of the firm of Wirth and Company Patent Solicitors at
Frankfort on the Main in the Empire of Germany
" AN IMPROVED
MANUFACTURE OF CERTAIN SULPHO-ACIDS AND OF COLORING MATTERS THERE-
"
FROM [A communication to him from the " Farbfabrick vormals Brönner" at
Frankfort-on-the Main Germany]
The process which forms the subject of this invention is founded on the hitherto
unknown fact that the hydroxyl group of the naphtholsulpho acids can be exchanged
for the amido group.
The process consists in the treatment of the naphtholsulpho
acids or their salts with ammonia at a high temperature. It is indifferent whether
the combinations are formed in a free condition or whether they result during the
reaction, whether their mutual reaction is carried on under pressure or not under
high or low temperature for a longer or shorter period with addition of water with
or without the presence of a water absorbing medium. For example, 60 kilogrammes
of neutral or acid ammonia salt of a betanaphtholmonosulpho acid which is
obtained by heating for several hours in a water bath of 1 part betanaphthol with
2 parts of sulphuric acid of 66° Beaumé, are heated for 24 hours to 150° or 180° C
under pressure along with 60 kilogrammes water and 12 kilogrammes bydrate of
lime. The product is dissolved in hot water, filtered from superfluous hydrate of
lime diluted with about 500 litres of water and acidulated. The resulting
betanaphthylaminesulphoacid separates at once in the form of fine crystals. After
cooling and filtering the acid is well pressed out.. To obtain the acid quite pure
it is only necessary to make one alkaline solution and restore by acid. The
betanaphthylaminesulpho acid thus obtained differs essentially in its properties

page_text: from the betanaphthylaminesulphoacids at present known. It is almost insoluble in
cold water, scarcely soluable in hot water from which it separates in brilliant silvery
glistening flakey crystals. It forms a very insoluable barium salts crystallising
in needles containing 5 equivalents of water of crystallisation. Its diazo combina-
tion with the phenols and the oxyphenols, their ether and sulpho compounds form
a set of novel colouring matters which for example according as they may be
compounded vary from yellow to violet red or brown red. A beautiful gold yellow
die is obtained by combining the diazo acid with resorcin in the known manner,
and an orange with phenol. A blood red dye results from combination with
alphanaphthol or its sulpho acid. The anidoazo compounds of the new acid form
brown dyes. In like manner the mono and disulpho acids of both naphthols can
be converted. And it is obvious that according to the position which the sulpho
groups occupy among the naphtho sulpho acids corresponding different naphthyla-
mine sulpho acids can be produced. Thus another betanaphthylaminesulpho acid
is obtained by the reaction under pressure of 50 kilogrammes of ammonium
betanaphthosulphonate 25 kilogrammes calcined soda of 98° with addition of
water at a temperature of about 180° C. This is almost insoluable in alcohol but
readily soluable in water. Its soda salt is readily soluable in alcohol. Its diazo
compound with alphanaphthol formed in the usual way produces a blue red dye.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Frank Wirth in the Great Seal Patent Office on the
24th January 1883.
-
FRANK WIRTH of the firm of Wirth and Company Patent Solicitors ab
Frankfort on the Main in the Empire of Germany "AN IMPROVED
MANUFACTURE OF CERTAIN SULPHO-ACIDS AND OF COLORING MATTERS THERE-
FROM "
A communication to me from the "Farbfabrick vormals Brönner "
at
Frankfort-on-the Main Germany
The process which forms the subject of this Invention is founded on the hitherto
unknown fact that the hydroxyl group of the naphtholsulpho acids can be
exchanged directly for the amido group. The process consists mainly in the
treatment of the naphtholsulpho acids or their salts with ammonia at a high
temperature. It is indifferent whether the combinations are formed in a free
condition or whether they result during the reaction, whether their mutual reaction
is carried on under pressure or not, under high or low temperature, for a longer or
shorter period, with addition of water, and with or without the presence of a water
absorbing medium. For example, 60 Kilogrammes of neutral or acid ammonia salt
of a betanaphtholmonosulpho acid which is obtained by heating for several hours
in a water bath of 1 part betanaphthol with 2 parts of concentrated sulphuric acid
of 66° Beaumé, are heated for 24 hours to 150° or 180° C under pressure along
with 60 kilogrammes water and 12 kilogrammes hydrate of lime. The product is
dissolved in hot water, filtered from superfluous hydrate of lime, diluted with about
500 litres of water and acidulated. The resulting betanaphthylaminesulphoacid
separates at once in the form of pure crystals. After cooling and filtering, the acid
is well pressed out. To obtain the acid quite pure it is mostly only necessary to
make one alkaline solution and precipitate by acid. The betanaphthylaminesulpho-
acid thus obtained differs essentially in its properties from the betanaphthylamine-
sulphoacid at present known. It is almost insoluble in cold water, scarcely
Boluble in hot water, from which it separates in brilliant silvery glistening flakey
crystals. It forms a very insoluble barium salt crystallising in needles containing
5 equivalents of water of crystallisation. Its diazo combination forms with the
phenols and the oxyphenols, their ether and sulphocompounds a set of novel
colouring matters, which, for example, according as they may be compounded, vary
from yellow to violet-red, or brown-red. A beautiful gold yellow dye is obtained
by combining the diazo acid with resorcin in the known manner, and an orange
with phenol. A pure blood red dye results from combination with alphanaphthol
or its sulpho acid. The amidoazo compounds of the new acid form brown dyes.
In like manner the mono and disulpho acids of both naphthols can be converted.
And it is obvious that according to the position which the sulpho groups occupy
among the naptho sulpho acids, corresponding different naphthylamine sulpho-
acids can be produced. Thus another betanaphthylaminesulphoacid is obtained
by the reaction, under pressure, of 50 kilogrammes of ammonium betanaphitho-
sulphonate, 25 kilogrammes calcined carbonate of soda of 98° with addition of
water at a temperature of about 180° C. This is almost insoluble in alcohol but
readily soluble in water. It soda salt is readily soluble in alcohol. Its diazo
compound with alphanaphthol formed in the usual way produces a blue red dye.
Having thus described the nature of this invention and in what manner the
same is to be performed as communicated to me by my correspondents, I
claim
First. The conversion of the naphtholsulphoacids into the corresponding naph-
thylamine sulphoacids by the action of ammonia, substantially as herein
described.

page_text: Second. The production of Azo colouring matters from the Diazo compounds
of the naphthylaminesulphoacids obtained as set forth in the preceding claim,
combined with the phenoles, oxyphenoles, or their ether and sulpho acids.
Third. The production of the amid oazo compounds of the naphthylamine
sulpho-acids obtained as set forth in the first claim, substantially as herein
described.
In Witness whereof I the said Frank Wirth have bereunto set my hand and
seal this nineteenth day of January in the year of our Lord One thousand
eight hundred and eighty-three.
FRANK WIRTH (L.S.)