IMPROVEMENTS IN COLOURING MATTERS
Year: 1883

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 "IMPROVEMENTS IN COLOURING MATTERS a communication
from Mess Dittler & Co trading under the firm of "Farbwerk Griesheim am
Main" at Griesheim near Frankfort /m Germany
PROVISIONAL SPECIFICATION left by the said Frank Wirth at the Office
of the Commissioners of Patents on the 25th April 1883.
FRANK WIRTH of the firm of Wirth and Company Patent Solicitors at
Frankfort on the Main in the Empire of Germany
"IMPROVEMENTS IN
COLOURING MATTERS." [A communication from Mess Dittler & Co trading
under the firm of "Farbwerk Griesheim am Main" at Griesheim near Frankfort
% Germany]
This invention relates to the manufacture of yellow and red colouring matters.
According to the said invention I first prepare sulphuretted "naphthylamine "as
follows that is to say, ten (10) parts of naphthalin are mixed with fifty (50) parts
of concentrated sulphuric acid and heated to a temperature of 160° (C) for about
four hours. Into the solution thus obtained and after it has cooled nine (9) parts
of nitric acid are slowly poured whilst the vessel containing the solutions is kept
cool. The mass when cool is diluted with water and then thoroughly reduced
with iron filings. The calcined salts which have been freed from sulphuric acid
and iron by means of lime milk are triturated with soda and lastly dried by
steam.
Instead of adding nitric acid to the mixture of acids resulting from the solution
of naphthalin in sulphuric acid, these said acids may be separated by other well
known means and then may be proceeded with as above.
If desired ten (10) parts of naphthalin may be mixed with from four (4) to
five (5) parts of fuming sulphuric acid containing 23% of anhydrous sulphuric
acid and heated for five (5) hours to a temperature of 180 C degrees, after which
the mixture is allowed to cool.

page_text: The resulting mass being diluted with a little water is gradually mixed with
nine (9) parts of nitric acid whilst the vessel is being cooled. Thus a nitrous
matter is obtained which can be reduced in the manner above described and
triturated with soda.
Instead of reducing with iron filings as bereinbefore described the acid solution
of naphthalin, sulphuric and nitric acid, the alkaline salts of naphthalin present
in the solution can be brought out as an alkaline solution, by heating with zinc in
powder and mixing with soda.
"
The salts obtained by the above methods of acidification of the naphthalin yield
by means of accessory operations with acids and nitrates a composition" which
being treated with Phenol and naphtha, gives a yellow and red colouring matter.
In the preparation of yellow colouring matter thirty (30) parts of the salts
obtained with soda by one of the above described methods are put in water to
which twelve (12) parts of muriatic acid are added. The mixture being cooled
down to 4° C a solution of seven (7) parts of a nitrate is added.
The composition thus obtained is then stirred into a solution in water of nine
(9) parts of Phenol and twelve (12) parts of soda and the yellow colouring matter
which precipitates is collected, filtered and dried.
In the preparation of scarlet if the composition obtained as above is stirred into
a solution in water of fourteen (14) parts of two naphthas which I hereinafter call
Alpha and Beta" (a and B) and twelve (12) parts of soda two red colours are
obtained of which the first is somewhat more yellow than the last.
«
If the composition above obtained be thrown into a solution of twenty five (25)
parts of the "Alpha" (a) naphtha, sulphate of soda and twelve (12) parts of
Boda, a red colouring matter will be formed in the shape of brownish red flakes.
These flakes are made more abundant by the addition of hydrochlorate of soda.
By using twenty five (25) parts of "beta" naphtha, sulphate of soda and two (2)
parts of soda a scarlet colour of paler hue is obtained.
If the composition is mixed with a solution of 35 kilogrammes of "beta" (8)
naphtha and bisulphate of soda a scarlet colouring matter will be produced with
a pale hue.
The colouring matter is obtained by means of suitable salts and when dried is in
the form of a brownish red powder.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent and of
an Order of the Lord Chancellor filed by the said Frank Wirth in the Patent
Office on the 7th February 1884.
"
FRANK WIRTH of the firm of Wirth and Company, Patent Solicitors, at
Frankfort on the Main, in the Empire of Germany "IMPROVEMENTS IN
COLOURING MATTERS A communication from Messrs Dittler and Co trading
under the firm of "Farbwerk Griesheim am Main," at Griesheim near Frankfort
o/M. Germany
This invention relates to the manufacture of yellow and red colouring or dyeing
matters.
According to the said invention I first prepare sulpho-naphthylamine as
follows, that is to say, ten (10) parts of naphthalene are mixed with fifty (50) parts
of concentrated sulphuric acid and heated to a temperature of 160° Celsius for
about four hours. Into the acid solution of disulpho naphthalic acids thus obtained,
and after it has cooled, nine (9) parts of nitric acid are slowly poured whilst the
vessel containing the solution is kept cool. The mass is now diluted with water
and thoroughly reduced with iron filings. Calcium salts freed from sulphuric acid
and iron are obtained by the addition of milk of lime, and are converted with the
addition of soda into salts of soda, and lastly dried by steam heat.
Instead, of treating with nitric acid the mass of disulpho naphthalic acid obtained,
each acid may be separated by other well known methods and converted in the
aforesaid manner into amido-products.
If desired ten (10) parts of naphthalene, may be mixed with from four (4) to
five (5) parts of fuming acid containing 23% of anhydrous sulphuric acid and
heated for five (5) hours at a temperature of 180 degrees Celsius, the mixture
being subsequently allowed to cool.
In the resulting mass, to which a small quantity of water is added, I pour,
whilst the vessel is being cooled, nine (9) parts of nitric acid, when a nitro-derivative
is obtained which can be reduced in the manner above described and converted
into salts of soda..
Instead of reducing, with iron, the above prepared nitro-sulpho naphthalic acids
in acid solution, alkaline salts may be produced from the said nitro-sulpho-
naphthalic acids, and such salts, may be, when boiled with pulverized zinc in
alkaline solution, converted into amido-sulpho acid salts.
The salts obtained by the above methods from the amido-sulpho naphthalic acids
yield, when treated by suitable acids and nitrites, Diazo compounds which, being
treated with phenol and naphthol, produce, according to the sulpho-acids employed,
a yellow or red colouring matter.
In the preparation of one of the Diazo compounds, thirty (30) parts of salts of soda,
from one or the other of the newly formed amido-sulpho naphthalic acids obtained
according to the above methods are dissolved in water, to which thirty two (32)
parts of muriatic acid are added. The mixture being cooled down to 4° Celsius a
solution of seven (7) parts of a nitrite is added. For the production of the yellow
colouring matter the Diazo compound thus obtained is stirred with an aqueous
solution of nine (9) parts of Phenol and twelve (12) parts of soda. The yellow
colouring matter which precipitates is collected filtered and dried.
When the Diazo compound obtained as above is treated with a solution in
water of fourteen (14) parts of either a or ẞ naphthol and twelve (12) parts of soda,
two red colours are obtained in each case, the one of which is somewhat more
yellow than the other.

page_text: -
When the aforesaid Diazo compound is treated with a solution of twenty five
(25) parts of a soda salt of a naphthol-monosulphonic acid and eleven (11) parts of
Boda, a red colouring matter will be formed and separate in the form of brownish
red flakes. These flakes precipitate more abundantly when common salt is added
to the mixture. This substance will serve as a scarlet dye or colour.
By using twenty five (25) parts of a soda salt of ẞ napthol-monosolphonic acid,
and eleven (11) parts of soda, a red colour of paler hue than those above described
is obtained
When the Diazo compound is mixed with a solution of 35 parts of a soda salt
of naphthol disulphonic acid and 11 parts of soda, a red colouring matter having
a pale hue will be produced.
The coloring matter is obtained by salting out (aussalzen) and when dried is in
the form of a brownish red powder.
Having thus fully described the said invention as communicated to me and the
manner of performing the same I wish it understood that I Claim ;-
First The preparation of sulpho-amido-naphthalic acids from disulpho and
trisulpho naphthalic acid, by nitrification and subsequent reduction.
Second. The production of yellow or red colouring matters by the combination
of a "Diazo" compound obtained from the sulpho-naphthalene with phenol and
soda, or with a naphthol, ẞ naphthol, a naphthol-mononsulphonic acid, B naphthol-
monosulphonic acid or ẞ naphthol-disulphonic acid and soda, as above set forth
In witness whereof I the said Frank Wirth have hereunto set my hand and
seal this Twenty fifth day of January in the year of our Lord One thousand eight
hundred and eighty four.
TD ANIZ WIDTH
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