Improvements in the Manufacture and Production of Dyestuffs.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
Improvements in the Manufacture and Production of Dyestuffs.
I, GEORGE WILLIAM JOHNSON, of 47, Lincoln's Inn Fields, in the County of
London, Patent Agent, do hereby declare the nature of this invention (which
has been communicated to me from abroad by Kalle & Co., of Biebrich-on-
Rhine, in the German Empire) to be as follows:-
The primary disazo dyestuffs of the amido-naphthol-di-sulpho acids already
known and introduced into the market contain the auxo-chrome group only in
the amido-naphthol employed in their preparation. The diazo compounds are
derived either from unsubstituted bases or from those derivatives of the same
in which the substitutes represent merely salt-forming or indifferent groups.
My foreign correspondents have found that in the preparation of primary
disazo dye-stuffs by starting from the amido-naphthol-di-sulpho acid K, diazo
compounds containing certain predetermined auxo-chrome groups may be em-
ployed, as, for example, nitro amido-phenol, nitro-amido-phenol-sulpho acids or
picramic acid. By such means, colouring matters are obtained possessing the
character of mordant dyes which, especially in the subsequent treatment with
chrome salts, will impart to the fibre deeper shades & considerably faster dyes.
From the other amido-naphthol-di-sulpho acids; such, for example, as amido-
naphthol-di-sulpho acid S, or amido-napthol-di-sulpho acid H, disazo dyestuffs
cannot be manufactured by resorting to nitrated amido phenols; as the pro-
ducts obtained by this method are unfit for use for industrial purposes.
The following examples will further illustrate the nature of this invention,
but it is not limited to the precise details.
EXAMPLE 1.
PICRAMIC ACID-AZO-K ACID-ANILINE.
22.1 kilogrammes of picramate of soda is dissolved in 1000 litres of water
with 6.9 kilogrammes of nitrite and then mixed with 30 kilogrammes of hydro-
hloric acid of a specific gravity of 20° Bé.
After stirring the mixture, the diazotizing process will be complete.
Into this diazo solution there is then poured a solution of 34 kilogrammes of
cid sodium-salt of the K acid and 5.5 kilogrammes of soda.
The "coupling" will be complete after about twenty hours stirring. There
then added the diazo solution obtained in the usual manner from 9.3 kilo-
rammes of aniline and an amount of acetate of sodium proportionate to the
ee acidity.
The formation of the diazo colouring agent, or dye-stuff, will be complete
ter several hours stirring. It is then salted out, pressed, and dried. The new
louring matter is a bronze red powder dissolving readily in water while u

page_text: is practically insoluble in alcohol. The solution in concentrated sulphuric acid
is green. The new colouring matter dyes wool in an acid bath, greenish-black.
By after treatment with chrome salts the shade of the dyes is but slightly altered
and their fastness is very considerably enhanced.
EXAMPLE II.
ALPHA-NAPHTHYLAMINE-AZO-K-ACID-AZO-PICRAMIC ACID.
To the diazo solution obtained from 14.5 kilogrammes of alpha-naphthylamine
is added a solution of 34 kilogrammes of acid sodium salt of the K acid and 5.5
kilogrammes of soda.
After stirring for about twelve hours the mixture is neutralised with caustic
soda lye, and mixed with 20 kilogrammes of soda.
A diazo solution obtained from 22.1 kilogrammes of picramate of soda in the
manner described in the first example is then added, the whole being stirred
some time, and slightly heated, and the diazo dye thus formed is salted out.
It is obtained in the condition of a brown powder with a bright bronze-
like lustre and is readily soluble in water. The solution in concentrated sul-
phuric acid is green. It dyes wool green in an acid bath. The fastness of the
dyes is materially enhanced by subsequent treatment with chrome. The sub-
stitution for picramic acid of amido-nitro-phenol-sulpho acid will make little,
or no, difference either to the process itself, or to its results.
Of the several classes of dyestuffs which may be produced in accordance with
the above examples those will generally be found to be most valuable which
contained nitro diazo phenol in the second place.
Dated this 91 dow of I.... 1900
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C.,
Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture and Production of Dyestuffs.
I, GEORGE WILLIAM JOHNSON, of 47, Lincoln's Inn Fields, in the County of
London, Patent Agent, do hereby declare the nature of this invention (which
has been communicated to me from abroad by Kalle & Co., of Biebrich on
Rhine, in the German Empire), and in what manner the same is to be performed
to be particulaly described and ascertained in and by the following statement; -
The primary disazo dyestuffs of the amido-naphthol-di-sulpho acids already
known and introduced into the market contain the auxo-chrome group only in
the amido-naphthol employed in their preparation. The diazo compounds are
derived either from unsubstituted bases or from those derivatives of the same
in which the substitutes represent merely salt-forming or indifferent groups.
My foreign correspondents have found that in the preparation of primary
disazo dye-stuffs by starting from the amido-naphthol-di-sulpho acid K, diazo
compounds containing certain predetermined auxo-chrome groups may be em-
ployed, as, for example, nitro amido-phenol, nitro-amido-phenol-sulpho acids or
pieramic acid. By such means, colouring matters are obtained possessing the
character of mordant dyes which, especially in the subsequent treatment with
chrome salts, will impart to the fibre deeper shades and considerably faster dyes.
From the other amido-naphthol-di-sulpho acids, such, for example, as amido-

page_text: cannot be manufactured by resorting to nitrated amido phenols; as the pro-
ducts obtained by this method are unfit for use for industrial purposes.
or amido-naphthol-di-sulpho acid H, disazo dyestuffs
The following examples will further illustrate the nature of this invention
and the manner of carrying the same into effect but it is not limited to the
precise details.

page_text: of mordant dyes by combining orthoamido azo colours, obtained from amido
naphthol disulphonic acid K and a suitable diazo body in acid solution, with
an equimolecular proportion of diazotized picramic acid, or nitroamido phenol
sulphonic acid, all substantially as hereinbefore described.
3. As new articles of manufacture the primary disazo colouring matters,
possessing the character of mordant dyes, such as can be obtained, substantially
as herein before described.
Dated this 23rd day of April 1900.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C.,
Agents.