Year: 1897

page_text: 15 kilos. of paraamidoacetanilid is diazotised in the usual way with hydrochloric
acid and 7 kilos. of nitrite of sodium, then combined with 24 kilos. of 8 1 amido
a 4 naphtol 8 3 sulpho acid in alkaline solution. The azo colouring matter is
filtered off, then dissolved in 500 liters of boiling water, 150 kilos. of caustic soda
lye of 40° Bé. added thereto and the whole boiled for about two hours. Then the
solution is allowed to stand until cold, acidulated with 250 kilos. of hydrochloric
acid of 22 per cent., mixed with 500 kilos. of ice, and diazotised with 14 kilos. of.
nitrite of sodium. The tetrazoazo compound thus formed is, in its solution con-
taining a surplus of hydrochloric acid, mixed with a solution of 11 kilos. of
metaphenylendiamine. After stirring for some hours the separation of a black

page_text: precipitate of the new diazodisazo compound is completed, the latter probably
possessing the formula
ATT

page_text: The diazodisazo compound prepared in accordance with Example I is introduced
into the solution of 24 kilos of ẞ1 a 4 amidonaphtol ẞ 3 sulpho acid in about
500 liters of water and 80 kilos. of carbonate of sodium. After standing for several
hours it is heated to about 80° Celsius and then the colouring matter filtered off
5 and dried. It dyes unmordanted cotton in deep blueish black shades.
EXAMPLE IV.
The diazodisazo compound prepared in accordance with Example II is
introduced into an alkaline solution of the azo colouring matter obtained from
15.5 kilos. of diazotised paramidosalicylic acid and 11 kilos. of metaphenylendi-
amine. The procedure is then as in Example III. The colouring matter dyes
unmordanted cotton in reddish black shades.
Dated this 3rd day of Santamber 1807
THOMAS R. SHILLITO,
89, Chancery Lane, London, W.C.
Manufacture of New Polyazo Colouring Matters or Dyes.
I, THOMAS RICHARD SHILLITO, of 89, Chancery Lane, London, W.C., Engineer
and Patent Agent, do hereby declare the nature of this invention and in what
manner the same is to be performed, a communication to me from abroad by
Messieurs John Rudolph Geigy & Co., of Basle, Switzerland, Colour Manufacturers,
to be particularly described and ascertained in and by the following statement:--
This invention relates to the production of new polyazo colours deriving from
new intermediary diazodisazo compounds which are formed by combination of a
tetrazoazo compound of the general formula
N=N-P-N-N-R-N-N
in an acid solution with one molecule of a metadiamine, metaamido-phenol,
resorcine, metaphenylenediaminsulpho acid, metatoluylendiaminesulpho acid or one
molecule of a chrysoidine, that is to say, a monoazo colour derived from meta-
phenylenediamine, metatoluylenediamine or metaphenylenediamine sulpho acid.
In this formula P signifies the rest of one of the following p-diamines :-Benzi-
dine, methylbenzidine, tolidine, aethoxybenzidine, diamidodiphenolaether, diamido-
stilbene, p-phenylenediamine, p-toluylenediamine, p-diamidodiphenylamine,
p-diamidophenyltolylamine, p-diamidoditolylamine, 1-4 naphtylenediaminė, 1.5"
naphtylenediamine or their sulpho acids.
R signifies the rest of one of the following compounds:
:-a naphtylamine, al
naphtylamine ẞ3 sulpho acid, a 1 naphtylamine ẞ4 sulpho acid, a 1 amido ẞ1
naphtolaether, a 1 amido ẞ1 naphtolaether 33 sulpho acid, a 1 amido 1 naphtol-
aether 4 sulpho acid, 81 amido a 4 naphtol 8 3 sulpho acid, ẞ1 amido a 4 naphtol
B2B 3 disulpho acid, a 1 a 4 amidonaphtol s 2 B 3 disulpho acid, s 1 amido
naphtol s 4 sulpho acid, p-xylidine, amidocresolether.
3

page_text: is filtered off, then dissolved in 500 liters of boiling water with 150 kilos. of caustic
soda lye of 40° Bé. added thereto, and boiled for about 2 hours. Then the solution
is allowed to stand until cold, acidulated with 250 kilos. of hydrochloric acid of
22 per cent., mixed with 500 kilos. of ice and diazotised with 14 kilos. of nitrite of
sodium. The tetrazoazo compound thus formed is mixed with a solution of 11 kilos.
of metaphenylenediamine. After stirring for some hours the separation of a black
precipitate of the new diazodisazo compound is completed.
The latter possesses probably the following formula :-

page_text: XAMPLE 111.
The diazodisazo compound prepared according to the prescription of Example I.
is introduced into the solution of 24 kilos. of 81 a 4 amidonaphtol s 3 sulpho acid
in about 500 liters of water with 80 kilos. of carbonate of sodium. After standing
some hours it is heated to about 80° Celsius and then the colouring matter filtered
off and dried. It dies unmordanted cotton in deep blueish black shades.
C
in an acid solution with one molecule of a metadiamine, metaamidophenol, resorcine,
metaphenylenediaminesulpho acid, metatoluylenediaminesulpho acid, or one
molecule of a chrysoidine, substantially as described.
2. The production of new polyazo colours by combination of the intermediary
compounds referred to with an amine or phenol or a derivate of them, substantially
as described.
3. The new colouring matters or dyes obtained substantially as described.
n
1000
THOMAS R. SHILLITO,
89, Chancery Lane, London, W.C.