Improvements in the Manufacture of Colouring Matters.
Year: 1898

page_text: Improvements in the Manufacture of Colouring Matters.
I, HENRY RAYMOND VIDAL, of 95, Boulevard Beaumarchais, Paris, in the Republic
of France, Chemical Engineer, do hereby declare the nature of this invention to be
as follows:-
I have found that some di-hydroxylated azo-compounds (azoïques dihydroxylés),
such as the product of the combination of one or two molecules of aniline with
resorcin, heated with sulphur in presence of alkaline sulphides, produce colouring
matters capable of dyeing vegetable fibre directly in dark shades.
Example: heat in an oil bath in a cast-iron vessel or digester, provided with a
stirring device or agitator, for about five hours and at a temperature of about from
220° to 280° C.
During the process of the reaction water is added to the mass from time to time
until the complete reduction of the azo-compound. This complete reduction may be
recognized by the disappearance of the orange colour of the azo-compound; and
thereupon no more water is added to the mass and the same is then evaporated to
dryness.
The product thus obtained forins a black, brittle mass which is soluble in water and
capable of dyeing cotton to a dark shade without a mordant.
In the reaction herein before described I may replace the product of the combination
of the one molecule of resorcin with one of aniline, by a corresponding product
obtained from the combination of two molecules of aniline with one of resorcin, but
in this case I double the quantity of sulphur and sulphide.
Furthermore I may sometimes employ instead of the two azo-compounds of resorcin
in connection with the examples given above, the product of the combination of one
or two molecules of aniline or of an analogous aromatic amine with the di-oxy-
naphthalines capable of combining in the same manner as resorcin.

page_text: Example I heat in an oil bath in a cast iron digester, provided with stirring
device, for five hours to about 220 to 280° C.
K.
During the process of the reaction water is added from time to time in the same
manner as in the previous example, until complete reduction of the azo compound.
After this the mass is evaporated to dryness.
The resulting product is a black brittle mass, soluble in water and capable, in this
state, of dyeing cotton to a dark shade without a mordant.
It will be understood that in the heating with sulphur and sulphide, I can replace
the before mentioned compounds by amido-resorcin and di-amido-resorcin as well as
by amido-di-oxy-naphthalines and di-amido-di-oxy-naphthalines, being products of
the reduction of the before inentioned corresponding azo-compounds and which are
formed in the reaction as intermediate products.
ated thig 91st dort of Lune 1000
1
"
; ↑
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.
Improvements in the Manufacture of Colouring Matters.
I, HENRI RAYMOND VIDAL, of 95, Boulevard Beaumarchais, Paris, in the Republic
of France, Chemical Engineer, 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 :-
I have found that some di-hydroxylated azo-compounds (azoïques dihydroxyles),
such as the product of the combination of one or two molecules of aniline with
resorcin, heated with sulphur in presence of alkaline sulphides, produce
colouring matters capable of dyeing vegetable fibre directly in dark shades.
Example: I heat in an oil bath in a cast-iron vessel or digester, provided with a
stirring device or agitator, for about five hours and a temperature of about from 220°
to 280° C.
During the process of the reaction water is added to the mass from time to time
until the complete reduction of the azo-compound. This complete reduction may
be recognized by the disappearance of the orange. colour of the azo compound; and
thereupon no more water is added to the mass and the same is then evaporated to
dryness.
The product thus obtained forms a black, brittle mass which is soluble in water and
capable of dyeing cotton to a dark shade without a mordant.
In the reaction hereinbefore described I may replace the product of the combina-
tion of the one molecule of resorcin with one of aniline, by a corresponding product

page_text: obtained from the combination of two molecules of aniline with one of resorcin, but
in this case I double the quantity of sulphur and sulphide.
Furthermore I may sometimes employ instead of the two azo compounds of
resorcin in connection with the examples given above, the product of the combina-
tion of one or two molecules of aniline or of an analogous aromatic amine with the
di-oxy-naphthalines capable of combining in the same manner as resorcin.
Example: I heat in an oil bath in a cast iron digester, provided with stirring
device, for five hours to about 220 to 280° C.
During the process of the reaction water is added from time to time in the same
manner as in the previous example, until complete reduction of the azo
compound.
After this the mass is evaporated to dryness.
The resulting product is a black brittle mass, soluble in water and capable, in this
state, of dyeing cotton to a dark shade without a mordant.
It will be understood that in the heating with sulphur and sulphide, I can replace the
before mentioned compounds by amido-resorcin and di-amido-resorcin as well as by amide-
di-oxy-naphthalines and di-amido di-oxy-naphthalines, being products of the reduc-
tion of the before mentioned corresponding azo-compounds and which are formed in
the reaction as intermediate products.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. A process for the production of colouring matters consisting in causing sulphur
to react on the azo-compounds resulting from the combination of di-azo-benzol or its
analogues with resorcin and di-oxy-naphthaline capable of combining under the same
conditions as resorcin or amido and diamido-di-oxy-benzol and di-oxy-naphthaline
products obtained from the reduction of the azo-compounds above mentioned, the
reaction taking place in the presence of an alkaline sulphide.
2. The colouring matters obtained by the process claimed in Claim 1 and forming
a black brittle mass, soluble in water and capable of dyeing cotton directly without a
mordant.
3. The application of the products above referred to in connection with dyeing and
printing operations.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.