Year: 1897

page_text: Date of Application in the United Kingdom, 16th Mar., 1897.
Complete Left, 15th Dec., 1897-Complete Accepted, 26th Feb., 1898
I, HENRI RAYMOND VIDAL, of 95, Boulevard Beaumarchais, Paris, in the
Republic of France, do hereby declare the nature of this invention to be as
follows:
In the Specification of my Application No. 6694 of even date herewith I have
indicated the formation of new dye stuffs by condensation of the amido-benzo or
naphtho sulphonic acids, with ortho, meta or para amidated, hydroxylated or dia-
midated derivatives of benzene or of naphthalene.
I have found that these new colouring matters are capable of combining with
sulphur so as to form other colouring matters of different shades or tints.
Thus on heating in the presence of sulphur, the blue colouring substance obtained
by the condensation of paramidophenol and sulphanilic acid, I obtain a product
which in the presence of an alkaline salt can be dissolved into blue black and which
directly dyes unmordanted cotton into shades or tints of a very deep black.
In carrying out my process I proceed in the following manner: that is to say,
I beat in an oil bath, placed in an iron vessel provided with a stirring device,
a mixture of the following ingredients:
'
28 kilogrammes of a colouring matter derived from parasulphanilic acid and
paramidophenol, and
25 kilogrammes of a solution of caustic soda of 33 per cent. strength, until the
mass has dissolved and sufficiently thickened.
I then pass into this mixture
6 kilogrammes of sulphur; and I maintain the temperature at 170 degrees
Centigrade until the stirring apparatus stops acting.
I may replace the colouring matter arising from the action of paramidophenol
upon parasulphanilic acid,
1. By colouring matters obtained by the condensation of paramidophenol, with
naphthionic, metasulphanilic acids.
2. By colouring matters obtained by the condensation of one of the following
acids parasulphanilic, naphthionic, metasulphanilic, with a diamine or one of
the following amidophenols or naphthols;
Paraphenylene diamine,
Naphthenediamine-a,-a..

page_text: Amidonaphthol-a₁-a.
In those instances where I cause sulphur to act upon a colouring matter derived
from a diamine, I do not employ caustic soda, because this colouring matter is
insoluble in such compound.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.
I, HENRI RAYMOND VIDAL, of 95, Boulevard Beaumarchais, Paris, in the
Republic of France, 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: -
It is known that new colouring matters are formed by the condensation of amido-
benzo- or naptho-sulphonic acids, with the amidated, hydroxylated or diamidated
derivatives, in ortho, meta or para-position, of benzene or naphthalene.
I have found that these new colouring matters are capable of combining with
sulphur so as to form other colouring matters of different shades or tints.
Thus on heating in the presence of sulphur, the blue colouring substance obtained
by the condensation of paramidophenol and sulphanilic acid, I obtain a product
soluble into blue black in an alkali and which directly dyes unmordanted cotton
in shades and tints of a very deep black.
"
In carrying out my process I proceed in the following manner: that is to say,
I heat in an oil bath, placed in an iron vessel provided with a stirring device,
a mixture of the following ingredients:
28 kilogrammes of a colouring matter derived from parasulphanilic acid and
paramidophenol, and
25 kilogrammes of a solution of caustic soda of 33 per cent. strength, until the
mass has dissolved and sufficiently thickened.
I then pass into this mixture
6, kilogrammes of sulphur; and I maintain the temperature at 170 degrees
Centigrade until the stirring apparatus stops acting.
I may replace the colouring matter arising from the action of paramidophenol
upon parasulphanilic acid,
1. By colouring matters obtained by the condensation of paramidophenol, with
naphthionic, metasulphanilic acids.
2. By colouring matters obtained by the condensation of one of the following
acids parasulphanilic, naphthionic, metasulphanilic, with a diamine or one of
the following amidophenols or naphthols;
Paraphenylene diamine,
Naphthylene diamine-a-a.
Metamidophenol,
Orthoamidophenol,
Amidonaphthol-a₁-a
In those instances where I cause sulphur to act upon a colouring matter derived
from a diamine, I do not employ caustic soda, because this colouring matter is
insolubl

page_text: Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is:-
1. A method of preparation of a black colouring matter, consisting in bringing
about in the presence of caustic soda a hot reaction of sulphur upon the blue
colouring agent obtained by the condensation of parasulphanilic acid with par-
amido-phenol.
2. A novel black colouring matter obtained by the process claimed in the first
claim soluble into blue black in the alkalies and adapted to dye vegetable fibre a
very rich (or deep) black.
3. A method of preparation of colouring materials consisting in bringing about in
the presence of caustic soda a hot reaction of sulphur upon the colouring agents
obtained by condensing par-amido-phenol with either naphthionic or meta-sulph-
anilic acid or a mixture of both these acids.
4. The colouring matters obtained by the process claimed in the 3rd Claim
soluble in the alkalies and adapted to dye vegetable fibre black.
5. A method of preparation of colouring matters consisting in causing a hot
reaction of sulphur to take place upon the colouring agents obtained by the con-
densation of one of the following acids: Para-sulph-anilic acid, naphthionic acid,
meta-sulph-anilic acid with one of the following diamines; Para-phenylene dia-
mine, naphthylenediamine 1-4, or one of the following amido-phenols or amido-
naphtols, metamido-phenol, ortho-amido-phenol and amido-naphthol 1-4, the
reaction in the case of the amido-phenols or amido-naphtols taking place in the
presence of caustic soda.
6. The colouring matters obtained by the process claimed in the 5th Claim
soluble in alkalies and adapted to dye vegetable fibre black.
Dated this 15th day of December 1897.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.