Improvements in the Manufacture of Colouring Matters.
Year: 1898

page_text: PROVISIONAL SPECIFICATION.
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 to be as follows:--
In the Specification of my former Application of March 13th 1897 No. 6694 I
have described a blue colouring matter which I obtain by dissolving, for 2-3 hours,
at a temperature of about 170°, a mixture of one molecule of paramidophenol
and one molecule of parasulphanilic acid. In the said specification I have stated
that this colouring matter dyes cotton blue in an alkaline bath.
Since then I have discovered that a prolonged melting, made at a higher
temperature, converts the blue into a darker colour, almost black.
In carrying out my improved process I heat in an oil bath, at 160-170°, in
an iron boiler, furnished with an agitator,
Parasulphanilic acid
Paramidophenol
17 kgs. 300 grms.
11 kgs.
The liquefied mass is maintained at this temperature for one hour, then it is
gradually raised to 250°, and maintained at this temperature from 4-5 hours.
The mass, which has become very thick is then taken out of the apparatus, cooled ...
and pulverized.
The pulverized product is then washed with a tepid solution of soda in the
proportion of 10, and dried.
It appears in the form of a gray powder, insoluble in water and dilute alkalinė
carbonates, soluble into blue-black in dilute caustic alkalies, into dark gray-blue
in, alkaline sulphurets, insoluble in acids, soluble into blue in alcohol. It dyes
cotton a blue-black in a bath of highly diluted caustic soda and sea salt, a richer
blue-black in a bath of sulphuret of sodium and sea salt. The passage into the
oxidizing bath of bichromate and acid does not visibly change the shade.
It differs, as is apparent, from the blue product described in the specification
of the aforesaid former application, by being insoluble in alkaline carbonates,
by its superior colouring power, and by its very different shade. Finally it is to be
noted that it dissolves into blue in alcohol, while the product of my first application
dissolved into red.
Dated this 10th day of March 1898.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.

page_text: 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:-
In the Specification of my former Application of March 13th 1897 No. 6694 I
have described a blue colouring matter which I obtain by dissolving, for 2-3 hours,
at a temperature of about 170°, a mixture of one molecule of paramidophenol
and one molecule of parasulphanilic acid. In the said specification I have stated
that this colouring matter dyes cotton blue in an alkaline bath.
Since then I have discovered that a prolonged melting, made at a higher
temperature, converts the blue into a darker colour, almost black and it is this
feature which forms the subject of the present application.
In carrying out my improved process I heat in an oil bath, at 160-170°, in
an iron boiler. furnished with an agitator,
Parasulphanilic acid.
Paramidophenol
-
-
17 kgs. 300 grms.
11 kgs.
The liquefied mass is maintained at this temperature for one hour, then it is
gradually raised to 250°, and maintained at this temperature for 4-5 hours.
The mass, which has become very thick is then taken out of the apparatus, cooled
and pulverized.
The pulverized product is then washed with a tepid solution of soda in the
proportion of 10, and dried.
It appears in the form of a gray powder, insoluble in water and dilute alkaline
carbonates, soluble into blue-black in dilute caustic alkalies, into dark gray-blue
in alkaline sulphurets, insoluble in acids, soluble into blue in alcohol. It dyes
cotton a blue-black in a bath of highly diluted caustic soda and sea salt, a richer
blue-black in a bath of sulphuret of sodium and sea salt. The passage into the
oxidizing bath of bichromate and acid does not visibly change the shade.
It differs, as is apparent, from the blue product described in the specification
of the aforesaid former application by being insoluble in alkaline carbonates,
by its superior colouring power, and by its very different shade. Finally it is to be
noted that it dissolves into blue in alcohol, while the product of my first application
dissolved into red.
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:
The prolonged action, at a high temperature, of parasulphanilic acid on
paramidophenol, for the purpose of obtaining a blue black colouring matter, dyeing
vegetable fibres into blue black shades in bath of caustic or of sulphurets of sodium.
Dated this 17th day of November 1898.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.