Improvement in the Manufacture of Colouring Matters.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
Improvement in the Manufacture of Colouring Matters.
I, JAMES YATE JOHNSON, of 47, Lincoln's Inn Fields, in the County of London,
Gentleman, do hereby declare the nature of this invention (which has been
communicated to me from abroad by the Badische Anilin & Soda Fabrik of
Ludwigshafen-on-Rhine, in the German Empire) to be as follows:-
In the Application for Letters Patent No. 20063 of the 21st September 1898
there are described a new colouring-matter intermediate product obtained from
one molecular proportion each of formic aldehyde and meta-toluylene-diamine,
a method of producing the same, and also a method of producing new colouring-
matter therefrom.
My foreign correspondents have now discovered that the said intermediate
product (which they term diamido-toluyl-alcohol) can be employed for the pro-
duction of colouring-matters by treating the said intermediate product (diamido-
toluyl-alcohol) with beta-naphthol and ferric chloride.
The following is an example of a mode of proceeding in accordance with this
invention, but the invention is not limited to this example:-
EXAMPLE.
With 95 parts of the intermediate product (diamido-toluyl-alcohol) obtained
from one molecular proportion each of formaldehyde and meta-toluylene-dia-
mine, grind one hundred and thirty parts of crystallised ferric chloride and add
this mixture to one hundred and fifty parts of molten beta-naphthol at a
temperature of 140° Centigrade, whilst stirring. Heat for about two hours.
whilst stirring, at a temperature of from 150 to 170° Centigrade. The melt
becomes darker and thicker. Pulverise the melt, when cold, and extract the
dye by boiling the powder with about fifteen thousand parts of water. Filter
from the insoluble resinous matters formed and precipitate the dye by means of
common salt solution. Purify the colouring-matter, if necessary, by treating
the hydrochloride so obtained with alkali, thus setting free the colour base,
recrystallize from boiling toluene and reconvert into the hydrochloride by means
of hydrochloric acid.
Dated this 21st dox of Juanat 1800

page_text: communicated to me from abroad by the Badische Anilin & Soda Fabrik of
Ludwigshafen-on-Rhine, in the German Empire) and in what manner the same
is to be performed to be particularly described and ascentained in and by the
following statement:
In the Specification of Letters Patent No. 20063 of the 21st September 1898
there are described a new colouring-matter intermediate product, obtained from
one molecular proportion each of formic aldehyde and meta toluylene-diamine,
a method of producing the same, and also a method of producing new colouring
maiter therefrom.
My foreign correspondents have now discovered that the said intermediate
product (which they term diamido-toluyl-alcohol) can be employed for the pro-
duction of colouring-matters by treating the said intermediate product (diamido-
toluyl-alcohol) with beta naphthol and ferric chloride.
The following is an example illustrating the best method with which I am
acquainted of proceeding in accordance with this invention but the invention is
not limited to this example:-
EXAMPLE.
With ninety five parts of the intermediate product (diamido-toluyl-alcohol)
obtained from one molecular proportion each of formaldehyde and meta-toluylene-
diamine, grind one hundred and thirty parts of crystallised ferric chloride and
add this mixture to one hundred and fifty parts of molten, beta-naphthol, at a
temperature of one hundred and forty degrees Centigrade whilst stirring.
Heat for about two hours, whilst stirring at a temperature of from one hundred
and fifty to one hundred and seventy degrees Centigrade. The melt becomes
darker and thicker. Pulverise the melt when cold and extract the dye by
boiling the powder with about fifteen thousand parts of water. Filter from
the insoluble resinous matters formed, and precipitate the dye by means of
common salt solution. Purify the colouring matter, if necessary, by treating
the hydrochloride so obtained with alkali, thus setting free the colour-base,
recrystallise from boiling toluene and re-convert into the hydrochloride by
means of hydrochloric acid.
In a similar manner the corresponding intermediate product obtained by the
condensation of one molecular proportion each of formaldehyde and meta-
phenylene-diamine (which my foreign correspondents term meta-diamido benzyl-
alcohol) can be employed, in place of meta-diamido toluykalcohol, for the
preparation of a similar colouring matter. The dye-stuff thus obtained dyes a
more greenish-yellow than the corresponding toluyl derivative.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed I declare that what I
claim is:
1. The manufacture of colouring matters by heating the condensation pro-
ducts of formaldehyde and a meta-diamine herein before set forth, with beta
naphthol, in the presence of ferric chloride.
2. The manufacture of colouring matters substantially as described in the
foregoing example.
Dated this 27th day of April 1900.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.