THE PRODUCTION OF COLOURING MATTERS FROM THE SULPHONIC ACIDS OF THE PHENOLS AND THE DIAZO-SULPHONIC ACIDS OF THE AMINES
Year: 1879

page_text: LETTERS PATENT to Raphael Meldola, Chemist, of the Firm of Brooke,
Simpson, and Spiller, of Atlas Works, Hackney Wick, in the County of
Middlesex, for the Invention of "THE PRODUCTION OF COLOURING MATTERS
FROM THE SULPHONIC ACIDS OF THE PHENOLS AND THE DIAZO-SULPHONIC
ACIDS OF THE AMINES."
Sealed the 1st August 1879, and dated the 10th May 1879.
PROVISIONAL SPECIFICATION left by the said Raphael Meldola at the
Office of the Commissioners of Patents on the 10th May 1879.
"
RAPHAEL MELDOLA, Chemist, of the Firm of Brooke, Simpson, and Spiller, of
Atlas Works, Hackney Wick, in the County of Middlesex. THE PRODUCTION
OF COLOURING MATTERS FROM THE SULPHONIC ACIDS OF THE PHENOLS AND THE
DIAZO-SULPHONIC ACIDS OF THE AMINES."
According to the present Invention new descriptions of the colours known as
"diazo-colours" are produced which contain three or more groups of the radical
HSO, (known to chemists as hydrosulphuryl) instead of only two such groups as
heretofore.
The method employed for this purpose consists in the formation of compounds
by the action of the diazo-sulphonic acids of the amines (such as aniline, toluidine,
xylidine, cumidine, and naphthylamine) on the sulphonic acids of the phenols (such
as resorcine napthole and carbolic acid). The colours thus obtained are valuable
dye-stuffs of various shades of orange and scarlet.
The nature of my Invention will be explained by the following processes :-
Manufacture of Orange Colouring Matter.-Ten parts of sulphanilic acid are
dissolved in twenty times their weight of water, and to the cold solution four parts
of pure nitrate of soda are added, and then sixteen to eighteen parts of commercial
hydro-chloric acid. The solution of diazo-sulphanilic acid thus obtained is poured
into a solution containing nineteen parts of the sodium salt of the disulphonic acid
of betanaphthol dissolved in about eight times its weight of water. Ammonia is .
then added to the mixed solutions till an alkaline reaction is exhibited. The
colouring matter is salted out, filtered, and pressed; after one more solution and
salting out it is collected and dried, and is then ready for use.
Manufacture of Scarlet Colouring Matter.-Ten parts of xylidine-sulphonic acid
(prepared by pouring xylidine into four times its weight of fuming sulphuric acid)
D..

page_text: are dissolved in three hundred parts of water, and to the solution three and a half
parts of pure nitrate of soda are added, and sixteen to eighteen parts of commercial
hydrochloric acid. A solution of sixteen parts of the sodium salt of betanaph-
thol-disulphonic acid in about four times its weight of water is then prepared, and
into this when cold the solution of diazoxylidine-sulphonic acid prepared as above
described is poured, and the mixed solutions made alkaline with ammonia. The
colour is formed immediately, and after being salted out is treated in the same
manner as above described for the manufacture of the orange colouring matter.
These two examples are illustrations of my said Invention of the manufacture of
diazo-colours containing three or more HSO, (hydrosulphuryl) groups. I wish it
to be understood that I do not limit myself to the above method of introducing the
HSO, (hydrosulphuryl) groups into the "diazo" colours, as the same end can be
attained, for example, by starting with betanopthol-trisulphonic acid, and acting
upon this with the chlorides of diazobenzine and its homologues, such as dia-zocumine.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Raphael Meldola in the Great Seal Patent Office on the 29th
October 1879.
RAPHAEL MELDOLA, Chemist, of the Firm of Brooke, Simpson, and Spiller, of
Atlas Works, Hackney Wick, in the County of Middlesex. "THE PRODUCTION
OF COLOURING MATTERS FROM THE SULPHONIC ACIDS OF THE PHENOLS AND THE
DIAZO-SULPHONIC ACIDS OF THE AMINES."
According to the present Invention new descriptions of the colours known as
" diazo-colours are produced which contain three or more groups of the radical
HSO, (known to chemists as hydrosulphuryl) instead of only two such groups as
heretofore. The method employed for this purpose consists in the formation of com-
pounds by the action of the diazo-sulphonic acids of the amines (such as aniline,
toluidine, cumidine, and napthylamine) on the sulphonic acids of the phenols (such
as resorcine napthol and carbolic acid). The colours thus obtained are valuable
dye-stuffs of various shades of orange and scarlet.
The following are examples of processes for the production of such colouring
matters according to my Invention:-
-
Manufacture of Orange Colouring Matter.-Ten parts of sulphanilic acid are
dissolved in twenty times their weight of water, and to the cold solution four parts
of pure nitrite of soda are added, and then sixteen to eighteen parts of commercial
hydrochloric acid. The solution of diazo-sulphanilic acid thus obtained is poured
into a solution containing nineteen parts of the sodium salt of the disulphonic acid
of betanapthol dissolved in about eight times its weight of water; ammonia is then
added to the mixed solutions till an alkaline reaction is exhibited. The colouring
matter is salted out, filtered, and pressed; after one more solution and salting out,
it is collected and dried, and it is then ready for use.
Manufacture of Scarlet Colouring Matter. Ten parts of xylidine-sulphonic acid
(prepared by pouring xylidine into four times its weight of fuming sulphuric acid)
are dissolved in three hundred parts of water, and to the solution three and a half
parts of pure nitrite of soda are added, and sixteen to eighteen parts of commercial
hydrochloric acid. A solution of sixteen parts of the sodium of salt of betanapthol-
di-sulphonic acid in about four times its weight of water is then prepared, and into
this when cold the solution of diazo-xylene-sulphonic acid prepared as above
described is poured, and the mixed solutions are made alkaline with ammonia.
The colour is formed immediately, and after being salted out is treated in the
same manner as above described for the manufacture of the orange colouring
inatter.
The two processes above described are examples of the manufacture according to
my Invention of diazo-colours containing three or more HSO, (hydrosulphuryl).
groups which might be introduced into the diazo-colours by other methods. For
example, betanapthol-trisulphonic acid might similarly be acted on by the chlorides
of diazo-benzene and its homologues such as diazo-cumene.
Having thus described the nature of my Invention, and in what manner the same
is to be performed, I claim,―
First. The manufacture of colouring matters containing three or more groups of
hydrosulphuryl radical by the action of diazo-sulphonic acids of amines on sulphonic
acids of phenols, substantially as herein described.
Second. The manufacture of orange colouring matter by producing and treating
as herein described a compound of diazo-sulphanilic acid with the sodium salt of
betanapthol-disulphonic acid.

page_text: Third. The manufacture of scarlet colouring matters by producing and treating,
as herein described, a compound of diazoxylene-sulphonic acid, or of diazo-cumene-
sulphonic acid, with the sodium salt of betanapthol-disulphonic acid.
In witness whereof, I, the said Raphael Meldola, have hereunto set my
hand and seal, this 28th day of October, in the year of our Lord One
thousand eight hundred and seventy nine.
RAPHAEL MELDOLA. (L.S.)