Method for the Production of Fast Colours on the Wool Fibre from Pioramic Acid Monoazo Dyestuffs.
Year: 1898

page_text: Date of Application, 4th Aug., 1898
Complete Specification Left. 4th May, 1899-Accepted, 1st July, 1899
PROVISIONAL SPECIFICATION.
Method for the Production of Fast Colours on the Wool Fibre from
Pioramic Acid Monoazo Dyestuffs.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings,
Chancery Lane, in the County of London, Chartered Patent Agent, do hereby
declare the nature of this invention (as communicated to me from abroad by The
Farbwerke vormals Meister Lucius and Brüning, of Hoechst a/Main, in the
Empire of Germany, Chemical Manufacturers) to be as follows:-
My correspondents have found that monoazo dyestuffs derived from the action of
diazotised picramic acid on the sulphonic acids (naphthylamin, naphthol, dioxy
and amido-oxy naphthalenes) are transformed into exceedingly fast tints by treat-
ing subsequently with chromates or chromium salts the shades obtained on wool
in an acid bath, comprising tints from red-brown and brown to black and green.
In contrast to the methods previously described for producing on the fibre
colours fast to milling and washing by means of oxidation, and where the forma-
tion of lakes takes place only by the action of simultaneous oxidising chromates
or bichromates on the monoazo-dyestuffs there employed, it appears that with
monoazo dyestuffs derived from picramic acid, the production of colours fast to
milling and washing is caused in the first place by a simple formation of lake.
These dyestuffs are transformed in many cases on the fibre in an acid bath by
chromium salts, for instance, chromium fluoride, into lakes fast to milling and
washing; in other cases the formation of lakes takes place even if the dyeing
follows the mordanting with chrome.
The formation of lake is fairly independent of the second component, the
sulphonic acid of a naphthylamin, naphthol, dioxy and amido oxy naphthalenes
coupled with picramic acid, the latter having a decisive influence only upon
the tint of the shade. The reason for this remarkable fact may be looked for in
the hydroxyl of the picramic acid being in "ortho" position to the combining azo
group, and the power of the lake formation is all the more astonishing, as a for-
ination of lake seemed to be entirely excluded according to the present views
based upon the researches of Kostanecki.
I will illustrate the above described method by the following examples:-
I BROWN ON 2 PIECES =40 KILOS ESKIMO.
The bath is made un to 1000 litres of water, the solution of 1 kilo. 600 grammes
ŋhe hath is made up to 1000 litres of water, the solution of 1 kilo. 600 grammes
of the monoazo dyestuff from diazotised pieramic acid and naphthylamin sulphonic
acid 1.7, 40 kilos. crystallised Glauber's salt, and 1.6 kilo. sulphuric acid of
66° Bé; the wetted goods are entered at a medium temperature, raised to the
boil in an hour, boiled 1 hour; to the bath is added 1.200 kilo. bichromate of
potassium (or bichromate of sodium) and the formation of lake is completed by one
"

page_text: the monoazo dyestuff from diazotised picramic acid and 2.5 ethylamidonaphthol-8-
sulphonic acid, 25 kilos. crystallised Glauber's salt and 2 kilos. sulphuric acid;
the well wetted wool is entered at a medium temperature, raised to the boil in
an hour, boiled 1 hour, whereupon the solution of 750 grammes of bichromate
of potassium is sprinkled over the dye-fluid and the dye developed by one hour's
boil.
III. DARK-OLIVE ON 40 KILOS, CHEVIOT YARN.
The bath is made up to about 1500 litres of water, 40 kilos. crystallised
Glauber's salt, 1.6 kilo. sulphuric acid and the solution of 1 kilo 400 grammes
of the monoazo dyestuff from diazotised picramic acid and 2.5 naphthylamin
sulphonic acid; the well wetted yarn is entered at a medium temperature, raised
to the boil and boiled 1 hour, whereupon the solution of 1.6 kilo. of chromium
fluoride is added and the colour developed by one hour's boil.
Dated this 4th day of Amat 1900
ABEL & IMRAY,
Agents for the Applicant.
Method for the Production of Fast Colours on the Wool Fibre from
Picramic Acid Monoazo Dyestufts.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings,
Chancery Lane, in the County of London, Chartered Patent Agent, do hereby
declare the nature of this invention (as communicated to me from abroad by The
Farbwerke vormals Meister Lucius and Brüning, of Hoechst a/Main, in the
Empire of Germany, Chemical Manufacturers) and in what manner the same is
to be performed, to be particularly described and ascertained in and by the follow-
ing statement:-
-
My correspondents have found that monoazo-dyestuffs derived from the action of
diazotised picramic acid on the sulphonic acids (naphthylamine, phenylene and
toluylene diamines, amidophenol and amidocresol, naphthol, dioxy-, diamido- and
amido-oxy-naphthalenes) are transformed into exceedingly fast tints by treating
subsequently with chromates or chromium salts the shades obtained on wool in an
acid bath, comprising tints from red-brown and brown to black and green.
In contrast with the methods previously described for producing on the fibre
colours fast to milling and washing by means of oxidation, and where the forma-
tion of lakes takes place only by the action of simultaneous oxidising chromates
or bichromates on the monoazo-dyestuffs there employed, it appears that with
monoazo-dyestuffs derived from pieramic acid, the production of colours fast to
milling and washing is caused in the first place by a simple formation of lake.
These dyestuffs are transformed in many cases on the fibre in an acid bath by
chromium salts, for instance, chromium fluoride, into lakes fast to milling and
washing, in other cases the formation of lakes takes place even if the dyeing
follows the mordanting with chrome.
The formation of lake is fairly independent of the second component, the
sulphonic acid of a naphthylamine, naphthol, dioxy-, diamido- and amido-oxy-
naphthalenes, phenylene and toluylene diamines, coupled with pieramic acid, the
latter having a decisive influence only upon the tint of the shade. The reason for
this remarkable fact may be looked for in the hydroxyl of the picramic acid being
in ortho" position to the combining azo-group and the power of the lake
formation is all the more astonishing as a formation of lake seemed to be entirely
excluded according to the present views based upon the researches of Kostanecki.
*

page_text: I will illustrate the above described method by the following examples:-
I. BROWN ON 2 PIECES = 40 KILOS ESKIMO.
The bath is made up to 1000 litres of water, and consists of a solution of
1 kilo. 600 grammes of the monoazo-dyestuff from diazotised picramic acid and
1:7-naphthylamin sulphonic acid, 40 kilos. crystallised Glauber's salt, and
1.6 kilo. sulphuric acid of 66° Bé.; the wetted goods are entered at a medium
temperature, raised to the boil in an hour, boiled 1 hour; to the bath is added
1.200 kilo. bichromate of potassium (or bichromate of sodium) and the formation
of lake is completed by one hour's boil.
II. BLACK ON 50 KILOS LOOSE WOOL.
The bath is made up to about 1200 litres of water, and consists of a solution
of 2 kilos. of the monoazodyestuff from diazotised pieramic acid and 2:5-ethyl-
amidonaphthol-8 -sulphonic acid, 25 kilos. crystallised Glauber's salt and 2 kilos.
sulphuric acid; the well wetted wool is entered at a medium temperature, raised
to the boil in an hour, boiled 1 hour, whereupon the solution of 750 grammes
of bichromate of potassium is sprinkled over the dye-fluid and the dye developed
by one hour's boil.
III. DARK-OLIVE ON 40 KILOS. CHEVIOT YARN.
The bath is made up to about 1500 litres of water, 40 kilos. crystallised
Glauber's salt, 1.6 kilo. sulphuric acid and the solution of 1 kilo. 400 grammes
of the monoazodyestuff from diazotised picramic acid and 2.5 naphthylamine
sulphonic acid; the well wetted yarn is entered at a medium temperature, raised
to the boil and boiled 1 hour, whereupon the solution of 1.6 kilo. of chromium
fluoride is added and the colour developed by one hour's boil.
Having now particularly described and ascertained the nature of this
invention and in what manner the same is to be performed, I declare that what
I claim is:-
Method for the production of fast colours from pieramic acid monoazodyestuff's
on the wool fibre, by dyeing the fibre with the monoazodyestuffs, obtained by the
action of diazotised picramic acid on the sulphonic acids of naphthylamines,
naphthols, dioxy-, diamido- and amidooxy-naphthalenes, m-phenylene and m-toluy-
lenediamines, amidophenols and amidocresols in an acid bath and subsequently
treating them in the same or in a second bath with chromates, bichromates,
chromic acid or chromium oxide salts, substantially as described.
Dated this 4th day of May 1899.
ABEL & IMRAY,
Agents for the Applicant.