The Manufacture and Production of New Black Colouring Matter, and the Production of Black Colour on Vegetable Fibre.
Year: 1894

page_text: Date of Application, 22nd Nov., 1894
Complete Specification Left, 12th Sept., 1895-Accepted, 12th Oct., 1895
PROVISIONAL SPECIFICATION.
The Manufacture and Production of New Black Colouring Matter,
and the Production of Black Colour on Vegetable Fibre.
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 and Soda Fabrik
of Ludwigshafen-on-Rhine, in the Empire of Germany) to be as follows:-
In the Specification of Letters Patent No. 10996 of 1893 granted to me the
manufacture of ner colouring matters from 1.1' dinitro naphthalene is described.
The said colouring matters are produced by the action of certain reducing agents
upon this dinitro body under conditions described in the said Specification. Thus
by the action of sodium sulphide under different conditions two colouring matters
are obtained which are termed dyes B and C respectively. In ordinary manu-
facture these dyes are usually obtained admixed with one another.
My foreign correspondents have discovered that if "dye B" be heated with
This
caustic soda solution it is converted into a new black colouring matter.
differs from dye B which is insoluble in water and practically insoluble in cold
The solution
caustic alkali in being very readily soluble in cold alkaline water.
of the new colouring matter possesses the novel and exceedingly valuable property
of dyeing directly in the cold unmordanted vegetable fibre in very fast shades.
My foreign correspondents have also found that the alkaline solution of dye C
can also be used in this way. Hence if a mixture of dye; B and dye C be heated
with caustic soda solution the new direct dyeing colouring matter is obtained and
the resulting mixture can at once be used for dyeing purposes in the cold without
the aid of a mordant.
In actual manufacture the production of the dye B whether alone or in admixture
with dye C and the conversion into the new product can readily be united into
one process in which the final operation is the digestion with caustic alkali herein-
before mentioned.
The following examples will serve to illustrate the nature of the invention, but
I do not confine myself to the details given as the proportions, strength of alkali
and temperatures can be considerably varied without departing from the nature of
the invention.
1
EVANDIT 1
Dnacts Containing about thirty per cent.
bout hundred parts of dye D is pacto (containing about thirty per cent.
dye B either alone or adinixed with dye C), and about one hundred parts of
caustic soda lye (containing about twenty three per cent. NaOH) and digest the
mixture for about one hour on the boiling water-bath. A blue-violet solution
results, this can be used without further treatment for dyeing purposes or the liquid
can be evaporated, the dry product constituting a black powder readily soluble in
Excess of alkali does not
cold water giving a blue-violet to black solution.
precipitate the dye but mineral acids give a black precipitate. The dye dissolve
in concentrated sulphuric acid giving a dirty green coloured solution,

page_text: The following example describes the preparation of dye B (containing some
dye C) and its conversion into the new direct dyeing colouring matter.
EXAMPLE 2.
Mix together about fifty parts of the 1.1' dinitro-naphthalene and about ten
thousand parts of water, boil the mixture and add about two hundred and fifty
parts of sodium sulphide (Na,S +9 Aq) boil for about half an hour or until no
dinitro-naphthalene remains unchanged. Filter, add to the violet solution obtained
about five hundred parts of hydrochloric acid (containing about thirty per cent. real
acid) boil two hours longer, filter, and wash. Mix the washed residue with
sufficient water to produce a thirty per cent. paste, and add to this paste half its.
weight of caustic soda solution (containing about twenty three per cent. NaOH)
and digest the mixture for about one hour on the boiling water bath, as described
in Example 1.
To produce black colour on cotton or other vegetable fibre with the new
colouring matter or with the alkaline solution of dye C or mixtures thereof the
cotton or other vegetable fibre is padded for about half an hour with a cold solution
of the colouring matter taken. The cotton or other vegetable fibre is then washed
and dried. A solution of one part of the new dye containing dye C in forty five
parts water gives a dead black on ten parts of cotton stuff.
A similar blue-black dye-stuff can be obtained by digesting with caustic alkali
the viclet dye obtained by Troost by treating dinitro-naphthalene with sodium..
sulphide.
Dated this 22nd day of November 1894.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.
The Manufacture and Production of New Black Colouring Matter,
and the Production of Black Colour on Vegetable Fibre.
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 Empire of Germany) 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 Letters Patent No. 10996 of 1893 granted to me the
manufacture of new colouring matters from 1.1' dinitro-naphthalene is described.
The said colouring matters are produced by the action of certain reducing agents
upon this dinitro body under conditions described in the said Specification. Thus
by the action of sodium sulphide under different conditions two colouring matters
are obtained which are termed dyes B and C respectively. In ordinary
manufacture these dyes are usually obtained admixed with one another.
My foreign correspondents have discovered that if "dye B" be heated with caustic
soda solution or other strongly alkaline solution such as a solution of caustic potash
or of sodium sulphide it is converted into a new black colouring matter. This
differs from the said dye B (which is insoluable in water and practically insoluble
in cold caustic alkali) in being very readily soluble in cold alkaline water.
solution of the new colouring matter possesses the novel, and exceedingly valuable
property of dyeing, directly in the cold, unmordanted vegetable fibre the dye being
very fast.
The
My foreign correspondents have also found that, the alkaline solution of dye C

page_text: of dye B either alone or admixed with dye C) and about one hundred parts of
caustic soda lye (containing about twenty three per cent. NaOH) and digest the
mixture for about one hour on the boiling water bath. A blue-violet solution
results and this can be used for dyeing purposes without further treatment or the
liquid can be evaporated the dry product constituting a black powder readily
soluble in cold water giving a blue-violet to black solution. Excess of alkali does
not precipitate the dye but mineral acids give a black precipitate. The
dye dissolves in concentrated sulphuric acid giving a dirty green coloured
solution.
The following example describes the preparation of dye B (containing some
dye C) and its conversion into the new direct dyeing colouring matter in one
continuous process.
EXAMPLE II.
Mix together about fifty parts of the 1.1' dinitro-naphthalene and about ten
thousand parts of water, boil the mixture and add about two hundred and fifty
parts of sodium sulphide (Na,S+9 Aq). Boil this mixture for about half an hour,
or until no dinitro-naphthalene remains unchanged. Filter, add to the violet
solution obtained about five hundred parts of hydro-chloric acid (containing about
thirty per cent. real acid) boil two hours longer, filter and wash. Mix the washed
residue with sufficient water to produce a thirty per cent. paste, and add to this paste
half its weight of caustic soda solution (containing about twenty three per cent.
NaOH) and digest the mixture for about one hour on the boiling water-bath as
described in Example I. To produce black colour on cotton, or other vegetable
fibre by means of the aforesaid new colouring matter, or of the alkaline solution of
dye C or mixtures thereof, the cotton, or other vegetable fibre is padded for about
half an hour with a cold solution of the colouring matter taken. The cotton, or
other vegetable fibre is then washed and dried. A solution of one part of the
new dye containing dye C in forty five parts water gives a dead black on ten parts
of cotton stuff.
A similar blue black dyestuff can be obtained by digesting with caustic alkali
the violet dye obtained by Troost by treating dinitro-naphthalene with sodium
sulphide.
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 new soluble black colouring matters by treating the
colouring matters derived from 1.1' dinitro naphthalene hereinbefore defined with

page_text: caustic soda, or other strongly alkaline solution substantially as hereinbefore set
forth.
2. The manufacture of new soluble black colouring matters by uniting the
production of the colouring matters derived from 1.1' dinitro-naphthalene herein-
before defined and the conversion thereof into the new products in one process in
which the final operation is the digestion with caustic alkali substantially as
herein before set forth.
3. The manufacture of the new soluble black colouring matters in the manners
herein before described in the examples.
4. As new articles of manufacture the soluble black colouring matters herein-
before described and such as can be obtained substantially as hereinbefore set
forth.
5. The application of the new soluble black colouring matters claimed by the
preceding claiming clauses to the production of black colour on vegetable fibre by
dyeing unmordanted vegetable fibre directly in the cold substantially in the
manner herein before set forth.
Dated this 12th day of September 1895.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.