Improvements in the Manufacture of Colouring Matters.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I, ROBERT BOLTON RANSFORD, of 41, Waldegrave Road, Upper Norwood, in the
County of Surrey, Gentleman, do hereby declare the nature of this invention
(which has been communicated to me from abroad by Leopold Cassella & Com-
pany, of Frankfort-on-Main, in the Empire of Germany,) to be as follows:-
If the dinitro oxydiphenylamine obtained from 1.3.4. dinitrochlorbenzene and
1.4 amidophenol is heated with caustic alkalis in an aqueous solution, it is com-
pletely transformed into a brown substance. The constitution of this body
has not yet been ascertained, but it must differ very considerably from the gene-
rating material. For whereas the latter when heated with alkaline sulphides
and sulphur yields an intense black colouring matter-the known "immedial
black" the transformed product when treated in a like manner yields a charac-
teristic yellowish brown colouring matter. The homologous dinitrophenyl_oxy-
tolylamine from dinitrochlorbenzene and amido-o-cresol (CH, OH; NH,
:
1: 2: 5) behaves in a similar way.
=
Example 1: 40 kilos. dinitro oxydiphenylamine, dissolved in 80 kilos. caustic
soda lye 40° Bé. and 240 litres water, are boiled for from 3 to 4 hours, until no
more ammonia is evolved. The solution is then diluted with water and the body
formed is precipitated by slightly acidulating with muriatic acid. This body,
when dry, is black amorphous powder.
25 kilos. of the same
are heated either with 50 kilos. caustic soda lve 40° Bé. and 20 kilos. sulphur or
with 52 kilos. sulphide of sodium and 13 kilos. sulphur, with the addition of
some water, and the temperature is gradually raised to about 160° C. The mass
finally becomes dry. The melt is used directly for dyeing.
a
Example 2: 25 kilos. dinitrophenyl oxytolylamine are boiled together with
50 kilos. caustic soda lye 40° Bé. and 150 litres water for several hours, then
The
20 kilos. sulphur are introduced and the temperature raised to 160° C.
dried melt is used directly for dyeing.
The dyestuffs thus obtained dissolve easily in water. They are precipitated by
acids and may be again dissolved with caustic alkalis or sulphide of sodium.
They dye cotton an intense yellowish brown, especially in a warm bath contain-
ing common salt. An after-treatment with chromates changes the shade towards
yellow and increases the fastness.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I, ROBERT BOLTON RANSFORD, of 41, Waldegrave Road, Upper Norwood, in the
County of Surrey, Gentleman, do hereby declare the nature of this invention
[Price 8d.l

page_text: (which has been communicated to me from abroad by Leopold Cassella & Com-
pany, of Frankfort-on-Main, 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:-
If the dinitro oxydiphenylamine obtained from 1.3.4. dinitrochlorbenzene and
1.4 amidophenol is heated with caustic alkalis in an aqueous solution, it is com-
pletely transformed into a brown colouring matter. The constitution of this body
has not yet been ascertained, but it must differ very considerably from the gene-
rating material. For whereas the latter when heated with alkaline sulphides
and sulphur yields an intense black colouring matter the known "immedial
black "the transformed product when treated in a like manner yields a charac-
teristic yellowish brown colouring matter. The homologous dinitrophenyl oxy-
tolylamine from dinitrochlorbenzene and amido-o-cresol (CH₂: OH; NH₂
1: 2: 5) behaves in a similar way.
-
Example 1 40 kilos. dinitro oxydiphenylamine, dissolved in 80 kilos. caustic
soda lye 40° Bé. and 240 litres water, are boiled for from 3 to 4 hours, until no
more ammonia is evolved. The solution is then diluted with water and the body
formed is precipitated by slightly acidulating with muriatic acid. This body,
when dry, is a black amorphous powder. It dissolves easily in presence of alkalis
and dyes on unmordanted cotton intense brown shades. 25 kilos. of the same
are heated either with 50 kilos. caustic soda lye 40° Bé. and 20 kilos. sulphur or
with 52 kilos. sulphide of sodium and 13 kilos. sulphur, with the addition of
some water, and the temperature is gradually raised to about 160° C. The mass
finally becomes dry. The melt is used directly for dyeing.
Example 2; 25 kilos. dinitrophenol oxytolylamine are boiled together with
50 kilos. caustic soda Ive 40° Bé. and 150 litres water for several hours, then
20 kilos. sulphur are introduced and the temperature raised to 160° C. The
dried melt is used directly for dyeing.
The dyestuffs thus obtained dissolve easily in water. They are precipitated by
acids and may be again dissolved with caustic alkalis or sulphide of sodium.
They dye cotton an intense yellowish brown, especially in a warm bath contain-
ing common salt. An after treatment with chromates changes the shade towards
yellow and increases the fastness.
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
1. The manufacture of colouring matters by heating dinitro oxy dialphyl-
amines, obtained by the action of dinitrochlorbenzene on p. amido-phenol or p.
amidocresol, with caustic alkalis substantially as described.
2. The manufacture of colouring matters from the products resulting from
the process above claimed by heating such products with alkaline sulphides and
sulphur substantially as described.
3. The new colouring matters herein before described.
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