Improvements in the Manufacture of Colouring Matter.
Year: 1891

page_text: Date of Application, 26th Sept., 1891
Complete Specification Left, 25th June, 1892-Accepted, 17th Sept., 1892
PROVISIONAL SPECIFICATION.
[Communicated from abroad by FRÉDÉRIC REVERDIN and CH. DE LA HARPE,
both of 9, Rue du Stand, Geneva, in the Republic of Switzerland.]
Improvements in the Manufacture of Colouring Matter.
I, HENRY HARRIS LAKE of the firm of Haseltine Lake & Co. Patent Agents,
45 Southampton Buildings in the County of Middlesex, do hereby declare the
nature of this invention to be as follows:-
This invention relates to the manufacture of a new colouring matter dyeing wool
violet black, by subjecting sulphoamidonaphthol CHOHA,H' HSO³ to the
(1) (2) (4)
action of an oxidizing agent and in particular to the action of the oxygen of the air
in presence of alkaline carbonates, carbonates of the alkaline earths or ammonia.
The sulphoamidonaphthol above mentioned is obtained by reduction of the
nitroso-derivative of sulphonaphthol 1.4.
In carrying the said invention into practice a solution consisting of 3 kilo-
grammes of sulphoamidonaphthol and 50 litres of water and containing 2.300 kilo-
grammes of carbonate of soda (solvay soda) is heated in an open vessel in a water
bath and stirred from time to time; the water which evaporates in the heating
during the first three hours is replaced, the heating being then continued until the
quantity of the solution is reduced to about 20 litres. Filtering is effected after
cooling the violet black colouring matter which is deposited in the form of a violet
black powder, whilst the liquor of filtration is coloured brown.
The colouring material thus obtained is dissolved with difficulty in cold water,
and easily dissolved in hot water. It is precipitated from its solutions by acids in
brown-red flakes which after some time assume a crystalline form, and become
green. It dissolves in concentrated sulphuric acid with green colouring, and water
precipitates it again from this solution.
This new colouring matter dyes in an acid bath unmordanted wool, or wool
unmordanted with chrome, violet black. The shades obtained resist the action of
light, fulling and soaping and may be considered black.
In the manufacture of this colouring matter the soda may be replaced by other
carbonates, such as carbonates of ammonia or of lime, or by ammonia.
A colouring matter possessing the same properties is produced by sulphonating
imido-oxy-naphthalin described by Liebermann (Liebig's Annalen, vol. 211,
page 55) and obtained by oxidation in the open air in presence of ammonia of
Bamido a naphthol. It is thus probable that the new colouring matter which forms
the subject of this invention is sulpho-imido-oxy-naphthalin of the constitution

page_text: DIECIFICATION.
Improvements in the Manufacture of Colouring Matter.
I HENRY HARRIS LAKE of the firm of Haseltine Lake & Co. Patent Agents
45 Southampton Buildings in the County of Middlesex do hereby declare the
nature of this invention and in what manner the same is to be performed, to
be particularly described and ascertained in and by the following statement :-
1 2
I have found that the amido-a-naphthol monosulpho acid 1, 2, 4 (C₁H₂O HN
H,SO,H) can be converted in solutions with alkaline carbonates or with alkaline
earths by the action of air and the oxidation caused thereby into a colouring matter.
This oxidation takes place very rapidly, when the current of air is introduced into
the heated solution while the latter is stirred.
It is immaterial according to my process what alkaline carbonate is used the
solutions may therefore be prepared with soda or ammonium carbonate or with
chalk or the like.
The colouring matter thus produced dissolves with difficulty in cold water but
dissolves rapidly in hot water. It dissolves in concentrated sulphuric acid with
a greenish colour and is completely precipitated in the form of flakes from such a
solution.
In boiling solutions which are slightly acidified it uniformly dyes unmordanted
wool or wool mordanted with chrome and the colours thus obtained will withstand
the action of light and fulling. The dark colours may be considered black.
Example-3 kilogrammes of amido-naphthol-sulpho acid are added to a solution
of 2 kilogrammes 300 grammes of calcined carbonate of soda in 50 litres of water,
this solution being heated in an open vessel in a boiling water bath while it is well
stirred. During the first three hours of the heating operation the evaporated
water is replaced from time to time and afterwards the evaporation proceeds until
a volume of about 20 litres is left when cooling takes place. The colouring matter
then separates as a violet black powder, the solution having a brown colour.
I filter thoroughly, wash out with cold water and dry the colouring matter.
The amido-naphthol-sulpho acid which I use is identical with that which König
obtained by reduction from the azo colouring matters which latter are prepared by
combining a diazo compound with a-naphol-sulpho-acid of the series 1, 4 or with
a-oxy-naphtho-sulpho-acid (Reports of the German Chemical Society vol. 23
page 806). This amido-naphtol-sulpho acid is however also obtained by reduction
by ordinary methods from the nitroso-derivative of a-naphthol-sulpho acid 1-4.
To prepare this nitroso-derivative I may proceed in two different manners:
(1) Direct nitrosation of an aqueous solution of a naphthol-sulpho acid 1.4.
(2) Action of nitrous acid on a solution of the oxynaphtoicsulphoacid (Reports
of the German Chemical Society vol. 22 page 787) whereby the carboxyl group
is eliminated and replaced by NOH.
n
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed as communicated to me by
my foreign correspondents I declare that what I claim is :—
A
process for the preparation of a violet black colouring matter from aqueous
bolutions of amido-a-naphtholmonosulpho acid 1, 2, 4 with alkaline carbonates or
alkaline earths by the action of the oxygen of the air.
Dated this 25th day of June 180D
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.