Year: 1888

page_text: [Communicated from abroad by Messrs. WIRTH & Co., of Frankfort on the Main, in
the Empire of Germany, acting as Agents of A. Leonhardt & Co., of Mülheim,
near Frankfort on the Main, in the Empire of Germany.]
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
Southampton Buildings, in the County of Middlesex do hereby declare the nature of
this invention to be as follows:-
This invention has for its object the production of certain colouring matters which
possess the property of dyeing cotton direct, and so as to resist the action of soap and
alkali.
The said invention comprises the treatment under heat of paranitrotoluolsulpho-acid
or its salts with caustic alkalies or caustic lyes in presence of suitable oxidizable
organic or mineral substances (for example glycorin, antimonious oxide, or the like),
and separating in a suitable manner the colouring matter formed.
When working with the acid or with a metallic salt of the acid, special care must
be taken that the alkali made use of shall be in excess, because it is necessary for the
reaction that free alkali shall be present.
When using a metallic salt of the acid, the metallic oxide.present can, of course,
serve as the oxidizable substance.
If the oxidizable substance is not already liquid it is advantageous to mix the
substances which are to undergo re-action with a dissolving or distributing
liquid.
Dated this 22nd day of February 1888.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.

page_text: general as follows, I dissolve or distribute paranitrotoluolsulpho-acid or a salt of this
acid, under addition of such oxidable substances, in water, or one of the above mentioned
liquid oxidable agents, for example spirit, glycerine, and heat the same with caustic
alkali until the formation of colouring-matter has terminated.
By employing more or less of the oxydable substances the shades of the colouring
matters obtained can be greatly varied.
In order to render the process better understood I give the following examples, to
which however I do not limit myself as they can be variously modified without
departing from the nature of the invention,
Example 1. Upon 10 kilogrammes of the sodium salt of paranitrotoluolsulpho-acid,
or an equivalent quantity of the free acid, are poured about 30 litres of spirit or
nethyl alcohol and heated in a vessel provided with an agitator and a reflux-cooler.
About 8 kilogrammes of caustic soda-lye of 40 degrees Baumé are then gradually
added and the whole is heated to ebullition. The colouring matter obtained is filtered,
pressed and dried.
Example 2. 10 kilogrammes of paranitrotoluolsulpho-acid are heated together with
about 20 kilogrammes of glycerine, and to the mixture is gradually added, at about
60 degrees centigrade, about 8 kilogrammes of caustic soda-lye of 40 degrees Baumé.
A powerful reaction which may occur, and which is accompanied by strong ebullition,
is inet by adding cold water or by externally cooling the vessel. The formation of
colouring matter is terminated in a short time. The thick paste obtained is gradually
introduced into about 100 litres of boiling salt-water which must be kept acid up to
the end, preferably by means of acetic acid. The colouring-matter thus separated is
filtered, pressed and dried.
Example 3. 20 kilogrammes of sodium salt of paranitrotoluolsulpho-acid and
4 kilogrammes of resorcine are dissolved in 60 litres of hot water, 20 kilogrammes
of caustic soda-lye of 40 degrees Baumé are added, and the mass is boiled up to the
end of the formation of the colouring matter. The colouring-matter is precipitated
by neutralization with an acid, and by the addition of common salt in the usual
manner.
Example 4. 5 kilogrammes of a naphthol are dissolved in 20 kilogrammes of caustic-
soda-lye of 40 degrees Baumé and 60 litres of water, 20 kilogrammes of the sodium
salt of paranitrotoluol-sulpho acid are added, heat being applied until the formation
of colouring matter is terminated. The colouring matter is then separated in the
usual manner.
The same process serves for the production of colouring-matters by means of
B naphthol Dioxynaphthalines and its sulpho acids.
Pyrogallic acid.
Resorcylic acid.
Oxynaphthoic acids.

page_text: Having now particularly described and ascertained the nature of my 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 :-
The process of producing colouring-matters fast to alkali which will dye cotton
yellow, orange to brown without mordant, by the action of suitable oxidable
substances and fix alkalies upon paranitrotoluolsulpho-acid, under heat substantially
as described.