Manufacture of Black Colouring Matters Directly Dyeing Cotton.
Year: 1899

page_text: Date of Application, 9th June, 1899
Complete Specification Left. 3rd Mar, 1900-Accepted, 7th Apr., 1900
PROVISIONAL SPECIFICATION.
Manufacture of Black Colouring Matters Directly Dyeing Cotton.
I, CHARLES DENTON ABEL, of Birkbeck Bank Chambers, Southampton Build-
ings, in the County of London, Consulting Engineer and Chartered Patent
Agent, do hereby declare the nature of this invention (as communicated to me
from abroad by The Actien Gesellshaft für Anilin Fabrikation, of Berlin, in the
Empire of Germany, Chemical Manufacturers,) to be as follows:-
-
It is known that a black colouring matter directly dyeing cotton is obtained
by treating quinonechlorimide with a solution of hyposulphite in the presence
of mineral acids.
In carrying these researches further my foreign correspondents have now found
that colouring matters of quite similar character may also be obtained by
substituting in the above process for quinonechlorimide certain derivatives of the
same, such as for instance its halogen-, carboxyl-, sulpho-, nitro-, and amido-
derivatives, or by using, as starting products, quinonedichlorimide or derivatives
of the same. The invention is illustrated by the following example.
=
Chloro-quinonechlorimide obtained in the known manner from 6 parts by
weight of the hydrochloride of chloro-para-amidophenol (OH:CL: NH
1:2:4)
is suspended in a concentrated solution of 20 parts of sodium hyposulphite.
200 parts of diluted sulphuric acid containing 33 per cent. of H₂SO, are added
to the mixture which is thereupon slowly heated to boiling.
The black colouring matter, which is separated during the process, is purified
by dissolving it in a solution of sodium carbonate or diluted soda lye, filtering
off and precipitating the dyestuff from the filtrate by means of common salt.
The product thus obtained dyes unmordanted cotton deep black shades.
==
Colouring matters of similar character, the shade of which is somewhat more
brown-black, are obtained by using in the above process. instead of chloro-
quinone-chlorimide. equivalent quantities of quinonechlorimide-carboxylic acid
(obtained from amidosalicylic acid OH: COOH.NH = 1:2:4), quinonechlorimide-
sulphonic acid. (obtained from p-amidophenolsulphonic acid OH SO₂H: NH,
1:2:4). nitroquinonechlorimide (obtained from nitro-p-amidophenol OH: NO, NH,
1:2:4). amidoquinonechlarimide (obtained from amido-p-amidophenol
OH:NH, NH, 1:2:4) quinonedichlorimide (obtained from p-phenylenedia-
mine) or nitroquinonedichlorimide (obtained from nitro-p-phenylenediamine).
===
=3
Dated this 9th day of June 1899
ABEL & IMRAY,
Agents for the Applicant.

page_text: Chloro-quinonechlorimide obtained in the known manner from 6 parts by
weight of the hydrochloride of chloro-para-amidophenol (OH: Cl: NH=1:2:4)
is suspended in a concentrated solution of 20 parts of sodium hyposulphite.
200 parts of diluted sulphuric acid containing 33 per cent. of FLSO, are added
to the mixture which is thereupon slowly heated to boiling.
The black colouring matter, which is separated during the process, is purified
by dissolving it in a solution of sodium carbonate or diluted soda lye, filtering
off and precipitating the dyestuff from the filtrate by means of common salt.
The product 'thus obtained dyes unmordanted cotton deep black shades..
EXAMPLE II.
Quinonedichlorimide obtained in the known manner from 50 parts by weight
of paraphenylenediamine is suspended in a concentrated solution of 100 parts of
sodium hyposulphite; 1,000 parts of sulphuric acid containing 33 per cent. H₂SO.
are added thereto, and the mixture is slowly heated to boiling. The product
of the reaction separates during the process. The dyestuff is isolated in the way
described in the Example I. It dyes unmordanted cotton in a bath containing
sodium sulphide deep black shades.
Colouring matters of similar character, the shade of which is somewhat more
brown-black are obtained by using in, the above process instead of chloroquinone-
chlorimide or quinonedichlorimide equivalent quantities of quinonechlorimide-
carboxylic acid (obtained from amidosalicylic, acid OH COOH: NH,= 1:2:4),
quinonechlarimidesulphonic acid (obtained from para-amidophenolsulphonic
acid OH: SO₂H: NH=1:2:4), nitro-quinonechlorimide (obtained from nitro-para-
amidophenol OH NO, NH, 1:2:4). amidoquinonechlorimide (obtained from
amido-para-amidophenol OH: NH, NH, = 1:2:4) or nitroquinonedichlorimide
(obtained from nitro-para-phenylenediamine).
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I wish it to be

page_text: understood that it has been proposed to produce black colouring matters which
dye cotton directly from a sodium sulphide bath by acting upon paranitro-
sophenol, paranitrosoaniline, or similar quinonoid compounds with two mole-
cular proportions of a thiosulphate in weak acid solution, heating the dithio-
sulphonic acid thus produced with quinone-chlorimide, and ultimately boiling
the intermediate product so formed in acid solution, such processes being carried
out successively or simultaneously in the same solution, and I make no claim
to such invention, but I declare that what I claim is:
1. The herein described manufacture of black colouring matters directly dyeing
cotton by treating with hyposulphites in the presence of mineral acids substitu-
tion products of quinonechlorimide, such as halogen-, carboxyl-. sulpho-, nitro-
or amido substitution products, or quinonedichlorimide or derivatives thereof.
2. The colouring matters manufactured as above set forth.
Dated this 3rd day of March 1900
ABEL & IMRAY,
Agents for the Applicant.