Improvements in the Manufacture of Colouring Matters.
Year: 1898

page_text: Date of Application, 17th Aug., 1898
Complete Specification Left. 17th May, 1899-Accepted, 1st July, 1899
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
We, READ HOLLIDAY & SONS LIMITED, of 11, Cambridge Buildings, Upperhead
Row, Huddersfield, in the County of York, Manufacturing Chemists, JOSEPH
TURNER, of Spink Field Road, Birkby, Huddersfield, JAMES TURNER, of Hudders-
field, and HARRY DEAN, of Greenhead Road, Huddersfield aforesaid Chemists, do
hereby declare the nature of this invention to be as follows:-
-
We have discovered that para amido phenol when heated with sulphur yields
colours which vary in shade and solubility according to the proportion of sulphur
employed and the temperature to which the mass is raised.
If the proportion of sulphur be small say 5 parts to 10 parts para amido phenol
and the temperature be raised to about 150° C. for two to three hours a reddish
blue soluble in alkalies is obtained. If the sulphur be increased to say 10 or even
30 parts the blue obtained is much greener in shade and less soluble.
Further if the temperature be raised to 200° to 250° C. for several hours the
colouring matter becomes practically insoluble in alkalies. All these products
may be converted into colours soluble in water by heating at about 140° to 200° C.
with say 5 parts caustic alkali or alkaline sulphides, with or without the further
addition of sulphur, until a sample taken shows no increase in the strength of
colour.
We have also found that colouring matters are obtained when para amido phenol
is heated in molecular proportions with any of the following substances, until a
sample taken is soluble in alkali with a blue colour, the para sulphonic acids of
phenol, cresol, naphthol or ortho toluidine, the nitroso derivatives of phenol, cresol,
a and snaphthol, dioxy naphthalene and amido azobenzene or amido azo toluol.
If the products of the reaction of any of the organic substances before men-
tioned with para amido phenol be heated at a temperature of say 150° to 200° C.
with about 5 parts of sodium sulphide and of a part of sulphur there are obtained
colouring matters which dye vegetable fibre black. We may use instead of sodium
sulphide any poly sulphides of the alkalies obtained by dissolving sulphur in
caustic alkali.

page_text: TURNER, of Spink Field Road, Birkby, Huddersfield, JAMES TURNER, of Hudders-
field, and HARRY DEAN, of Greenhead Road, Huddersfield aforesaid, Chemists, 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:
We have discovered that para amido phenol when heated with sulphur yields
colours which vary in shade and solubility according to the proportion of sulphur
employed and the temperature to which the mass is raised.;;
If the proportion of sulphur be small say 5 parts, to 10 parts para amido pheno!
and the temperature be raised to about 150° C. for two to three hours a reddish
blue soluble in alkalies is obtained. If the sulphur be increased to say 10 or even
30 parts the blue obtained is much greener in shade and less soluble.
Further if the temperature be raised to 200° to 250° C. for several hours the
colouring matter becomes practically insoluble in alkalies. All these products
may be converted into colours soluble in water by heating at about 140° to 200°C.
with say 5 parts caustic alkali or alkaline sulphides, with or without the further
addition of sulphur, until a sample taken shows no increase in the strength of
colour.
1
19.
We have also found that colouring matters are obtained when para amido phenol
is heated in molecular proportions with any of the following substances; until a
sample taken is soluble in alkali with a blue colour, the para sulphonic acids of
phenol, cresol, naphthol or ortho toluidine, the nitroso derivatives of phenol, cresol,
a and naphthol, dioxynaphthalenes and amido azobenzene, or amido. azo toluol.
If the products of the reaction of any of the organic substances before men-
tioned with para amido phenol be heated at a temperature of say 150° to 200° C.
with about 5 parts of sodium sulphide and of a part of sulphur there are obtained
colouring matters which dye vegetable fibre black. We may use instead of sodium
sulphide any poly sulphides of the alkalies obtained by dissolving sulphur in
caustic alkali.
The following examples serve to illustrats the nature of this invantian

page_text: acid to a temperature of 160° to 180° C. for a few hours. The colouring matter
so produced dissolves in caustic alkalies with a deep blue colour.
EXAMPLE VI.
109 parts of para amido phenol are heated with 173 parts nitroso
a
naphtol te.
a temperature of 160° C. for a few hours. The colouring matter so obtained dis-
solves in alkalies with a violet black colour.
EXAMPLE VII.
109 parts of para amido phenol are heated with 197 parts of para amido azo
benzene for several hours to about 170° C. The product of the reaction dissolves
in water containing caustic alkali or alkali sulphides, with a violet black colour.
EXAMPLE VIII.
100 parts of the product obtained by the interaction of para amido phenol with
phenol para sulpho acid are heated with 300 parts of crystallized sodium sulphide
and 75 parts sulphur from 150° to 250° C. for a few hours.
We do not limit ourselves to the exact particulars given herein as the process
and quantities may be varied within certain limits.
The dyestuff so formed dyes vegetable fibres black.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed we declare that what
we claim is:-
1. The production of colouring matters dyeing animal and vegetable fibres,
shades varying from a reddish to a greenish blue by the action of various propor-
tions of sulphur upon para amido phenol at temperatures from 150 to 250° C.
2. The production of dyestuffs by heating the products obtained by the action
of sulphur upon para amido phenol with sodium sulphide or caustic alkalies either
with or without the further addition of sulphur.
3. The production of colouring matters by heating together in molecular propor-
tions, para amido phenol with the following substances viz.:-The para sulphonic
acids of phenol, cresol, naplitol and ortho toluidine, the nitroso derivatives of
phenol, cresol, a and s naphthol dioxynaphtalene and amido azobenzene or amido
azotoluol to temperatures varying between 150° and 250° C.
4. The production of dyestuffs by heating the products obtained by the action
of para amido phenol upon the substances referred to in Claim 3, with sodium
sulphide and sulphur or caustic alkalies and sulphur to a temperature of 150°
to 250° C.
5. The production of colouring matters as set forth in the preceeding claims.