Production of Blue Colouring Matters.
Year: 1891

page_text: Date of Application, 8th May, 1891
Complete Specification Left, 5th Feb., 1892-Accepted, 12th Mar., 1892
PROVISIONAL STEOITATION.
[Communicated from abroad by THE FARBWERKE VORMALS MEISTER LUCIUS
AND BRUNING, of Hoechst-am-Maine, in the Empire of Germany, carrying on
business as Chemical Manufacturers.]
Production of Blue Colouring Matters.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Fellow of the Institute of Patent Agents, do hereby declare
the nature of this invention to be as follows:-
―:
My foreign correspondents, who communicate this invention, manufacture and
sell blue acid coloring matters called "Patent Blues," the production of which is
described in the Specifications No. 12796 of 1888 and No. 14822 of 1888.
These sulphonic acids of the meta-oxy- and meta-amido-tetralkyl-diamidotriphenyl
carbinols, on being oxidised, furnish blue coloring matters of great value;
especially the products obtained from the sulphonic acids of
meta oxy tetra methyl
ethyl
dimethyl dibenzyl
diethyl
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amido tetra methyl
diamido-triphenyl carbinol
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ethyl
dimethyl-dibenzyl
diethyl-
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and from the sulphonic acids of the products prepared by benzylising these amido
tetralkyl diamido triphenyl carbinols. These products dye on animal fibre very
uniform and solid blue tints.
The oxidation of the sulphonic acids mentioned above may be effected by
treating them with fuming sulphuric acid, but in this case the oxidation is not
very complete.
These sulphonic acids are gently and evenly converted into the novel colouring
matters by oxidising them in aqueous solution and preferably in presence of salts
of oxide of iron or of chromic acid.
The process may be understood from the following examples:
A. SULPHATE OF OXIDE OF
OXIDATION OF
AGENT.
IRON AS OXIDISING
OXY TETRA METHYL DIAMIDO TRI-
THE SULPHONIC ACID OF META
PHENYL CARBINOL.
20 parts by weight of tetra-methyl-patent blue (the mono calcium salt of the
disulphonic acid of meta-oxy-tetra-methyl-diamido-triphenyl-carbinol) are dissolved
hailing and slowly

page_text: B. CHROMIC ACID AS OXIDISING AGENT.
The results obtained by oxidising the patent blue colouring matters with chromic
acid are much more satisfactory. Either an aqueous solution of chromic acid can
be used or the solution of a chromate mixed with the quantity of mineral acid
necessary to form free chromic acid.
OXIDATION OF THE SULPHONIC ACID OF META OXY TETRA-ETHYL-DIAMIDO-
TRIPHENYL-CARBINOL.
"
246 parts by weight of tetra ethyl patent blue (the mono-calcium salt of the
disulphonic acid of meta-oxy-tetra-ethyl-diamido-triphenyl carbinol) are dissolved
in from 200 to 300 parts by weight of water, the solution is heated to boiling and
very slowly mixed with a solution of 8 parts by weight of Cro, in water.
The
oxidation is complete after about 2 hours, this being ascertained by finding a
sample of the solution free from chromic acid. The solution of the colouring
matter is filtered off from the precipitate of chromo-hydroxide and is evaporated to
dryness.
Among the new blue colouring matters produced in this way, with suitable
variation of the quantities of the bodies submitted to reaction in accordance with
their molecular weights, may be mentioned as examples the colouring matters
produced from the sulphonic acids of
meta-oxy-tetra-methyl
-
diamido-triphenyl carbinol
"
"
"
دو
"
"
"
ethyl
dimethyl dibenzyl
diethyl
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amido-tetra-methyl
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دو
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ethyl
dimethyl-dibenzyl
diethyl
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and from the sulphonic acids of the products prepared by benzylising these amido-
tetralkyl-diamido-triphenyl carbinols.
The colouring matters may be produced also by oxidising the sulphonic acids of
the corresponding meta-oxy- and meta-amido-triphenyl-methans by treatment with
the necessary quantity of the oxidising agents named, but it is more advantageous to
convert first the leuco sulphonic acids into the colouring matters in the manner
described in the Specifications No. 12796 of 1888 and No. 14822 of 1888, and then
to oxidise the colouring matters thus prepared in the manner hereinbefore set
forth.
The novel colouring matters are powders of copper red colour with metallic
lustre, easily soluble in water showing intense blue.
When boiled with ammonia or soda solution the aqueous solution of the colouring
matter does not undergo any perceptible change; when mixed with an excess of
mineral acid it assumes a green colour..
In an acid bath the coloring matters dye wool and silk with very uniform blue
shades, which excel by their great resistance to action of soap, light and air,
surpassing in this respect the products now known that are used for dyeing in acid
bath.
ABEL & IMRAY,
Agents for the Applicant.

page_text: OXIDATION OF THE SULPHONIC ACID OF META OXY TETRA-ETHYL-DIAMIDO-
TRIPHENYL-CARBINOĻ.
24-6 parts by weight of tetra ethyl patent blue (the mono-calcium salt of the
disulphonic acid of meta-oxy-tetra-ethyl-diamido-triphenyl carbinol) are dissolved
in from 200 to 300 parts by weight of water, the solution is heated to boiling and
The
very slowly mixed with a solution of 8 parts by weight of Cro, in water.
oxidation is complete after about two hours, this being ascertained by finding a
sample of the solution free from chromic acid. The solution of the colouring
matter is filtered off from the precipitate of chromo hydroxide and is evaporated
to dryness.
Among the new blue colouring matters produced in this way, with suitable
variation of the quantities of the bodies submitted to reaction in accordance with
their molecular weights, may be mentioned as examples the colouring matters
produced from the sulphonic acids of
meta-oxy-tetra-methyl
-
ethyl
dimethyl dibenzyl
diethyl
amido-tetra-methyl
"
"
"
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diamido-triphenyl carbinol
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"
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"
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"
"
"
"
"
"
ethyl
dimethyl-dibenzyl
diethyl
and from the sulphonic acids of the products prepared by benzylising these amido-
tetralkyl-diamido triphenyl carbinols.
The colouring matters may be produced also by oxidising the sulphonic acids of
the corresponding meta-oxy- and meta-amido-triphenyl-methans by treatment with
the necessary quantity of the oxidising agents named, but it is more advantageous
to convert first the leuco sulphonic acids into the colouring matters in the manner
described in the Specifications No. 12796 of 1888 and No. 14822 of 1888, and then
to oxidise the colouring matters thus prepared in the manner hereinbefore set
forth.
The novel colouring matters are powders of copper red colour with metallic lustre,
easily soluble in water showing intense blue.
When boiled with ammonia or soda solution the aqueous solution of the colouring
matter does not undergo any perceptible change; when mixed with an excess of
mineral acid it assumes a green colour.
In an acid bath the colouring matters dye wool and silk with very uniform blue
shades, which excel by their great resistance to action of soap, light and air,
surpassing in this respect the products now known that are used for dyeing in acid
bath.
Having now particularly described and ascertained the nature of this inven
tion and in what manner the same is to be performed, I declare that what I
claim is :-
1. The production of novel blue coloring matters, substantially
mi
111
11
as described.
Dated this on day of February 1992.
ABEL & IMRAY,
Agents for the Applicant.
ABEL & IMRAY,
Agents for the Applicant.