Year: 1896

page_text: We, IVAN LEVINSTEIN and LEVINSTEIN LIMITED, both of Minshull Street
Manchester in the County of Lancaster, Chemical Manufacturers, ido.. hereby. declare
the nature of this invention to be as follows:-
. In the specification left by us with our application for Letters Patent No. 2946
dated the 10th February 1896, we have described the production of amido-azo and
tetrazo colouring matters from the a, a, naphthylenediamine ẞ, sulpho-acid. 'We have
now found that if the amido-azo colouring matters obtained by combining the 'diazo
compound of a₁ a, naphthylenediamino 3, sulpho-acid with suitable diazotisable
amines, amidonaphthols, amidonaphtholethers, or their sulpho-acids, are diazotised or
tetrazotised; and the diazo or tetrazo hodies so obtained are combined with phenols,
amines; diamines and the like, specially valuable colouring matters are obtained which
dye not only animal but also vegetable fibres a deep black. In order to produce these
colours we may proceed as follows:-
STEP 2. CONVERSION OF THE AMIDO-AZO COLOURING MATTER OF EXAMPLE I, INTO A
. DIAZO-AZO COMPOUND, AND COMBINATION OF THIS "WITH ONE MOLECULE OF
METATOLUYLENEDIAMINE.
53-2 kilos. of the colouring matter obtained as described under "Example: I: are
dissolved in about 600 litres of water. The solution is cooled with ice, acidified with
70 kilos. of commercial hydrochloric acid.of.189 Bé., and then an aqueous solution of
7-2 kilos. of sedium nitrite is gradually added whilst stirring. The temperature is
preferably not allowed to arise above 8.or 10° C. After a few hours the original
dye-stuff will be found to have been converted into the dark coloured diazo compound
which is then run into an aqueous solution: containing 12.5. kilos.. métatoluylene-
diamine; whilst stirring. The, free mineral acid present: is..neutralised.with. sodium
acetate,and after.. a short time the. combination is completed. The whole is then
made alkaline by addings sodium carbonate or other, suitable alkali. and, the new
colouring matter is salted. out, filtered, pressed..and dried. It.dyes..animal, and
vegetable, fibres a deep black.

page_text: CONVERSION OF THE AMIDO-AZO COLOURING MATTER OF EXAMPLE I, INTO A TETRAZO
COMPOUND, AND THE COMBINATION OF THIS WITH TWO MOLECULES OF META-
TOLUYLENEDIAMINE.
We proceed, in order to obtain the result, in a similar manner to that described in
Example I, Step 2, with the exception that we take 144 kilos. of sodium nitrite
instead of 7-2 kilos., and 25 kilos. of metatoluylenediamine instead of 12.5 kilos.
The colouring matter thus obtained dyes animal and vegetable fibres a deep jet-
black.
If, instead of metatoluylene-diamine in the above two examples, resorcinol in the
molecular proportions represented by 11 and 22 kilos. respectively, are used, and
the combination is carried out in an alkaline solution, a colouring matter is
obtained which dyes wool in a neutral bath, a greyish black, and cotton and
vegetable fibres, a greenish-black colour, and similar colouring matters may be
produced by substituting toluylenediamine or resorcinol by other diamines, phenols,
amidophenols, dioxy bodies both of the benzene and naphthalene series, as well as
their sulpho- and carboxylic-acids.
JCT.... AD 100
W. E. HEYS & SON,
Agents for the Applicants.
Manufacture or Production of New Colouring Matters.
We, IVAN LEVINSTEIN and LEVINSTEIN LIMITED, both of Minshull Street,
Manchester in the County of Lancaster, Chemical Manufacturers, 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:-
In the specification left by us with our application for Letters Patent No. 2946
dated the 10th February A.D. 1896, we have described the production of amido-
azo and tetrazo colouring matters from the a, a, naphthylenediamine B, sulpho acid.
We have now found that if the amido-azo colouring matters obtained by combining
the diazo compound of as a naphthylenediamine ẞ, sulpho acid with suitable
diazotisable amines, amidonaphthols, amidonaphtholethers, or their sulpho acids, are
diazotised or tetrazotised, and the diazo or tetrazo bodies so obtained are combined
with phenols, amines, diamines and the like, specially valuable colouring matters
are obtained which dye not only animal, but also vegetable fibres a deep black.
In order to produce these colours we may proceed as follows:-

page_text: within a short time. The colouring matter so produced is salted out, filtered and
pressed. It dyes wool, in an acid bath, a deep violet black.
STEP 2. CONVERSION OF THE AMIDO-AZO COLOURING MATTER OF EXAMPLE I, INTO A
DIAZO-AZO COMPOUND, AND COMBINATION OF THIS WITH ONE MOLECULE OF
METATOLUYLENEDIAMINE.
53-2 kilos. of the colouring matter obtained as described under Example I, are
dissolved in about 600 litres of water. The solution is cooled with ice, acidified
with 70 kilos. of commercial hydrochloric acid 18° Bé., and then au aqueous.
solution of 7-2 kilos. of sodium nitrite is gradually added whilst stirring. The
temperature is preferably not allowed to rise above 8° or 10° (. After a few
hours the original dye stuff will be found to have been converted into the dark:
coloured diazo compound which is then run into an aqueous solution containing
12.5 kilos. of metat oluylenediamine whilst stirring. The free mineral acid present is
neutralised with sodium acetate, and after a short time the combination is completed..
The whole is then made alkaline by adding sodium carbonate or other suitable alkali
and the new colouring matter is salted out, filtered, pressed and dried. It dyes.
animal and vegetable fibres a deep black.
CONVERSION OF THE AMIDC-AZO COLOURING MATTER OF EXAMPLE I INTO A TETRAZO-
COMPOUND, AND THE COMBINATION OF THIS WITH TWO MOLECULES OF META-
TOLUYLENEDIAMINE.
We proceed, in order to obtain the result, in a similar manner to that described
in Example I, Step 2, with the exception that we take 144 kilos. of solium:
nitrite instead of 7.2 kilos., and 25.0 kilos. of metatoluylenediamine instead of
12.5 kilos. The colouring matter thus obtained dyes animal and vegetable fibres.
a deep jet-black.
If, instead of metatoluylenediamine in the above two examples, resorcinol in the
molecular proportions represented by 110 and 22.0 kilos. respectively are used,.
and the combination is carried out in an alkaline solution, a colouring matter is
obtained which dyes wool in a neutral bath, a greyish black colour, and cotton
and vegetable fibres, a greenish black, and similar colouring matters may be.
produced by substituting toluylenediamine or resorcinol by other diamines, phenols,
amidophenols, dioxy bodies both of the benzene and naphthalene series, as well as
their sulphonic and carboxylic acids.
Having now particularly described and ascertained the nature of our said inven-
tion and in what manner the same is to be performed, we declare that what
we claim is :-
1. The hereinbefore described process for the production of amido-azo colouring
matters, substantially as set forth.
2. The hereinbefore described process for the production of diazo-azo colouring
matters combined with metatoluylene, resorcinol, or with other diamines, phenols,
amidophenols, dioxy bodies both of the benzene and naphthalene series as well as.
their sulphonic and carboxylic acids, substantially as set forth.
3. The hereinbefore described process for the production of tetrazo colouring
matters combined with two molecules of metatoluylenediamine, resorcinol, or of
other diamines, phenols, amidophenols, dioxy bodies both of the benzene and
naphthalene series as well as their sulphonic and carboxylic acids, substantially as
set forth.
4. As new substances the hereinbefore described amido-azo colouring matters.

page_text: 5. As new substances; the hereinbefore described odiazo-azo colouring matters
combined with metatoluylenediamine, resorcinol, or with other diamines, phenols,
amidophenols, dioxy bodies both of the benzene and naphthalene series as well as
their sulphonic and carboxylic acids.
6. As new substances, the hereinbefore described tetrazo colouring matters
combined with two molecules of metatoluylenediamine, resorcinol, or with other
diamines, phenols, amidophenols, dioxy bodies both of the benzene and naphthalene
series as well as their sulphonic and carboxylic acids.
.
Dated this 30th day of April; A.D. 1897.
W. E. HEYS & SON,
'
Agents for the Applicants.
W. E.THEYS & SON,
Agents for the Applicants.