Improvements in the Manufacture of Colouring Matters.
Year: 1892

page_text: Date of Application, 22nd Dec., 1892
Complete Specification Left, 7th Sept., 1893-Accepted, 21st Oct., 1893
PROVISIONAL SPECIFICATION.
[Communicated from abroad by Messrs. KALLE & Co., of Biebrich on the Rhine,
in the Empire of Germany, Manufacturers.]
Improvements in the Manufacture of Colouring Matters.
I, HENRY HARRIS LAKE, of the Firm of Haseltine Lake & Co., Patent
Agents, 45 Southampton Buildings, in the County of Middlesex, do hereby declare
the nature of this invention to be as follows :-
This invention relates to the manufacture of colouring matters.
A process for preparing a yellowish red dye stuff obtained by continued heating
of 1 part paranitrotoluolsulphonate of soda with 01 part soda to 102°-103°, is
described in the Bulletin de la Soc. ind de Mulbouse and fully quoted in the Ch.
Ind. 1887 page 307.
The dyestuff thus produced dissolves with a violet colour in concentrated
sulphuric acid. The same product is also obtained by mixing according to the
directions given in German Patent 38735, 5 parts paranitrotoluolsulphonate of
soda with 70 parts water and 3 parts soda lye of 40° Be.
By using a considerable excess of soda lye however, already at a low temperature,
a body of a more yellowish colour and increased tinctorial power is formed,
dissolving in sulphuric acid with a pure cherry-red colour and having the
composition of a sodiumsalt of the dinitrosostilbenedisulphonic acid. This product
dyes untanned cotton in a common salt bath, and wool in an acid bath, a reddish
yellow. By treatment with reducing agents it is transformed into an orange red
dyeing colour whereas by employing oxidation agents a product is obtained which
dyes a greenish yellow. The former dissolves with a blue colour, the latter with a
brown colour in concentrated sulphuric acid.
In order to obtain the new condensation product we proceed for instance as
follows:
10 kgs. paranitrotoluolsulphonate of soda are dissolved in 100 litres water and
20 kgs. soda-lye of 40° Bé. and the solution is maintained during about an hour at
about 70°. The colour of the solution is at first an intense magenta and afterwards
changes to orange yellow. At the same time the sodium salt of the new acid is
separated out in indistinct orange yellow crystals.
In order to obtain the oxydation product the dyestuff paste prepared as before
described is mixed with 7.5 kgs. sulphuric acid (2 : 1) and then 4.2 kgs. powdered
kaliumbichromate are introduced while stirring at the ordinary temperature.
After standing for 12 hours the reaction is complete. The mass is diluted with the
same volume of water, the dyestuff filtered off, washed with a diluted solution of
common salt, dissolved in ammonia and the solution evaporated to dryness. In
place of chromates other oxydation agents, such as peroxide of manganese,
peroxide of lead and the like may be used.
In order to obtain the reduction product I mix a solution of 10 kgs. sodiumsalt
of the new acid in 100 litres of water with 13.4 kgs. copperas and as much ammonia
as will completely precipitate the protoxide of iron, boiling is continued until the
latter is transformed into ferric oxide and filtered hot. The solution is precipitated
with common salt. A product of the same properties can be obtained by heating
under pressure an aqueous solution of a salt of the new acid. For example heat.
for three hours at 180° C. 1 part of the natriumsalt above described and 5 parts of
water.
Dated thin oond of Dreamber 1000

page_text: COMPLETE SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I, HENRY HARRIS LAKE, of the Firm of Haseltine Lake & Co., Patent
Agents, 45 Southampton Buildings, in the County of Middlesex, 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 :—
This invention relates to the manufacture of colouring matters.
A process for preparing a yellowish red dyestuff' obtained by continued heating
of 1 part paranitrotoluolsulphonate of soda with 0-1 part soda to 102°-103° is
described in the Bulletin de la Soc. ind de Mulhouse and fully quoted in the Ch.
Ind. 1887, page 307.
The dyestuff thus produced dissolves with a violet colour in concentrated
sulphuric acid. The same product is also obtained by mixing, according to the
directions given in German Patent 38735, 5 parts paranitrotoluolsulphonate of soda
with 70 parts water and 3 parts soda-lye of 40° Be.
By using a considerable excess of soda-lye however, already at a low temperature,
a body of a more yellowish colour and increased tinctorial power is formed,
dissolving in sulphuric acid with a pure cherry-red colour and having the
composition of a sodiumsalt of the dinitrosostilbenedisulphonic acid. This product
dyes untanned cotton in a common salt bath, and wool in an acid bath, a reddish-
yellow. By treatment with reducing agents it is transformed into an orange-red
dyeing colour, whereas by employing oxydation agents a product is obtained which
dyes a greenish-yellow. The former dissolves with a blue colour the latter with a
brown colour in concentrated sulphuric acid.
In order to obtain the new condensation product we proceed for instance as
follows:
10 kgs. paranitrotoluolsulphonate of soda are dissolved in 100 litres water and
20 kgs. soda-lye of 40° Bè. and the solution is maintained during about an hour at
about 70°. The colour of the solution is at first an intense magenta and afterwards
changes to orange yellow. At the same time the sodium salt of the new acid is
separated out in indistinct orange-yellow crystals.
In order to obtain the oxydation product the dyestuff-paste prepared as before
described is mixed with 7.5 kgs. sulphuric acid (2:1.) and then 4.2 kgs. powdered
kalium-bichromate are introduced while stirring at the ordinary temperature.
After standing for 12 hours the reaction is complete. The mass is diluted with the
same volume of water, the dyestuff filtered off, washed with a diluted solution of
common salt, dissolved in ammonia and the solution evaporated to dryness. In
place of chromates other oxydation agents, such as peroxide of manganese, peroxide
of lead and the like may be used.
In order to obtain the reduction product I mix a solution of 10 kgs. sodiumsalt
of the new acid in 100 litres of water with 13-4 kgs. copperas and as much ammonia
as will completely precipitate the protoxide of iron, boiling is continued until the
latter is transformed into ferricoxide and filtered hot. The solution is precipitated
with common salt. A product of the same properties can be obtained by heating
under pressure an aqueous solution of a salt of the new acid. For example heat
for three hours at 180° C., 1 part of the natriumsalt above described and 5 parts of
water.
Having now particularly described and ascertained the nature of the 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 :-
1. The production of an homogeneous body having the composition
of

page_text: dinitrosostilbenedisulphonic acid by treating paranitrotoluolsulphonic acid with
soda-lye of at least 10° Bè. at a temperature below 100° C.
2. The production of derivatives of the said dinitrosostilbenedisulphonic acid by
treating the same with reducing or oxydizing agents, substantially as set forth.
Dated this 7th day of September 1893.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.