|Improvements in the Manufacture of Azo-colouring Matters.
Year: 1892

page_text: Date of Application, 9th June, 1892
Complete Specification Left, 3rd Mar., 1893-Accepted, 22nd Apr., 1893
PROVISIONAL SPECIFICATION.
|Improvements in the Manufacture of Azo-colouring Matters.
We, BROOKE, SIMPSON AND SPILLER, LIMITED, of the Atlas Works, Hackney
Wick, in the County of Middlesex, Aniline Dye Manufacturers, and ARTHUR
GEORGE GREEN of the same address and THOMAS ATKINSON LAWSON, of the
same address, Fellows of the Institute of Chemistry and Chemists to the said firm
of Brooke, Simpson and Spiller, Limited, do hereby declare the nature of this
invention to be as follows:-
Our invention relates to the manufacture of a red colouring matter, which dyes
wool from an acid bath and withstands the action of milling and scouring to a very
remarkable extent.
We obtain this colour by treating the azoxy-toluidine, which melts at 168° centi-
grade, and has the chemical formula (1:2:4) C.H, (CH) (NH) NO C.H,
(NH) (CH3) (4: 2: 1), with nitrous acid, and combining the tetrazo compound,
so obtained, with one molecule of alpha-naphthol-para-sulphonic acid and one
molecule of beta-naphthol-disulphonic acid R.
The azoxy-toluidine employed was first obtained by Limpricht in 1885, (see
Berichte der Deutschen Chemischen Gesellschaft, Vol. XVIII, p. 1403).
The following is an example of the process for preparing the said colouring
matter. A solution of 14 lbs. of sodium nitrite (96%) in 20 gals. of water is added
slowly to an iced solution of 25+ lbs. of the aforesaid azoxy-toluidine in 100 gals.
of water, containing 4 gals. of hydrochloric acid (31 %).
The solution of the tetrazo compound thus obtained is then added to a solution
containing 25 lbs. of sodium alpha-naphthol-para-sulphonate and about 20 lbs. of
crystallized sodium acetate in 100 gals. of water. A solution of 35 lbs. of sodium
beta-naphthol-di-sulphonate R and 24 lbs. of commercial anhydrous sodium
carbonate, or its equivalent in ordinary crystallized soda, in 100 gals. of water is
then run in.
The insoluble intermediate compound, which had first formed, dissolves as the
combination takes place, and when the solution, which has throughout been
well agitated, becomes quite clear, the colouring matter is precipitated from its
solution by the addition of common salt, filtered off and dried.
Dated this 9th day of June 1892.
AMBROSE MYALL,
21, Cockspur Street, London, S.W., Agent for the Applicants.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Azo-colouring Matters.
We, BROOKE SIMPSON & SPILLER LD., of the Atlas Works, Hackney
Wick, in the County of Middlesex, Aniline Dye Manufacturers, and ARTHUR
GEORGE GREEN, of the same address and THOMAS ATKINSON LAWSON, of the
same address, Fellows of the Institute of Chemistry, and Chemists to the said
firm of Brooke Simpson & Spiller, Limited, 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 :-
Our invention relates to the manufacture of a red colouring matter, which dyes
wool from an acid bath and withstands the action of milling and scouring to a very
remarkable extent.

page_text: We obtain this colour by treating the azoxytoluidine, which melts at 168° centi-
grade, and has the chemical formula [124] C.H, (CH) (NH2) NO CH.
(NH) (CH) [4:2:1] with nitrous acid, and combining the tetrazo compound, so
obtained, with one inolecule of alpha-naphthol-para-sulphonic acid and one molecule
of beta-naphthol-disulphonic acid R.
The azoxytoluidine employed was first obtained by Limpricht in 1885 (see
Berichte der Deutschen Chemischen Gesellschaft, Volume 18 page 1403).
The following is an example of the process for preparing the said colouring
matter.
A solution of 14 lbs. of sodium nitrite (96%) in 20 gals. of water is added
slowly to an iced solution of 25 lbs. of the aforesaid azoxytoluidine in 100 gals. of
water containing 4 gals. of hydrochloric acid (31%).
The solution of the tetrazo compound thus obtained is then added to a solution
containing 25 lbs. of sodium alpha-naphthol-para-sulphonate and about 20 lbs. of
crystallized sodium acetate in 100 gals. of water.
A solution of 35 lbs. of sodium beta-naphthol-di-sulphonate R and 24 lbs. of
commercial anhydrous sodium carbonate, or its equivalent in ordinary crystallized
soda in 100 gals. of water is then run in.
The insoluble intermediate compound, which had first formed, dissolves as the
combination takes place, and when the solution, which has throughout been well
agitated, becomes quite clear, the colouring matter is precipitated from its solution
by the addition of common salt, filtered off and dried.'
The colouring matter so obtained, is in the form of a dark red powder, which is
easily soluble in water, but is insoluble in alcohol. The addition of caustic soda or
potash to the aqueous solution changes the red colour to an orange red. Dilute
acids do not precipitate the solution. The colour itself dissolves in concentrated
sulphuric acid with a bluish red colour.
In an acidified bath it dyes woollen goods a bright red closely approaching in
shade cochineal scarlet. The dye thus used resists the action of soap and alkali, as
used in milling or domestic washing, in a remarkable manner. The dyed goods are
not altered in colour by the action of 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 herein described process for the preparation of a colouring matter,
consisting in the treatment of azoxy-toluidine of melting point 168° C. with nitrous
acid and combining the tetrazo compound thus obtained with one molecule of alpha-
naphthol-para-sulphonic acid and one molecule of beta-naphthol-di-sulphonic acid R,
and finally precipitating the colouring matter, substantially as described.
2. As a new article of manufacture, a colouring matter derived by the process
set forth, and consisting of a dark red powder, easily soluble in water but insoluble
in alcohol, the addition of caustic soda or potash to such aqueous solution, changing
the red colour to orange red, said solution not capable of precipitation by dilute
acids, said colour dissolving in concentrated sulphuric acid with a bluish red colour,
said colour in an acidified bath dyeing woollen goods a bright red, said dye so used
resisting the action of soap and alkali in milling and washing and said dyed goods
not altered in colour by the action of acids, substantially as described.
Dated this 3rd day of March 1893.
AMBROSE MYALL,
21, Cockspur Street, London; S.W., Agent for the Applicants.