Production of Azo-colours.
Year: 1893

page_text: Date of Application, 16th June, 1893
Complete Specification Left, 1st Mar., 1894-Accepted, 7th Apr., 1894
Production of Azo-colours.
1, THOMAS RICHARD SHILLITO of 89 Chancery Lane, in the County of
Middlesex, Engineer and Patent Agent, do hereby declare the nature of this
invention, a communication to me from abroad by John Rudolph Geigy of Basle,
Switzerland, to be as follows:-
This invention relates to the reaction between solutions of diazophenols, diazo-
cresols or the known carbo-acids, sulfo acids or carbo sulfo-acids of them and
alkaline solutions of gallic acid, ethers of gallic acid, gallamide, anilide or toluides
or xylides or naphtylamides of gallic acid, pyrogallic acid, tannin, quercetine (or
flavin) morin (or extract of fustic), solutions of catechu or gambir or of kino,
fisetine, rhannetine, etcetera. The residues resulting from the production of gallic
acid from tannin may also be used. In this way new colouring matters are obtained
which dye chrome mordanted wool or cotton a brownish yellow and redish brown
to dark brown shades.
The following are examples of the method of carrying out the invention :-
1st.) 21.5 kilogrammes of p-amidophenol are dissolved in 300 liters of water with
addition of 30 kilogrammes of hydrochloric acid of 21° Beaumé and diazotized at
a temperature near to 0° C. with 14 kilogrammes of nitrite of sodium. This is then
mixed with a solution of 38 kilogrammes of gallic acid in 300 liters of water and
60 kilogrammes of ammonia of 22° Beaumé. The intensely brown coloured solution
is then acidulated with 150 kilogrammes of acetic acid (40 per cent.) and the
colouring matter precipitated by addition of salt.
2nd.) 24 kilogrammes of amidosulfosalicylic acid are suspended in 100 liters of
water, 15 kilogrammes of hydrochloric acid of 21 Beaumé are added and then
diazotized with 7 kilogrammes of nitrite of sodium at a temperature of about 5° C.
The diazo compound is then mixed with a solution containing 12.5 kilogrammes
of pyrogallic acid and 18 kilogrammes of carbonate of sodium in 60 liters of water.
To the brown coloured solution thus formed 50 kilogrammes of 40% acetic acid
are added. The paste is employed direct for dyeing and printing.
3rd.) 30 kilogrammes of a-p-amidophenoldisulfo acid of the kind described in
Specification of Letters Patent No. 15692 of 1892 are dissolved in 300 liters of
hot water. The mass having become quite thick in cooling is mixed with 15 kilo-
grammes of hydrochloric acid of 21 Beaumé and at a temperature of about 5° C.
diazotized with 7 kilogrammes of nitrite of sodium. The diazo compound is then
precipitated with 50 kilogrammes common salt, filtered off and mixed with a cold
paste containing 30 kilogrammes of quercetine in 100 liters of water previously
heated with addition of 10 kilogrammes of carbonate of sodium. To this mixture
are added 30 kilogrammes of ammonia of 22 Beaumé. A deep brown solution is
formed which after an interval of one hour is mixed with 10 kilogrammes of
sulphuric acid and 50 kilogrammes of 40% acetic acid. The product is an orange
paste.
Dated this 16th day of June 1893.
THOMAS R. SHILLITO,
89, Chancery Lane, London, W.C.

page_text: COMPLETE SPECIFICATION.
Production of Azo-colours.
I, THOMAS RICHARD SHILLITO of 89 Chancery Lane, in the County of
Middlesex, Engineer and Patent Agent, do hereby declare the nature of this
invention, a communication to me from abroad by John Rudolph Geigy of Basle,
Switzerland, Colour Manufacturer, and in what manner the same is to be
performed, to be particularly described and ascertained in and by the following
statement :-
Since filing the Provisional Specification of this invention, experience has tended
to shew that only the combinations of the diazo compounds of alpha para-amido-
phenol-disulfo acid of the kind described in the Specification of Letters Patent
No. 15692 of 1892, and of para-amido-phenol monosulfo acid with pyrogallic acid
are commercially valuable and therefore the invention is limited so as to consist in
the production of azo colours by combination of the diazo compounds of alpha
para-amido-phenol disulfo acid of the kind stated, or of para-amido-phenol-mono-
sulfo acid with pyrogallic acid.
The following is an example of the method of carrying out the invention:-
30 kilogrammes of alpha para-amido-phenol-disulfo acid is dissolved in 300 liters
of hot water, left to stand until cold, then mixed with 50 kilogrammes of ice and
15 kilogrammes of hydrochloric acid of 21° Beaumé and diazotised with 7 kilo-
grammes of nitrite of sodium. The diazo compound thus obtained is precipitated
with 50 kilogrammes of common salt, filtered off, and mixed with 50 kilogrammes
of ice. A solution of 15 kilogrammes of pyrogallic acid in 20 liters of water is
then added and after this, a solution of 18 kilogrammes of carbonate of sodium in
60 liters of water. To the brown coloured paste thus formed 50 kilogrammes of
40% acetic acid are added after a repose of 12 hours. The paste thus produced
may be employed direct for dyeing or printing or the colouring matter may be
filtered off and dried.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what I
claim is
The production of azo-colours by combination of the diazo compounds of alpha
para-amido-phenol disulfo acid of the kind' referred to in the Specification of
Letters Patent No. 15692 of 1892 or of para amido-phenol-monosulfo acid with
pyrogallic acid, substantially as described.
Dated this 1st day of March 1894.
THOMAS R. SHILLITO,
89, Chancery Lane, London, W.C.