A NEW new coloring matter by the
Year: 1883

page_text: PROVISIONAL SPECIFICATION left by the said Henry Oswald Miller at the
Office of the Commissioners of Patents on the 30th April 1883.
HENRY OSWALD MILLER of Moscow, in the Empire of Russia
COLOURING-MATTER
"
"A NEW
new coloring matter by the
The object of this invention is to produce a
oxidation of hydro sulphocyanic acid, or of its salts.
The oxidation may be effected by the action of chromic acid on the hydro
sulphocyanido, but the effect may also be obtained by the action of chlorine or of
bromine.
In carrying out my invention with regard to the treatment of sulphocyanide
of potassium with bromine I proceed as follows:-I dissolve in one litre of water
one kilo of sulphocyanide of potassium, and I add thereto about twenty cubic
centimetres of muriatic or hydrobromic acid. To this mixture I add in small
quantities at a time, and at the same time refrigerating the solution, one kilo: of
Bromine.
In effecting the desired result through the agency of chlorine I make a
mixture of say 370 cubic centimetres of concentrated sulphuric acid, 660 cubic
centimetres of inuriatic acid, and 1380 cubic centimetres of water.
To this mixture I add a second mixture composed of 1, kilo: sulphocyanide
of potassium and, 500 grammes chlorate of Potash keeping the temperature below
60° centigrade
In both cases I obtain a precipitate of an orange colour the weight of which,
after it is washed and dried, represents 40% of the sulphocyanide employed.
The colouring matter thus obtained is a rather heavy powder of a clear orange
colour and contains according to the mode of preparation small quantities of chlorine
or of bromine.
The product is not soluble in water, alcohol or ether, nor in ordinary acids but is
soluble only in concentrated sulphuric acid and in the caustic alkalies.
By combining with the above product a hydric solution of potassium of greater
or less strength the colour may be varied from yellow to a reddish brown, and the
product can be used as a direct colouring matter for dyeing cottons.
This new colouring matter stands in the same relation to cotton as picric acid
and most of the aromatic colours do to silk, and wool.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said Henry Oswald Miller in the Great Seal Patent Office on tho
30th October 1883,
HEINRICH [sic] OSWALD MILLER of Moscow in the Empire of Russia
COLORING MATTER”
" A NEW
The object of this Invention is to produce a new coloring matter to which I
have given the name of "canarine."
Canarine is produced by the oxidation of the pseudo sulphocyanides. It is
obtained by the action of chlorine or of bromine on hydrosulphocyanic acid or its
salts, and it is composed of the following elements viz: carbon, hydrogen nitrogen,
sulphur, and oxygen.
Canarine can be obtained by one of the following modes:—
First In the production of "canarine by means of sulphocyanide of
potassium, chlorate of potassium and muriatic acid I proceed as follows.
I take three kilogrammes of sulphocyanide of potassium one and a half kilos of
chlorate of potassium, six kilos of muriatic acid at twenty one degrees Baumé and
six kilos of water.
The sulphocyanide of potassium is dissolved in six kilo of the water which is
hot and is placed in a suitable earthen vessel.-When the temperature of the
solution becomes about equal to 40 degrees centigrade. I add 300 grammes of
chlorate of potassium and 2400 grammes of muriatic acid. Reaction immediately
commences and a precipitate of an orange color (the "canarine") is deposited.
At the same time a great quantity of gaseous products are formed and the
temperature of the liquid rises considerably.
Once the reaction is commenced, the vessel containing the liquid is placed in
cold water to about half its height and the subsequent operations are carried out
at a temperature of from 50° to 80° centigrade.
The remainder of the chlorate of potassium and muriatic acid is added a little
at a time and the liquid is stirred continually to ensure the proper mixing of the
various ingredients.
The transformation of the three kilos of sulphocyanide of potassium is effected' in
about two hours.
"
The precipitate (the "canarine") separated from the liquid is washed with hot
water until it becomes neutral.
Second. In the production of "canarine" by the action of bromine and of
muriatic acid on sulphocyanide of potassium, I take one kelogramme of the sulpho-
cyanide of potassium one kilo of water, twenty cubic centimetres of muriatic acid,
and one kilo of bromine.
The one kilo of the sulphocyanide is dissolved in one litre of water in a suitable
vessel and the muriatic acid is then added thereto. The liquid is then cooled and
continuously stirred, during which time the one kilo of bromine is added, the
bromine being allowed to run, in fine streams.
The precipitate (the "canarine") is then washed first in cold water and then in
hot water until it becomes neutral.
THE CHARACTERISTIC PROPERTIES OF "CANARINE
"
Canarine is a powder of deep orange color-it is insoluble in water and in ether
and only slight traces remain in a solution of alcohol.-Concentrated sulphuric
مم المت

page_text: alkalis at boiling point, a deep red solution being formed, the color of which does
not alter os diresmees by boiling
"
By heating the "canarine in the form of a dry powder it is decomposed the
sulphuric acid and the sulphur separate, and there remains a brown residue.
The above described properties of canarine enable it to be readily distinguished
from pseudo sulphocyanide, for the latter is notably (1) soluble in concentrated
sulphuric acid without being decomposed; (2) caustic alkalis decompose it at
boiling point and the solution becomes discolored; (3) being heated in the form
of dry powder it is decomposed and yields sulphur, sulphuret of carbon and a
vellow residue.
By heating the "canarine" in the form of a dry powder it is decomposed the
sulphuric acid and the sulphur separate, and there remains a brown residue.
The above described properties of canarine enable it to be readily distinguished
from pseudo sulphocyanide, for the latter is notably (1) soluble in concentrated
sulphuric acid without being decomposed; (2) caustic alkalis decompose it at
boiling point and the solution becomes discolored; (3) being heated in the form
of dry powder it is decomposed and yields sulphur, sulphuret of carbon and a
vellow residue.
-
THE APPLICATION OF
CANARINE
"
The solution of "canarine" in caustic potash is applicable to dyeing tissues and
thread, yellow or orange. "Canarine" is distinguished from other yellow coloring
matters by the reason that it becomes immediately fixed in vegetable textile
materials without the use of mordants.
Materials dyed by "canarine" have a bright appearance which does not fade
from the use of soap or the action of light.
נו
To prepare a coloring solution of "canarine" I take say one part of "canarine
one part of caustic potash, one hundred parts of condensed water and one quarter
of a part of dry oleine soap.
These materials are mixed together in a suitable vessel and are caused to boil
until the complete dissolution of the "canarine" is effected.
Having now described the nature of my Invention for "A new coloring matter"
and explained the manner of carrying the same into effect I claim.
First-The new coloring matter which I term "Canarine" obtained from the
oxydation of hydrosulphocyanic acid or its salts and distinguishable by the
characteristics above set forth.
Second: Effecting the oxydation of hydrosulphocyanic acid or its salts by
means of chlorine or bromine in the presence of muriatic or other suitable acid
substantially as herein described to produce the new coloring matter termed
"canarine" as setforth.
In witness whereof I the said Heinrich [sic] Oswald Miller have hereunto set my
hand and seal the Twenty-fourth day of October in the year of our Lord One
thousand eight hundred and eighty three.