IMPROVEMENTS IN THE PRODUCTION OF COLOURING MATTERS SUITABLE FOR DYEING AND PRINTING
Year: 1882

page_text: LETTERS PATENT to Joseph Anthony Dixon, of No 151, St. Vincent Street,
Glasgow, in the County of Lanark, North Britain, Solicitor, for an invention
of "IMPROVEMENTS IN THE PRODUCTION OF COLOURING MATTERS SUITABLE
FOR DYEING AND PRINTING-A communication from abroad by the Farbwerke
Vorm Meister, Lucius, and Brüning, a Company carrying on business as
Chemical Manufacturers at Höchst-an-Main, in the empire of Gerinany.
PROVISIONAL SPECIFICATION left by the said Joseph Anthony Dixon at
the Office of the Commissioners of Patents on the 9th May 1882.
JOSEPH ANTHONY DIXON, of 151 St. Vincent Street, Glasgow, in the County
of Lanark, North Britain, Solicitor, "IMPROVEMENTS IN THE PRODUCTION OF
COLOURING MATTERS SUITABLE FOR DYEING AND PRINTING [A communication
from abroad by the Farbwerke Vorm: Meister, Lucius, and Brüning, a Company
carrying on business as Chemical Manufacturers at Höchst-am-Main, in the empire
of Germany.]
The nature and object of this Invention is the production of Alpha-Napthyl-
amine-Trisulpho-acid, and the further production of a yellow dyestuff therefrom.
The process hereinafter described for the production of the said yellow dyestuff,
is founded on the simultaneous action of nitrates and nitrites in acid solution on
the said napthylaminetrisulpho-acid.
I shall first describe the production of the said trisulpho acid of Alpha-
napthylamine (till now unknown), and then give the process for the conversion of
this trisulpho acid into the said yellow colouring matter.
First step. Production of the Alphanapthylaminetrisulpho acid.
It is advantageous for the production of the said trisulpho acid of Alpha-
napthylamine, first to convert the napthylamine into its mono-sulpho acid and then
to sulphonate this acid further.
I add one part of the difficultly soluble Alphnapthylaminemono-sulpho-acid to
three or four parts of fuming sulphuric acid (40 % SO₂).—keeping the mixture

page_text: .cool by means of cold water, and heat this mixture slowly to 248°. Fahrenheit
(120°. Centigrade) at which temperature I continue the heating for from 6 to 10
hours.
I then pour the product of the sulphonization into cold water, neutralize the
liquid with limewater, remove the sulphate of lime thus formed and evaporate
the lye.
The residue consists of the calcium salt of alphanapthylaminetrisulpho-acid which
can be used as aftermentioned, without further purification.
Of course the trisulpho acid can also be obtained by the action of other
sulphonating agents on Alphanapthylaminesulpho acid, for example by the action
of sulphuric acid monochlorhydrine or of pure sulphuric acid (H, SO) in presence
of dehydrating agents.
From napthylamine and fuming sulphuric acid only small quantities of trisulpho
acid are formed.
Second step. Production of a yellow colouring matter from Alphanapthylamine-
trisulpho acid.
The conversion of the trisulpho acid into the yellow colouring matter can be
effected in various ways.
Thus by the action of nitrous acid on the trisulpho acid the yellow colouring
matter is at once formed.
The following process is found to be the most suitable.
I dissolve, in a spacious vessel, ten parts of Alphanapthylaminetrisulphonate of
lime, three or four parts of nitrite of soda, and six parts of Chili salpetre in thirty
parts of boiling water, and then add to this solution, a boiling mixture of eight
parts of English sulphuric acid, and eight parts of water.-As soon as the strong
evolution of nitrogen which takes place accompanied by the developement of a
reddish yellow colouration has ceased, I neutralize with potash.-A thick yellowish
brown paste of the potassium salt of the yellow colouring matter is thus formed,
which is afterwards pressed and recrystallized.
By double decomposition of the potassium salt by sulphate of soda, I obtain
finally the natrium salt of the yellow colouring matter.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by Mrs. Joan Thomson or Dixon of Glasgow in the County of Lanark, North
Britain Executrix of Joseph Anthony Dixon late of 151 St. Vincent Street,
Glasgow aforesaid, Solicitor, deceased in the Great Seal Patent Office on the
6th November 1882.
"
Mrs. JOAN THOMSON or DIXON, of Glasgow, in the County of Lanark, North
Britain, Executrix of Joseph Anthony Dixon late of 151 St. Vincent Street,
Glasgow, aforesaid, Solicitor, deceased. IMPROVEMENTS IN THE PRODUCTION OF
COLOURING MATTERS SUITABLE FOR DYEING AND PRINTING," the said Invention
being a communication from abroad by the Farbwerke Vorm: Meister Lucius and
Brüning, a Company carrying on business as Chemical Manufacturers at Hochst-
am-Main, in the Empire of Germany,
The nature and object of this Invention is the production of Alpha-Napthyl-
amine-Trisulpho acid and the further production of a yellow dyestuff therefrom.
The process hereinafter described for the production of the said yellow dyestuff
is founded on the simultaneous action of nitrates and nitrites in acid solution, on
the said Napthylamine-trisulpho acid.
The production of the said trisulpho acid of Alpha-napthylamine (till now
unknown) shall be first described and then the process for the conversion of this
trisulpho acid into the said yellow colouring matter, shall be given.
First Step. Production of the Alphanapthylamine trisulpho acid.
It is advantageous for the production of the said trisulpho acid of Alpha-
napthylamine, first to convert the napthylanine into its mono-sulpho acid and then
to sulphonate this acid further.
One part of the difficultly soluble alphanapthylamine-monosulpho acid is added
to three or four parts of fuming sulphuric acid (40%, SO,),-Keeping the mixture
cool by means of cold water, and this mixture is slowly heated to 248° Fahrenheit
(120° Centigrade) at which temperature the heating is continued for from 6 to 10
hours.
The product of the sulphonization is then poured into cold water, the liquid
neutralized with lime water, the Sulphate of Lime thus formed is removed and the
lye evaporated.
The residue consists of the calcium salt of Alphanapthylaminetrisulpho acid
which can be used as aftermentioned without further purification.
Of course the trisulpho acid can also be obtained by the action of other
sulphonating Agents on Alphanapthylaminesulpho acid, for example by the action
of sulphuric acid monochlorhydrene, or of pure sulphuric acid (H, SO₁) in presence
of dehydrating Agents.
From Napthylamine and fuming sulphuric acid, only small quantities of trisulpho
acid are formed.
Second Step. Production of a yellow colouring matter from Alphanapthylamine-
trisulpho Acid.
The conversion of the trisulpho acid into the yellow colouring matter can be
effected in various ways.
Thus by the action of nitrous acid on the trisulpho acid the yellow colouring
matter is at once formed.
The following process is found to be the most suitable.
There is dissolved in a spacious vessel, ten parts of Alphanapthylaminetri.
sulphonate of lime, three or four parts of nitrate of soda, and six parts of Chili
saltpetre in thirty parts of boiling water, and then add to this solution a boiling

page_text: As
mixture of eight parts of English sulphuric Acid, and eight parts of water.
soon as the strong evolution of nitrogen which takes place, accompanied by the
developement of a reddish yellow colouration has ceased, it is neutralized with
potash. A thick yellowish brown paste of the potassium salt of the yellow
colouring matter is thus formed which is afterwards pressed and recrystallized.
By double decomposition of the potassium salt by sulphate of soda the natrium
salt of the yellow colouring matter is finally obtained
Having now described and particularly ascertained the nature of the said
Invention and the system, mode or manner in or under which the same is or may
be used or practically carried into effect, it is to be observed in conclusion that
what is considered to be novel and original and therefore claimed as the Invention
secured by the hereinbefore in part recited Letters Patent is-
First. The production, in manner herein before described or in manner sub-
stantially the same, of the Alphanapthylamine-trisulpho acid from the alpha-
naptlylamine.
Second. The production, in manner hereinbefore described or in manner
substantially the same of a yellow colouring matter from Alphanapthylamine-
trisulpho acid.
:
In witness whereof I the said Mrs. Joan Thomson or Dixon have hereunto
set my hand and seal this second day of November in the year of Our
Lord One thousand eight hundred and eighty two.