A NEW OR IMPROVED DRY PROCESS OF OXIDISING ANTHRACENE', AND IMPROVE- MENTS IN THE MANUFACTURE OF DYES AND OTHER COLOURING MATTERS FROM THE PRODUCT SO OBTAINED
Year: 1874

page_text: LETTERS PATENT to Carl Rumpff, of New York, in the State of New
York, United States of America, but at present residing in Glasgow,
in the County of Lanark, North Britain, for the Invention of "A
NEW OR IMPROVED DRY PROCESS OF OXIDISING ANTHRACENE', AND IMPROVE-
MENTS IN THE MANUFACTURE OF DYES AND OTHER COLOURING MATTERS FROM
THE PRODUCT SO OBTAINED."-Partly a communication from abroad by
Friedrich Bayer, Freidrich Weskott, and August Siller, all of
Barmen, Rhenish Prussia.
PROVISIONAL SPECIFICATION left by the said Carl Rumpff at the
Office of the Commissioners of Patents, with his Petition, on the
15th June 1874.
I, CARL RUMPFF, of New York, in the State of New York, United
5 States of America, but at present residing in Glasgow, in the County
of Lanark, North Britain, do hereby declare the nature of the said
Invention of "A NEW OR IMPROVED DRY PROCESS OF OXIDISING 'ANthracene,'

page_text: AND IMPROVEMENTS IN THE MANUFACTURE OF DYES AND OTHER COLOURING MATTERS
FROM THE PRODUCT SO OBTAINED," partly my own Invention and partly
a communication to me from abroad by Friedrich Bayer, Friedrich
Weskott, and August Siller, all of Barmen, Rhenish Prussia, to be as
follows, that is to say:-
This Invention, which relates to a new and improved dry process of
oxidising "anthracene," and also to improvements in the manufacture
of dyes and other colouring matters suitable for dyeing and printing
from the "anthraquinone" thereby obtained, consists as regards the
process of oxidising anthracene in heating the anthracene with peroxide
of manganese, whereby the oxygen becomes free and is taken up by the
anthracene, thereby converting the same into anthraquinone, which at
the same time by this process sublimes in yellow crystals, and this
without the employment of acid. The anthracene and peroxide of
mangnnese may be heated together in a closed vessel in various pro-
portions. Good proportions to employ are from 4 to 5 parts of peroxide
of manganese to 1 part of pure anthracene, but it is to be understood
that I do not confine myself to these proportions.
6
The anthraquinone obtained as herein-before described is heated with
strong fuming oil of vitriol (Nordhausen acid) until it is entirely
dissolved, anthraquinone bi-sulphuric acid {C₁, H 6 O₂2 (So 3 H)} being
thereby formed. This acid is then neutralized with slaked lime or chalk,
and the anthraquinone bisulphate of lime {C₁4 H₁ O₂² (So, Ca)} is
extracted by boiling it repeatedly with water. The solution of the
above-named lime salt is then mixed with carbonate of soda (Na O.
CO₂), and anthraquinone bisulphate of soda {С₁ H 6 O₂2 (So, Na)} is
obtained together with insoluble carbonate of lime, which is separated by
subsidence and filtration. The pure solution of anthraquinone bisulphate
of soda is evaporated with addition of caustic soda (Ná O H), and the
dry mass is fused until by dissolving a portion thereof in water a blue
violet colour is shewn, at which point the anthraquinone bisulphate of
soda has been formed into alezarate of soda {C14 H6. Na, O4)}. By
dissolving this product in water and adding any acid to the solution
alezarine is obtained, which by pressure and washing is purified, and so
rendered fit for dying and printing purposes.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Carl Rumpff in the Great Seal Patent Office on
the 4th December 1874.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, CARL
RUMPFF, of New York, in the State of New York, United States of
America, but at present residing in Glasgow, in the County of Lanark,
North Britain, send greeting.
Majesty Queen Victoria, by Her
Fifteenth day of June, in the
WHEREAS Her most Excellent
Letters Patent, bearing date the
year of our Lord One thousand eight hundred and seventy-four, in
the 37th year of Her reign, did, for Herself, Her heirs and suc-
cessors, give and grant unto me, the said Carl Rumpff, Her
special license that I, the said Carl Rumpff, my executors, adminis-
trators, and assigns, or such others as I, the said Carl Rumpff, my
exccutors, administrators, or assigns, should at any time agree with,
and no others, from time to time and at all times thereafter during
the term therein expressed, should and lawfully might make, use,
exercise, and vend, within the United Kingdom of Great Britain and
Ireland, the Channel Islands, and Isle of Man, an Invention for "A
NEW OR IMPROVED DRY PROCESS OF OXIDISING 'ANTHRACENE,' AND IMPROVEMENTS
IN THE MANUFACTURE OF DYES AND OTHER COLOURING MATTERS FROM THE PRODUCT
SO OBTAINED," partly my own Invention and partly a communication to
me from Friedrich Bayer, Friedrich Weskott, and August Siller, all of
Barmen, Rhenish Prussia, upon the condition (amongst others) that I,
the said Carl Rumpff, by an instrument in writing under my hand and
seal, should particularly describe and ascertain the nature of the
said Invention, and in what manner the same was to be performed, and
cause the same to be filed in the Great Seal Patent Office within six
calendar months next and immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said Carl Rumpff, do hereby declare
the nature of the said Invention and in what manner the come in to ho

page_text: oxidising
anthracene.'
The Invention consists in heating the anthracene with peroxide of
manganese, whereby the oxygen becomes free and is taken up by the
anthracene, thereby converting the same into anthraquinone, which at
the same time by this process sublimes in yellow crystals, and this
without the employment of acid. The anthracene and peroxide of
manganese may be heated together in a closed vessel in various pro-
portions. Good proportions to employ are from 4 to 5 parts of peroxido
of manganese to 1 part of pure anthracene, but it is to be understood
that in practising the Invention it is not confined to these proportions.
0 2
°
The anthraquinone obtained as herein-before described constitutes the
essence of the said Invention, and in order to obtain alizarine therefrom
it may be treated by any of the well-known methods, as for example, by
heating it with strong fuming oil of vitrol. (Nordhausen acid) until it is
entirely dissolved, anthraquinone bi-sulphuric acid (C₁ H, O. (So, H),}
being thereby formed. This acid is then neutralized with slaked lime or
chalk, and the anthraquinone bisulphate of lime {C₁ H₁ O₂ (So, Ca),}
is extracted by boiling it repeatedly with water. The solution of the
above-named lime salt is then mixed with carbonate of soda {Na OCO,},
and anthraquinone bisulphate of soda {C₁, H, O₂ (So, Na),} is obtained
together with insoluble carbonate of lime, which is separated by sub-
sidence and filtration. The pure solution of anthraquinone bisulphate
of soda is evaporated with addition of caustic soda (Na O H), and the
dry mass is fused until by dissolving a portion thereof in water a blue
violet colour is shewn, at which point the anthraquinone bisulphate of
soda has been formed into alizarate of soda {C₁ H₁ Na, O₁}. By
dissolving this product in water and adding any acid to the solution
alizarine is obtained, which by pressure and washing is purified, and so
rendered fit for dyeing and printing purposes.
14
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, I would
observe in conclusion that what I consider to be novel and original, and
therefore claim as the Invention secured to me by the herein-before in

page_text: part recited Letters Patent is, obtaining anthraquinone by the dry
process of oxidising anthracene, substantially as herein-before described.
In witness whereof, I, the said Carl Rumpff, have hereunto set my
hand and seal, this Thirtieth day of November, One thousand
eight hundred and seventy-four.