An Improved Method of Separating Sulphur from Sulphureous Pig Iron.
Year: 1890

page_text: Date of Application, 19th July, 1890
Complete Specification Left, 18th Apr., 1891-Accepted, 27th June, 1891
PROVISIONAL SPECIFICATION.
An Improved Method of Separating Sulphur from Sulphureous
Pig Iron.
We, GUSTAV HILGENSTOCK, Engineer, at Hoerde, Westphalia, Hochofenstrasse 1.
and JOSEPH MASSENEZ, Director trading under the name of the firm of Hoerder
Bergwerks- und Hütten-Verein at Hoerde, Westphalia, Kingdom of Prussia do
hereby declare the nature of this invention to be as follows:-
If common sulphuret of iron (Fe S) containing about 36% of sulphur is melted
with pig iron rich in manganese or if the melted sulphuret of iron is mixed with
liquid manganesian pig-iron, all the sulphur is separated as sulphide of manganese
in the form of slag the resulting product being pig-iron free from sulphur.
The same result is obtained by mixing liquid pig-iron, rich in sulphur, with
molten manganesian iron at a temperature above that at which the iron melts
(heisflüssig). Experience has shown that the iron so treated does not contain more
of sulphur.
The sulphide of manganese slag thus separated contains 20% or more of sulphur
and 50% or more of manganese.
If again the slag consisting of sulphide of, manganese in addition to earth bases,
such as limestone or the like, is submitted to a reducing melting operation,
manganesian iron will be obtained which may be employed a second time for
the elimination of sulphur.
In separating the sulphur from the iron as sulphide of manganese, it is necessary
that the bath remain liquid long enough and that, if necessary, it should be heated
by special appliances in order to accomplish the complete separation of the sulphide
of manganese.
The method is as follows:
-
The sulphureous pig-iron, either taken directly from the blast furnace or remelted
is mixed in a special vessel with as much refractory (heissflüssig) manganesian iron
as corresponds to the sulphur existing in the bath.
The
The quantity of manganesian iron to be used must conform to the degree of
desulphurization required and must be determined for each particular case.
vessel which I prefer to use constitutes a kind of Bessemer converter without
nozzles in the bottom. The liquid sulphureous pig-iron and the molten manganesian
iron is introduced into the previously heated vessel.
After a certain time the sulphide of manganese separates from the molten mass
and may then be removed as slag. The purified pig-iron is then removed for further
treatment according to requirements.
In order to get a thicker layer of slag and to remove it more easily it is desirable
to effect several operations successively. This is to be recommended for producing
by the repeated pouring in of the molten mass, the stirring or agitating of the bath
and for hastening the separation of the sulphide of manganese. For this purpose
metallic oxides are also added, either at the time of, or after pouring in the metal.
The method is especially applicable for treating sulphureous "Thomas"
pig-iron.
Dated this 19th day of July 1890.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicants.

page_text: COMPLETE SPECIFICATION.
An Improved Method of Separating Sulphur from Sulphureous
Pig Iron.
We, GUSTAV HILGENSTOCK, Engineer, at Hoerde, Westphalia, Hochofenstrasse 1
and JOSEPH MASSENEZ, Director, trading under the name of the firm of Hoerder
Bergwerks und Hütten-Verein at Hoerde, Westphalia, Kingdom of Prussia, 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 :-
If common sulphuret of iron (Fe S) of about 36% sulphur is melted with
pig-iron rich in manganese or if the melted sulphuret of iron is mixed with liquid
manganesian pig-iron, all the sulphur is separated as sulphide of manganese in the
form of slag the resulting product being pig-iron free from sulphur.
The same result is obtained by mixing liquid pig-iron rich in sulphur with molten
manganesian iron at a temperature above that at which the said iron melts
(heissflüssig). Experience has shown that the iron so treated does not contain more
than 0.01% sulphur.
The sulphide of manganese slag thus separated contains 20% or more of sulphur
and 50% or more of manganese.
If again the slag, consisting of sulphide of manganese in addition to earth bases
such as limestone or the like is submitted to a reducing or melting operation,
manganesian iron will be obtained which may be employed a second time for the
elimination of sulphur.
In separating the sulphur from the iron as sulphide of manganese it is necessary
that the bath remains liquid long enough and that, if necessary it should be heated
by special appliances in order to accomplish the complete separation of the sulphide
of manganese.
The method is as follows;
The sulphureous pig-iron either taken directly from the blast furnace, or remelted
is mixed in a special vessel with as much molten maganesian iron as corresponds to
the sulphur existing in the bath.
The quantity of manganesian iron to be used must conform to the degree of
desulphurization required, and must be determined for each particular case.
The vessel which I prefer to use constitutes a kind of Bessemer converter
without nozzles in the bottom. The liquid sulphureous pig-iron and the molten
manganesian iron is introduced into the previously heated vessel.
After a certain time the sulphide of manganese separates from the molten mass
and may then be removed as slag.
In general the desulphurization is effected so much surer and the more complete,
the more manganese is contained in the bath, but even a small quantity of
manganese is sufficient to completely separate the sulphur.
For instance if the vessel contains 60 tons of pig-iron having 0.15% (per cent.)
sulphur and 0.9% manganese a good purification is obtained by adding 10 tons of
manganesian iron having 4.5 % of manganese and 0.02% of sulphur or for a bath
containing 20 tons of pig-iron having 0.3% of sulphur and 0.8% of manganese the
appropriate addition is about 50 tons pig-iron containing 2% of manganese and
0.04% of sulphur, or for a bath of 20 tons of pig-iron containing about 0.5% of
manganese and about 1-2% of sulphur it is convenient to add 50 tons of pig-iron
having 3% of manganese and 0.02 %% of sulphur.
In all these cases the separation of the sulphur is carried so far that the purified
iron contains about 1 % manganese and 0.03 to 0.05% sulphur. The sulphide of
manganese slag having 30 % or more of manganese is mixed with so much lime
stone as corresponds to its contents of silica. This quantity of lime stone is
determined in the known manner. I prefer to melt this mixture together with iron

page_text: ore in a pit furnace and this is more conveniently done in that high furnace which is
to produce the manganesian iron for the desulphurization process. The mixture may
however also be used without iron ore for producing manganesian iron containing
20% or more iron in a pit furnace with coke or by the open hearth process by the
same intimately mixed with coal to form cakes or bricks. The purified pig-iron
is then removed for further treatment according to requirements.
In order to get a thicker layer of slag and to remove it more easily it is desirable
to effect several operations successively. This is to be recommended for producing
by the repeated pouring in of the molten mass, the stirring or agitating of the bath
and for hastening the separation of the sulphide of manganese. For this purpose
metallic oxides are also added either at the time of, or after pouring in the metal.
The method is especially applicable for treating sulphureous
"Thomas'
pig-iron.
"
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 :-
First. The herein described method of separating sulphur from sulphureous
pig-iron by mixing liquid sulphureous pig-iron with molten manganesian iron of
high temperature (hot-molten) and allowing the mixture to stand whereby
sulphide of manganese is formed and caused to separate out in the form of slag
substantially as described.
Second. The method of transforming the slag above mentioned into manganesian
iron by submitting the said slag to a reducing or melting operation in the presence
of earth bases, substantially as described.
Dad sh 101 1.— Ր
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicants.