IMPROVEMENTS IN THE METHOD OF PRODUCING GOLDEN SULPHURET OF ANTIMONY OR PENTA- SULPHIDE OF ANTIMONY
Year: 1883

page_text: LETTERS PATENT to Alfred George Brookes of 59 Chancery Lane, in the
county of Middlesex, Patent Agent. for an Invention of IMPROVEMENTS IN
THE METHOD OF PRODUCING GOLDEN SULPHURET OF ANTIMONY OR PENTA-
SULPHIDE OF ANTIMONY, communicated to him from abroad by Thomas
Sanders of Haverhill in the County of Essex and State of Massachusetts one
of the United States of America
.
PROVISIONAL SPECIFICATION left by the said Alfred George Brookes at
the Office of the Commissioners of Patents on the 2nd August 1883.
ALFRED GEORGE BROOKES of 59. Chancery Lane in the County of Middlesex
Patent Agent IMPROVEMENTS IN THE METHOD OF PRODUCING GOLDEN SULPHURET
OF ANTIMONY OR PENTASULPHIDE OF ANTIMONY. (Communicated to me from
Abroad by Thomas Sanders of Haverhill in the County of Essex and State of
Massachusetts one of the United States of America)
These improvements have reference to the method or art of producing that
chemical compound of antimony and sulphur which is commonly known as the
golden sulphuret of antimony;" but which, in technical nomenclature, is
designated as the "pentasulphide of antimony."
This compound has usually been produced by treatment of the gray sulphide of
antimony or native product known as "antimony glance" either in the crude
condition of the ore or separated by fusion from the gangue with which it is found
associated. Such gray sulphide, when chemically considered apart from impurities,
is the trisulphide of antimony and the pentasulphide has been produced therefrom
in the following mode. among others: The native product, after being pulverized.
is introduced along with a quantity of free sulphur, into a solution of carbonate of
potash or carbonate of soda made caustic by the addition of quick lime and is
boiled therein for several hours until the trisulphido of antimony and free sulphur
so introduced have been dissolved. The solution thus obtained is freed from the
lime and other sedimentary and insoluble substances either by allowing the latter
to subside and drawing off the supernatant fluid or by filtration, and then it is
treated with hydrochloric or sulphuric acid, which precipitates the golden sulphuret
of antimony.

page_text: By this process or any other heretofore known, very considerable proportions of
the antimony and sulphur originally introduced-into the alkaline solution remain
unconverted into the golden sulphuret of antimony, and are consequently wasted;
but by my process, hereinafter described, such waste is substantially prevented, and
much time and labor saved besides.
The solvent which I employ is a saturated solution of caustic soda or of caustic
potash, and I dissolve therein the native sulphide of antimony and the free sulphur
separately and afterward add the two solutions together. Thus: I introduce into a
saturated solution of caustic soda a quantity of pulverized native sulphide of
antimony, and stir or otherwise agitate the same therein until fully dissolved.
I also introduce into another saturated solution of caustic soda a quantity of crude
brimstone or free sulphur in any of its ordinary commercial forms, and dissolve
the same therein by boiling or otherwise applying heat to facilitate the operation.
I allow this sulphur solution to cool and then pour it into the sulphide of antimony
solution and stir the whole mixture to promote chemical reaction, which is attended
with the evolution of considerable heat. When the fluid mass has cooled 1 dilute
it largely with water and so reduce its specific gravity as to readily perinit the
insoluble impurities-such as rock, iron, and other foreign matters to subside.
The aqueous solution is then drawn off, and the golden sulphuret of antimony is
precipitated therefrom by the introduction therein of either sulphuric or hydro-
chloric acid
The proportions of the chemical reagents above mentioned which I have found
best adapted to accomplish the desired results may be stated as follows: For each
pound of pulverized native sulphide of antimony averaging about eighty two
per centum of trisulphide of antimony. I employ eight fluid ounces of saturated
solution of caustic soda, and for every two pounds of free sulphur I employ a
saturated solution of caustic soda containing one pound of anhydrous soda or sodic
oxide Of this sulphur solution I take eight fluid ounces. for mixture with the
trisulphide of antimony solution last above mentioned
I have also found it desirable, in order to attain the best results, that the
trisulphide of antimony should be dissolved in the saturated solution of caustic
alkali at the temperature of about 60° Fahrenheit, and that the sulphur solution
should be cooled down to about the same temperature when it is added to the
antimonial solution.
Caustic potash may be substituted for caustic soda, or may be used in connection
therewith; but the latter, being less expensive, would, for that reason, be preferred.
The proportions of the caustic solvent employed may vary from those hereinabove
specified but any considerable variation therefrom would cause waste of material
and be undesirable on the score of economy.
My process is distinguished from the old processes in several important
particulars The solvent employed is a saturated solution of caustic alkali. The
trisulphide of antimony is dissolved therein not only without boiling but at a cool
temperature
The free sulphur is dissolved before being added to the antimonial solution.
The reactions are such as to convert substantially all of the antimony and sulphur
contained in the mixed solutions into the golden sulphuret of antimony or
pentasulphide of antimony without material waste, and the whole process may be
conducted and completed with in a very short time-say from 15 to 20 minutes or
even less.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Alfred George Brookes in the Patent Office on the 29th January
1884.
ALFRED GEORGE BROOKES of 59, Chancery Lane in the County of Middlesex
Patent Agent IMPROVEMENTS IN THE METHOD OF PRODUCING GOLDEN SULPHURET
OF ANTIMONY OR PENTASULPHIDE OF ANTIMONY (A communication to me from
Abroad by Thomas Sanders of Haverhill in the County of Essex and State of
Massachusetts one of the United States of America)
These improvements have reference to the method or art of producing that
chemical compound of Antimony and Sulphur which is commonly known as tho
golden sulphuret of Antimony" but which in technical nomenclature is designated
as the "pentasulphide of Antimony"
6
This compound has usually been produced by treatment of the gray sulphide of
Antimony or native product known as "Antimony glance" either in the crudo
condition of the ore or separated by fusion from the gangue with which it is found
associated Such gray sulphide when chemically considered apart from impurities,
is the trisulphide of Antimony and the pentasulphide has been produced therefrom
in the following modo among others; The native product, after being pulverized,
is introduced, along with a quantity of free sulphur, into a solution of carbonate of
potash or carbonate of soda made caustic by the addition of quicklime, and is boiled
therein for several hours until the trisulphide of Antimony and free sulphur so
introduced have been dissolved. The solution thus obtained is freed from the
lime and other sedimentary and insoluble substances either by allowing the latter
to subside and drawing off the supernatant fluid or by filtration, and then it is
treated with hydrochloric or sulphuric acid, which precipitates the golden sulphuret
of Antimony. By this process, or any other heretofore known, very considerable
proportion of the Antimony and sulphur originally introduced into the alkaline
solution remain unconverted into the golden sulphuret of antimony, and are
consequently wasted; but by my process; hereinafter described, such waste is
substantially prevented, and much time and labor saved besides. The solvent
which I employ is a saturated solution of caustic soda or of caustic potash, and I
dissolve therein the native sulphide of Antimony and the free sulphur separately,
and afterward add the two solutions together. Thus: I introduce into a saturated
solution of caustic soda a quantity of pulverized native sulphido of antimony, and
stir or otherwise agitate the same therein until fully dissolved. I also introduce
into another saturated solution of caustic soda a quantity of crude brimstone or
free sulphur in any of its ordinary commercial forms, and dissolve the same therein
by boiling or otherwise applying heat to facilitate the operation I allow this
sulphur solution to cool, and then pour it into the sulphide of Antimony solution
and stir the whole mixture to promote chemical reaction, which is attended with
the evolution of considerable heat. When the fluid mass has cooled I dilute it
largely with water and so reduce its specific gravity as to readily permit the
insoluble impurities-such as rock, iron, and other foreign matters to subside. The
aqueous solution is then drawn off and the golden sulphuret of antimony is
precipitated therefrom by the introduction therein of either sulphuric, or hydro-
chloric acid. The proportions of the chemical reagents above mentioned which I
have found best adapted to accomplish the desired results may be stated as
follows: For each pound of pulverized native sulphide of Antimony averaging
about eighty two per centum of trisulphide of Antimony I employ eight fluid
ounces of saturated solution of caustic soda, and for every two pounds of free sulphur

page_text: .
I employ a saturated solution of caustic soda containing one pound of anhydrous
soda or sodic oxide. Of this sulphur solution I take eight fluid ounces for
mixture with the trisulphide of Antimony solution last above mentioned.
I have also found it desirable, in order to attain the best results, that the
trisulphide of Antimony should be dissolved in the saturated solution of caustic
alkuli at the temperature of about 60° Fahrenheit, and that the sulphur solution
should be cooled down to about the same temperature when it is added to the
antimonial solution.
.
Caustic Potash may be substituted for caustic soda, or may be used in connection
therewith; but the latter, being less expensive, would for that reason, be preferred.
The proportions of the caustic solvent employed may vary from those hereinabove
specified but any considerable variation therefrom would cause waste of material
and be undesirable.on.the.score of economy.
My process is distinguished from the old processes in several important
particulars The solvent employed is a saturated solution of caustic alkali. The
trisulphide of Antimony is dissolved therein not only without boiling but at a cool
temperature. The free sulphur is dissolved before being added to the antimonial
solution.
The reactions are such as to convert substantially all of the antimony and sulphur
contained in the mixed solutions into the golden sulphuret of Antimony or
pentasulphide of Antimony without material waste, and the whole process may be
conducted and completed within a very short time-say from fifteen to twenty
minutes or even less.
Having thus described the said Invention and means I adopt in carrying the
same into practical effect I would have it understood that what I claim is
The improved process of producing golden sulphuret of Antimony by dissolving
native sulphide of Antimony_and_free_sulphur_separately_in_saturated solutions of
Caustic Alkali, and afterward adding the same together and heating the mixture
with acid, substantially as described.
In witness whereof I the said Alfred George Brookes have hereunto set my
hand and seal this twenty ninth day of January in the year of our Lord One
thousand eight hundred and eighty four.
ALFRED CFORCE BROOKES (TO)