IMPROVEMENTS IN AND RELATING TO THE DESULPHURATION OF LIQUIDS AND GASES."
Year: 1881

page_text: LETTERS PATENT to Friedrich Lux, of Ludwigshafen-on-the-Rhine, in the
Kingdom of Bavaria and German Empire, for an Invention of "IMPROVEMENTS
IN AND RELATING TO THE DESULPHURATION OF LIQUIDS AND GASES."
PROVISIONAL SPECIFICATION left by the said Friedrich Lux at the Offico
of the Commissioners of Patents on the 14th June 1881.
FRIEDRICH LUX, of Ludwigshafen-on-the-Rhine, in the Kingdom of Bavaria and
German Empire.
"IMPROVEMENTS IN AND RELATING TO THE DESULPHURATION
OF LIQUIDS AND GASES."
Hitherto native sesquioxide of iron and hydrated peroxide of iron have been
applied for the desulphuration of liquids and gases, especially in the desulphuration
of illuminating gasses. These chemical substances are however defective in their
operation, inasmuch as at the beginning of the desulphurating process their purifying
or desulphurizing qualities do not come into full action, and the results obtained aro
therefore imperfect at the commencement of the operation. They come into full
action by degrees only, after becoming fluxed, and even their full action or effect
when it takes place is not inproportion to the iron they contain.
According to my said Invention, in order to avoid such deficiencies, I make use
of a mass containing in addition to the iron a certain percentage of alkali, and in
this mass the hydrated peroxide of iron is contained in a molecular state, in con-
sequence of fusion and lixiviation.
In carrying the said Invention into practice, I make use of such minerals as
contain hydrated peroxide of iron and hydrate of alumina (like bauxite, for
instance, a mineral found near the City of Baux, in France), and I fuse the said
minerals with carbonate of soda, and lixiviato the fused mass with water. By this
process the alumina is extracted, and the hydrated peroxide of iron will be left in a
state of the finest distribution. The lixiviation is continued until the remaining
hydrated peroxide of iron will contain in an air dried state about five per cent. of
carbonate of soda.

page_text: In the manufacture of alumina preparations (such as sulphate of alumina, alum,
hydrate of alumina and the like) when treating the crude mass in the usual
manner, there remains a residue containing in addition to the hydrated peroxide of
iron, and in addition to the carbonate of soda, other ingredients, such as clay and
sand. This mass would serve for the purpose of my Invention, and it would not
be necessary to elutriate or "wash" the sand before applying the mass for the
desulphurizing process. The said other ingredients would be of no avail in the
purifying process; they would neither delay nor accelerate the same, but the acting
elements which would in this instance consist of about from 60 to 70 per cent. of
hydrated peroxide of iron, and of about 5 per cent. of carbonate of soda, would have
the same desulphurizing qualities as they would have if the mass consisted entirely
of the same.
The main point which must be observed in the practice of my Invention is to
give to the hydrated peroxide of iron (being in a molecular state) an addition of
carbonate of soda, so as to cause it to work energetically from the beginning of the
purifying process.
The mass which I propose to apply for practical use would be composed of about
sixty five (65) per cent. of hydrated peroxide of iron, five (5) per cent. of carbonato
of soda, and about thirty (30) per cent. of clay, sand, and moisture, and this mass
can be obtained best and cheapest in the manufacture of alumina preparations.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by the
said Friedrich Lux in the Great Seal Patent Office on the 13th December 1881.
FRIEDRICH LUX, of Ludwigshafen-on-the-Rhine, in the Kingdom of Bavaria and
German Empire. "IMPROVEMENTS IN AND RELATING TO THE DESULPHURATION
OF LIQUIDS AND GASES."
Heretofore native sesquioxide of iron and hydrated peroxide of iron, or sesquioxido
of manganese and hydrous oxide of manganese, have been used in desulphurating
liquids and gases, especially in desulphurating illuminating gases. These chemical
substances have been found to be deficient in their action, inasmuch as in tho
beginning of the desulphurating process their purifying or desulphurizing qualities
would not come into full action, and the results obtained were imperfect at that
stage of the process. These qualities would come into full action by degrees only,
after the chemical substances had become fluxed, and even their full action would
not be such as to be in proportion to the iron they contained.
The object of my Invention is to overcome the defects heretofore existing, and to
obtain a inore perfect desulphuration of the liquid or gas under treatment at the
beginning of and throughout the entire process, and to this end the said Invention
consists in preparing a desulphurizing agent or mass containing besides the iron or
the manganese, a certain porcentage of alkalies.
The alkalies, as also the carbonates, will instantly absorb the sulphide of hydrogen
contained in the unpurified gas, and deliver it to the iron or manganese. This
process continues when using the material in a molecular condition, until all the
iron or manganese in the desulphurizing compound has been converted into sulphide
of iron or of manganese.
Therefore in desulphurizing gases, and more particularly in desulphurizing
illuminating and heating-gases, I make use of any of the following chemical iron or
manganese-combinations, that is to say, native or artificial protoxide of iron or
sesquioxide of iron, or oxidulated iron, or of the hydrates of the same, or of native
or artificial protoxide of manganesc, or peroxide of manganese, or sesquioxide of
manganese, or of their hydrates, and by combining one or more of the said com-
binations with alkalies, such as potash, natron or ammonia, or with the carbonates
of the same, I produce my improved compound for the desulphurizing purpose
above referred to.
In mixing the said iron or manganese combinations with the alkali, I may
procced as follows, that is to say :-I take the said iron or manganese and reduce
the same in any convenient manner, and then mix it with an aqueous solution of
one or the other of the said alkalies or their carbonates, the mass being stirred
during the mixing process, until it has become dry enough for pulverization. In
order to accelerate the drying of the said mass, I prefer to mix the said chemicals
in a heated room, or in a receptacle hented by means of a stove in any suitable
manner. I prefer to make use of five (5) parts by weight, more or less, of alkalies,
to an hundred (100) parts by weight of the said iron or manganese, but such pro-
portions may be varied without affecting the efficiency of my said desulphurizing mass.
I may also mix the pulverized iron or manganese with the pulverized alkali or
its carbonate in a dry state, and in this instance I do not moisten the mass, or if
moistening be desired the mass should be so moistened as to avoid agglomeration.
I may also take a mixture of the iron or manganese ore, and of alkali, and frit
the same in a calcar or calcining furnace and lixiviate the resulting composition
of fritted mass with water until the lye running off indicates only about 1° Beaumé,
whereupon I interrupt the lixiviation to dry the remaining residue which will then
contain about five per cent. of alkali.
I may also suspend in a solution of alkalies or their carbonates the said protoxide,
sesquioxide, or peroxide of iron or of manganesc, or the hydrates of the same, and
may in this instance effect desulphuration by allowing the gas to bo purified by
passing through or across tho said combined liquid.

page_text: preferably make use of a mass containing hydrated peroxide of iron in a
molecular state in consequence of fusion and lixiviation. In preparing this mass I
use minerals which contain hydrated peroxide of iron and hydrate of alumina (such
as bauxite, for. instance, a mineral found near the City of Baux, in southern France),
and fuse the said mineral with carbonate of soda, and then lixiviate the fused mass
with water. By this process the alumina is extracted and the hydrated peroxide of
iron will be left in a state of the finest molecular division. The lixiviation is
continued until the remaining hydrated peroxide of iron will contain in an air-
dried state about five per cent. (more or less) of carbonate of soda. The quantity of
carbonate of soda applied depends on the hydrate of alumina present, that is to say,
three equivalents of carbonate of soda are used with one equivalent of hydrate
Al 2
of alumina. Al² O₂, 3 H₂O + 3CONAO,. .=
Nn² 6 } 0 6 + 3 H, O + 3 CO̟
This is equivalent to three hundred and eighteen parts by weight of carbonato of
soda being used with one hundred and fifty-six and four tenths parts by weight of
hydrate of alumia contained in bauxite; or approximatively for one part by weight
of hydrate of alumina, two parts by weight of carbonate of soda must be used. The
. lixiviation will be stopped if the solution flowing from the tank or other receptacle
indicates only 1° Beaumé. The mass remaining in the tank will then contain about
five per cent. of carbonate of soda after it has become air-dried.
In the manufacture of preparations of alumina, such as sulphate of alumina,
alum, hydrate of alumina, and the like, there remains, when treating the crude
mass in the usual manner, a residuo containing, besides the hydrated peroxide of
iron and the carbonate of soda, other ingredients, such as clay or sand. This
residue would not interfere with the purpose of my desulphurating mass, and it
would not be necessary to elutriate or wash the sand before using the said mass
for the desulphurizing process, as it would neither retard nor accelerate the same,
and the acting elements which would in this instance consist of about from sixty
to seventy per cent. of hydrated peroxide of iron and about five per cent. of
carbonate of soda would act with the same efficiency in desulphurating liquids or
The main point
gases as when forming the only component parts of the mass.
to be observed is to add to the iron compound which is in a molecular condition,
the proper proportion of carbonate of soda, so that the mass will work onergetically
from the beginning of the purifying process.
The mass which I propose to apply to practical use will be composed of the
before-mentioned ingredients in about the following proportions, that is to say:-
Hydrated peroxide of iron, sixty-five per cent.; carbonate of soda, five per cent. ;
sand, or clay, or moisture, thirty per cent. This mass will be obtained in the best
and cheapest manner in the manufacture of preparations of alumina, and especially
when using bauxite in such manufacture.
Having thus fully described my said Invention and the manner of performing
the same, I wish it understood that I claim,—
In the desulphuration of liquids and gases, more particularly illuminating gas,
the use of native or artificial protoxide of iron, or sequioxide of iron, or oxidulated
'iron, or of protoxide of manganese, or sesquioxide of manganese, or of their hydrates,
all or any of the combined with alkalies or their carbonates, substantially as above
set forth and for the purpose specified.
In witness whereof, I, the said Friedrich Lux, have hereunto set my hand
and seal, this Eighth of December, in the year of our Lord One thousand