IMPROVEMENTS IN THE PREPARATION OF HYDRATED OXIDE OF IRON, AND THE APPLICATION OF SUCH PREPARED OXIDE FOR THE ABSORPTION OR SEPARATION OF SULPHUR FROM CERTAIN GASES."
Year: 1861

page_text: LETTERS PATENT to Jacob Geoghegan Willans, of 2, Clarence Place,
Belfast, for the Invention of "IMPROVEMENTS IN THE PREPARATION OF
HYDRATED OXIDE OF IRON, AND THE APPLICATION OF SUCH PREPARED OXIDE
FOR THE ABSORPTION OR SEPARATION OF SULPHUR FROM CERTAIN GASES."
PROVISIONAL SPECIFICATION left by the said Jacob Geoghegan Willans
at the Office of the Commissioners of Patents, with his Petition, on the
27th March 1861.
I, JACOB GEOGHEGAN WILLANS, of 2, Clarence Place, Belfast, do hereby
declare the nature of the Invention for "IMPROVEMENTS IN THE PREPARATION OF
HYDRATED OXIDE OF IRON, AND THE APPLICATION OF SUCH PREPARED OXIDE FOR
THE ABSORPTION OR SEPARATION OF SULPHUR FROM CERTAIN GASES," to be as
follows:-
My Invention relates to the preparation of hydrated oxide of iron from such
iron ores as are hydrated oxides by crushing or grinding the ores and separating
the fine particles from the coarser by means of water or other fluid, or by a
current of air or other gaseous matter, or by such apparatus as is commonly
used for sifting wheaten flour.
My Invention also consists in employing the oxide so prepared for the
purification of coal gas from sulphur, or for absorbing or collecting sulphur
from sulphuretted hydrogen gas given off from substances containing sulphur
whilst undergoing decomposition or chemical action.

page_text: My Invention further relates to the preparation or manufacture of oxide
which will be hydrated from ores of iron containing oxygen which are not
hydrated oxides, or from ores of iron containing hydrated oxide, also from
materials rich in iron, such as burnt pyrites, wherever obtained, or cinder
produced at iron works or smelting works, or hammer slag or similar scaly
particles formed during the process of hammering or rolling iron or steel.
This is effected by acting upon any of the above at or above a red heat, with
carbon or other deoxidizing agent, afterwards exposing the same to the
influence of air and moisture, or other oxidizing and hydrating influences.
The Invention also consists in employing the hydrated oxides so obtained
for the same purposes to which I apply the natural hydrated oxide, as above
stated.
The hydrated oxides prepared as above, and which may be so applied, may
be revived after use in like manner as is usual at gasworks with bydrated
oxide, if so desired.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Jacob Geoghegan Willans in the Great Seal Patent Office
on the 27th September 1861.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JACOB
GEOGHEGAN WILLANS, of 2, Clarence Place, Belfast, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-seventh day of March, in the year of our Lord
One thousand eight hundred and sixty-one, in the twenty-fourth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me, the said
Jacob Geoghegan Willans, Her special licence that I, the said Jacob Geoghegan
Willans, my executors, administrators, and assigns, or such others as I, the
said Jacob Geoghegan , my executors, administrators, and 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
"IMPROVEMENTS IN THE PREPARATION OF HYDRATED OXIDE OF IRON, AND THE
APPLICATION OF SUCH PREPARED OXIDE FOR THE ABSORPTION OR SEPARATION OF
SULPHUR FROM CERTAIN GASES," upon the condition (amongst others) that
I, the said Jacob Geoghegan Willans, my executors or administrators,
by an instrument in writing under my, or their, or one of their hands

page_text: and seals, 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 Jacob Geoghegan Willans, do hereby
declare the nature of my said Invention, and in what manner the same is to be
performed, to be particularly described and ascertained in and by the following
statement thereof, that is to say:-
The first part of my Invention relates to the means of bringing ores of iron
which are hydrated oxide ores, and raised in a lumpy or gravelly state, such
as many kinds of brown hematite bog iron and others of the goethite and
limonite species, that contain hydrated oxide in large proportions, to a fine
state of division; and I would here remark that I am sometime aware that
natural fine soft yellow hydrated oxide ore has been used for the absorption of
sulphur from gas, but I have since discovered that the more abundant and
harder brownish ores above alluded to may be utilized with equal or greater
advantage, provided they be prepared as follows:-My manner of treating
the said hydrated oxide iron ores is by crushing or grinding them by mill-
stones or other mechanical means, and then separating the fine particles from
the coarser by means of water, currents of air, or by such apparatus as used
for sifting flour commonly called bolting machinery; and the said fine particles
may be used for the absorption or separation of sulphur from coal gas or
from sulphuretted hydrogen gas which may be given off from alkaline, metallic,
or earthy substances containing sulphur whilst undergoing decomposition or
chemical action. When performing the grinding for separation by means
of water, I prefer to use a flint mill, in like manner as flints are ground with
water for pottery, or a metal pan with edge runners, as frequently used for
grinding or tempering mortar, and to float off the fine particles from the
coarser by water into one or more vats, which, when settled to the bottom, may
be collected and dried for use by drawing off the water above it, and placing
the wet pulpy or slimy mass upon a heated flue, or by other convenient drying
means, as ground chalk is prepared for whiting. I prefer also that the
material be so finely ground as not to feel gritty when tested between the
fingers. Any coarser quality which might come over with the water I prefer
to have reground.
When grinding for separation by air or by bolting machinery, I prefer
that French burr millstones be used, the ore being first thoroughly dried, and
either to pass the ground material through a bolting machine in the usual

page_text: manner, the meshes of which sieve may be from 1,500 to 2,000 per square
inch, or to let the ground material as it comes from the millstones fall into
a chamber before a strong current of air or other gaseous matter supplied
by a blowing machine or available in any other way, whereby the fine particles
will be driven to a greater distance than the coarser, and may be lifted
separately; those that feel sandy when rubbed in the hand to be reground,
or the hydrated oxide ore of iron may be ground in a wet state in a flint or
other mill, and when dried thoroughly sifted by either of the above means.
In order to absorb sulphur from the gases specified by means of any
of the above prepared fine particles of ground oxide, it should be slightly
damped and placed in shallow trays in a purifier, as used in gasworks for
dry lime, through which the coal gas containing sulphur or the sulphuretted
hydrogen gas before stated is to be passed at the necessary pressure, by which
sulphur will be absorbed therefrom.
What I claim as the first part of my Invention is the preparation as herein
described and application of hydrated oxide iron ores in the absorbing or
separation of sulphur from gases as herein explained.
The second part of my Invention is that ores of iron containing oxygen,
whether hydrates or such others as commonly used for the production of
iron, also certain irony materials, viz., iron pyrites, mineral which has been
deprived to a great degree of its sulphur, cinder from puddling and other
furnaces at iron works or other melting works which may contain 30 per
cent. or upwards of metallic iron, also the black colored scaly particles separated
from iron and steel during the process of hammering and rolling, may be
deprived of oxygen by a strong heat in contact with carbon or other deoxidizing
agents, and thereby brought more or less to the metallic state, and afterwards
may be converted into a sufficiently hydrated oxide state for the absorption or
separation of sulphur from gas by being exposed to the action of oxygen
and hydrogen.
When treating any of the above I prefer to have them first reduced to a
fine state of division (so as not to feel sandy) in any convenient manner, and
then to mix up intimately therewith a quantity of finely divided carbonaceous
matter sufficient to afford solid carbon or ccke at least equal in weight to the
oxygen contained in the irony materials, which may be ascertained by analysis,
but a slight excess will not be injurious; sawdust or partly dried peat along
with a little tar, being well adapted for the purpose, is to be preferred. The
mixed iron and carbonaceous matter is then to be placed in a retort such as
at gasworks, and kept at a bright red heat for such length of time without
access of air as to bring the iron particles to the metallic state, but not to a

page_text: fused state, which will depend upon the size of the retorts, but generally
3 to 5 hours' time will be ample, after which the material is to be withdrawn
as rapidly and with as little access of air as possible into water placed under
neath the mouth of the retort, and then removed therefrom to be exposed in
a moist state in a heap about 18 inches deep for three or more weeks to the
action of the atmosphere, care being taken to turn it over with the shovel
daily, so as to expose fresh surfaces to the air, and sprinkling water thereon in
case of its becoming dry, when it will be found of a rust color, and applicable
for use in a purifier or other convenient apparatus. For the absorption of
sulphur from sulphuretted bydrogen which may be given off from alkaline,
metallic, or earthy substances containing sulphur whilst undergoing decompo-
sition or chemical action, such as the action of carbonic or other acids upon
sulphuret of sodium, and for the purification of coal gas from sulphur, instead
of reoxidizing by exposure to air alone, weak acids or chemical solutions
which have a rusting tendency on iron may likewise be applied.
I would remark that I am aware that other artificially prepared hydrated
oxides of iron have before been used for separating sulphur from some gases,
I do not therefore claim the use of artificially prepared hydrated oxide of iron
generally; but I do claim, secondly, the preparation and application of hydrated
oxide of iron from the materials herein described by first depriving them of
oxygen, and afterwards reoxidizing and hydrating the same, and absorbing or
collecting thereby sulphur from the gases herein described.
In witness whereof, I, the said Jacob Geoghegan Willans, have here-
unto set my hand and seal, this Twenty-sixth day of September, in
the year of our Lord One thousand eight hundred and sixty-one.
J. G. WILLANS. (L.S.)