MAUVEMENTS IN THE PRODUCTION OF POTASSIUM, SODIUM, AND ZINC
Year: 1869

page_text: LETTERS PATENT to Henry Larkin, of No, 6, Torriano Cottages,
Leighton Road, and William White, of No. 30, Thurlow Road,
Hampstead, both in the County of Middlesex, for the Invention of
MAUVEMENTS IN THE PRODUCTION OF
POTASSIUM, SODIUM, AND ZINC.
PROVISIONAL SPECIFICATION left by the said Henry Larkin and
William White at the Office of the Commissioners of Patents, with
their Petition, on the 3rd December 1869.
We, HENRY LARKIN, of No. 6, Torriano Cottages, Leighton Road,
and WILLIAM WHITE, of No. 30, Thurlow Road, Hampstead, both in
the County of Middlesex, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN THE PRODUCTION OF POTASSIUM, SODIUM, AND
ZINC," to be as follows:-
Potassium and sodium are usually obtained by the reaction of carbou
on their several carbonates at a high temperature. The dry carbonate,
or in some cases the hydrate of the required metal, is intimately mixed
in proper proportions with powdered coke or coal, sometimes with the

page_text: addition of chalk, and placed in an iron retort; it is then exposed to a
bright red heat approaching to whiteness in a suitable furnace, when the
metal distils off and is collected by a condenser. We greatly facilitate
the bringing of the entire mass to the requisite high heat by previously
adding to the materials employed a proportion of nitrate of the metal to
be obtained. By this addition as soon as any portion of the contents of
the retort becomes heated to redness the nitrate by freely parting with
two-thirds of its oxygen to the heated carbon carries a vivid combustion
into the very centre of the retort, and its entire contents become rapidly
and spontaneously heated. The oxide also which remains from the
nitrate becomes material for a further quantity of metal in addition to
that contained in the carbonate. It is not necessary in all cases to use
the nitrate of the metal to be obtained, although we prefer doing so on
account of the greater purity of the yield. If convenient nitrate of
sodium may be used in producing potassium, or nitrate of potassium in
producing sodium. Any suitable nitrate, as nitrate of calcium, or
chlorate, as chlorate of potassium, or any other suitable material which
freely parts with oxygen at an increase of temperature, such as the
peroxide of manganese, may be thus used for the purpose of facilitating
the reduction of the required metal. The production of zine from the
oxide of zinc, which is a very similar operation to the production of
potassium and of sodium, may also be greatly facilitated by the same
means. We thoroughly mix the ingredients in the form of fine powder
previous to placing them in the retort. In some cases we also work the
mixed powder into a stiff paste with water or other suitable liquid. When
nitrate of calcium or any other highly deliquescent material is used we
dissolve such material in the water previous to adding it to the other
ingredients. This paste is then dried in cakes in a hot oven, and broken
into small lumps ready for the retort. This not only insures an intimate
mingling of the materials, but also, when a large proportion of nitrate or
other oxygenated substance is used, prevents waste of material which
would otherwise arise from its being blown out of the retort as dust
by the rapidity of the combustion. In the production of potassium and
sodium we use cylindrical retorts similar in size and proportions to those
generally employed, or they may be somewhat larger in diameter. The
hinder end of the retort is closed, so as to prevent leakage of the fused
alkali. The front end is made with a flange, to which a cover may be
tiglitly secured by screws or otherwise. In this cover are two apertures,
one level with the top of the inside of the retort, the other with the

page_text: bottom. The upper aperture is for the introduction of a stream of gas,
the lower one for the discharge of the gas and the metal as it distills of.
To the inside of the lower aperture an exit tube is adjoined, which is
carried diagonally through the interior of the retort to its upper surface
and to within about an inch of its interior end. The front of the furnace
consists of an iron plate or plates with circular holes for the reception of
the retorts. Within the furnace and opposite to the holes in the iron
plate plumbago or other refractory cases or jackets of a cylindrical form
are horizontally fixed for the reception and protection of the iron retorts,
which they are made to fit loosely. These cases, like the retorts, should
be closed at their extreme ends. When the furnace fire is sufficiently
kindled and the refractory cases within it have reached a full red heat,
or somewhat higher, the retorts charged with the requisite ingredients
are slipped in through the circular openings in the front, and become at
once acted upon by the full heat from the furnace. In a very short
time by the combined action of the furnace heat and of that generated
by the oxygenated substance employed the entire mass becomes red hot,
while carbonic oxide is rapidly evolved. During this time the exit tube,
which runs diagonally through the interior of the retort, is plugged up at
its further end by means of an iron rod to prevent its becoming clogged
during the first violence of the action, and the carbonic oxide is allowed
to escape through the upper aperture in the front of the retort. As soon,
however, as there are indications that the reduction of the metal is
commencing the lower aperture is opened by withdrawing the iron rod
and plug, and the upper aperture is connected with a gas pipe con-
veniently arranged for the purpose. By turning a stop-cock a stream of
gas, which may consist of hydrogen or ordinary coal gas, is made to pass
through the said upper aperture into the retort, and thence down the
exit tube through the lower aperture before described. To this aperture
a condenser similar to that generally used is attached. By this means
any metallic vapors rising in the retort are at once swept out from the
hottest end of the retort into the condenser, where they are collected,
while the gas escapes through and may be received into any suitable
vessel or holder. By thus using a stream of gas as a carrier of the
metallic vapors the necessity is avoided of raising the vapors to the
great heat hitherto required to give them the propulsive elasticity
essential for their free distillation. In short it is only necessary to
volatilize the metal instead of as hitherto to raise it to its boiling point.
Previous to the gas being thus passed into the retort it is very highly

page_text: heated by being made to pass through a retort or chamber partially
filled with pieces of coke or charcoal kept at a red or even white heat.
Or it may be made at the time of using by dropping oil upon red-hot
coke in a retort arranged for the purpose. When the whole of the
metal is thus distilled off the retort is withdrawn from the refractory
case or jacket in the furnace, and immediately transferred to a similar
chanıber of brickwork or other suitable material, where it is protected
from the air while cooling, and the heat thus given out by it made
available for drying or other useful purposes. As soon as the retort
is withdrawn the furnace is again ready to receive another.
A similar arrangement of exit tube to that already described for
drawing off the metallic vapors from the hottest end of the retort and of
a stream of gas acting as a carrier of metallic vapors is also applicable to
the distillation of zinc, but instead of iron, as in the oases of potassium
and sodium, the exit tubes should be made of clay, such as is usually
employed in the construction of zinc retorts.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Henry Larkin and William White in the Great
Seal Patent Office on the 3rd June 1870.
.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, HENRY
LARKIN, of No. 6, Torriano Cottages, Leighton Road, and WILLIAM
WHITE, of No. 30, Thurlow Road, Hampstead, both in the County of
Middlesex, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Third day of December, in the year
of our Lord One thousand eight hundred and sixty-nine, in the thirty-
third year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto us, the said Henry Larkin and William White, Her
special licence that we, the said Henry Larkin and William White, our
executors, administrators, and assigns, or such others as we, the said
Henry Larkin and William White, our 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

page_text: of Man, an Invention for "IMPROVEMENTS IN THE PRODUCTION OF POTASSIUM,
SODIUM, AND ZINC," upon the condition (amongst others) that we, the
said Henry Larkin and William White, our executors or adminis-
trators, by an instrument in writing under our or their hands and
seals, or under the hand and seal of one of us or them, should particu-
larly 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 we, the said Henry Larkin and William White,
do hereby declare the nature of the said Invention, and in what manner
the same is to be performed, to be particularly described and ascer-
tained in and by the following statement thereof, that is to say:
Potassium and sodium are usually obtained by the reaction of carbon
on their several carbonates at a high temperature. The dry carbonate, or
in some cases the hydrate of the required metal, is intimately mixed in
proper proportions with powdered coke or coal, sometimes with the addition
of chalk and placed in an iron retort. It is then exposed to a bright red
licat approaching to whiteness in a suitable furnace, when the metal distils
off and is collected by a condenser. We greatly facilitate the bringing
of the entire mass to the requisite high heat by previously adding to the
materials employed a proportion of nitrate of the metal to be obtained.
We prefer to add the nitrate in the proportion of about 20 per cent. by
weight of the carbonate contained in the mass. Care should be taken that
the mixture contain a considerable excess of carbon beyond the requisite
combining equivalent. By this addition of nitrate as soon as any portion
of the contents of the retort becomes heated to redness the nitrate by
freely parting with two-thirds of its oxigen to the heated carbon carries
a vivid combustion into the very centre of the retort, and its entire con-
tents become rapidly and spontaneously heated. The oxide also which
remains from the nitrate becomes material for a further quantity of metal
in addition to that contained in the carbonate. It is not necessary in all
cases to use the nitrate of the metal to be obtained, although we prefer
doing so on account of the greater purity of the yield. Nitrate of sodium
may be used in producing potassium, or nitrate of potassium in producing
sodium. Any suitable nitrate, as nitrate of calcium, may be used or a
chlorate as chlorate of potassium may be substituted for nitrate, or any
other suitable material which freely parts with oxygen at an increase

page_text: of temperature, such as the peroxide of manganese may be thus used for
the purpose of facilitating the reduction of the required metal. The pro-
duction of zinc. from the oxide of zinc, which is a very similar operation
to the production of potassium and of sodium may also be greately
facilitated by the same means. In this case we should prefer to employ
the oxide of manganese on account of its cheapness, but other materials
capable of yielding oxygen when exposed to heat might be employed.
We thoroughly mix the ingredients in the form of fine powder previous
to placing them in the retort. In some cases we also work the mixed
powder into a stiff paste with water or other suitable liquid. When
nitrate of calcium or any other highly deliquescent material is used we
dissolve such material in the water previous to adding it to the other in-
gredients. This paste is then dried in cakes in a hot oven and broken
into small lumps ready for the retort. This not only ensures an intimate
mingling of the materials, but also when a large proportion of nitrate or
other oxygenated substance is used prevents waste of material which
would otherwise arise from its being blown out of the retort as dust by
the rapidity of the combustion.
In the production of potassium and sodium we use cylindrical retorts
similar in size and proportions to those generally employed, or they may
be somewhat larger in diameter. The hinder end of the retort is closed.
The front end is made with a flange, to which a cover may be tightly
secured by screws or otherwise. In this cover are two apertures one level
with the top of the inside of the retort, the other with the bottom. The
upper aperture is for the introduction of a stream of gas, the lower one
for the discharge of the gas and the metal as it distils off. To the inside
of the lower aperture an exit tube is adjoined, which is carried diagonally
through the interior of the retort to its upper surface and to within about
an inch of its further end. The front of the furnace consists of an iron
plate or plates with circular holes for the reception of the retorts within
the furnace and opposite to the holes in the iron plate, plumbago or other
refractory cases or jackets of a cylindrical form are horizontally fixed for
the reception and protection of the iron retorts which they are made to
fit loosely. These cases like the retorts should be closed at their extreme
ends. When the furnace fire is sufficiently kindled and the refractory
cases within it have reached a full red heat or somewhat higher the
retorts charged with the requisite ingredients are slipped in through the
circular openings in the front and become at once acted upon by the heat.

page_text: In a very short time by the combined action of the furnace heat and of
that generated by the oxygenated substance employed the entire mass
becomes red hot while carbonic oxide is rapidly evolved. As soon as there
are indications that the reduction of the metal is commencing the upper
aperture is connected with a gas pipe conveniently arranged for the
purpose. By turning a stop cock a stream of gas, which may consist of
hydrogen or ordinary coal gas is made to pass through the said upper
aperture into the retort and thence down the exit tube through the lower
aperture before described. To this aperture a condenser similar to that
generally used is attached. By this means any metallic vapours rising
in the retort are at once swept out from the hottest end of the retort into
the condenser, where they are collected, while the gas escapes through and
may be received into any suitable vessel or holder. By thus using a
stream of gas as a carrier of the metallic vapors the necessity is avoided
of raising the vapours to the great heat hitherto required to give them
the propulsive elasticity essential for their free distillation. In short it
is only necessary to valatilize the metal instead of as hitherto to raise it to
its boiling point. Previous to the gas being thus passed into the retort it
is very highly heated by being made to pass through a retort or chamber
partially filled with pieces of coke or charcoal kept at a red or even white
heat. This may conveniently be effected by heating the retort or
chamber containing the charcoal in the same furnace as the retort in
which the metallic vapors are produced, or the heated gas may be made
at the time of using by dropping oil upon red hot coke in a retort
arranged for the purpose. When the whole of the metal is thus distilled
off the retort is withdrawn from the refractory case or jacket in the
furnace and immediately transferred to a similar case of refractory
material or to a chamber of brickwork or other suitable material, where
it is protected from the air while cooling. As soon as the retort is
withdrawn the furnace is again ready to receive another. A stream of gas
passed through the retort may similarly be employed to carry off the
metallic vapors of potassium and sodium as they are formed, whether
material capable of yielding oxygen be mixed with the materials in the
retort, or whether the process be conducted as heretofore without the
addition of such material. Retorts fitted with a tube passing from the
front to the back of the retort to conduct away the metallic vapors as
they are produced from the hottest end of the retort may also be
employed without at the same time employing the current of heated gas.

page_text: A similar arrangement of exit tube to that already described for
drawing off the metallic vapours from the hottest end of the retort and
of a stream of gas acting as a carrier of the metallic vapours is also
applicable to the distillation of zinc, but instead of iron, as in the cases
of potassium and sodium, the exit tubes should be made of clay such as
is usually employed in the construction of zinc retorts.
Having thus described the nature of our Invention, and the manner
of performing the same, we would have it understood that what we
claim is,―
First. The employment of nitrate of soda or potassium or other suitable
substance capable of yielding oxygen as herein described in the
manufacture of potassium and sodium.
Second. The employment as herein described of an oxygen yielding
substance in the manufacture of zinc..
Third. The employment of a current of gas passed through the retort
to carry off the metallic vapors produced when manufacturing
potassium and sodium, as herein described.
Fourth. The employment in the manufacture of potassium, sodium,
and zinc of a retort fitted with a tube passing from the front towards the
back of the retort to enable the metallic vapors to be drawn off from 2
the hottest end of the retort, as herein described.
In witness whereof, we, the said Henry Larkin and William White,
have hereunto set our hands and seals, this First day of June,
in the year of our Lord One thousand cight hundred and seventy.
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