Improvements in or relating to the Manufacture of Sodium or Potassium.
Year: 1888

page_text: Date of Application, 31st Mar., 1888
Complete Specification Left, 31st Dec., 1889
Complete Specification Accepted 5th, Feb., 1889
Improvements in or relating to the Manufacture of Sodium or
Potassium.
I, GEORGE ARTHUR JARVIS of Eyton Cottage, St. Georges, near Wellington,
Salop, Metallurgical Chemist, do hereby declare the nature of this invention to be as
follows
Heretofore sodium and potassium have been manufactured by intimately mixing
the carbonates of the alkalies with an excess of charcoal and submitting the mixture to
a high temperature in iron cylinders or retorts, the alkali metal being thereby reduced
and distilled and then condensed in appropriate receivers
The required heat to perform the reduction and to distil the metal is very high,.
consequently the iron cylinders or retorts are soon rendered worthless. Also by this
mode of manufacture it has been found that to attain any practical result the charcoal
or carbon in the mixture must be largely in excess of the amount required
theoretically to perform the reduction, owing to the fact that the mixture must be
kept from fusing, to prevent the separation of the charcoal and alkali, and also to
prevent the otherwise inevitable choking of tube of retort with alkali mixture,
which would be the case if fluid; although this might be prevented by the use of
larger retorts with relatively less quantity of alkali mixture.
A certain process is also mentioned in scientific works by which the alkali metals
are produced by decomposing the hydrates of the alkalies with iron borings at a
white heat in iron retorts. This has never received practical application, owing
mostly to the intense heat required to perform the reaction.
The objects of my invention are to reduce the carbonates or other reducible salts of
sodium or potassium without the expense and loss attendant on the use of iron
crucibles or retorts, and also avoiding the employment of a large excess of carbon.
To avoid the expense and waste incurred by the employment of iron crucibles,
cylinders or retorts, I use crucibles, cylinders or retorts made of a refractory basic
material which when fired shall produce a vessel or lining therefor, not readily acted
upon and impervious to melted alkali and the vapour of sodium. Among other

page_text: materials which I have found useful, I may mention magnesia as having proved by
my experiments very applicable.
On the large scale, I prefer using double or compound crucibles, cylinders or
retorts, that is, crucibles, cylinders or retorts, made of fireclay, containing an inner
lining or cylinder composed of magnesian line, magnesia, or a mixture of these with
aluminate of soda or other basic bodies or basic mixtures, and these double or
compound crucibles, cylinders or retorts, may also have sheet iron enclosed between
the outer case of clay and the inner of basic material.
A series of such cylinders or retorts with suitable condensers may be used for the
reduction and distillation of sodium and potassium, arranged in a similar way as gas
retorts for distillation of gas, and to economise fuel, I recommend that regenerative
furnaces be employed for heating the retorts.
To avoid using a large excess of carbon, I use a mixture of tar or pitch and alkali
(by alkali I mean either caustic or carbonated alkali) in such proportion that when
coked, the then fixed carbon of the tar or pitch is sufficient for the reduction. This
mixture is coked by heating in suitable vessels or moulds, excluding access of air,
and when cold, the coked mass is broken into small lumps or pieces and charged into
the crucibles or retorts. Or to avoid using any excess of carbon for the reduction of
the alkali, I may make a mixture of small charcoal, coke, coal or other dense form of
carbon, with tar or pitch and coke such mixture in suitable moulds, around bars or
tubes of iron. When coked and stripped of moulds, I have then dense and heavy
rods of carbon with which to perform the reduction of the alkali, and these carbon
rods are placed in the basic retorts containing the alkali to be reduced. Similarly
these carbon rods can be used for the reduction of alkali in iron cylinders or retorts.
The tubes or inner basic linings are made best with hard burnt magnesia, to which
may be added fluorspar, and finely ground magnesia with oxide of iron answers very
well.
I find the carbonatos of the alkalies are far easier and quicker to reduce than the
hydrates, and by using basic cylinders or retorts, it can be so arranged that they can
be worked continuously, especially when bars or spiral rods of carbon are used for the
reduction.
The manufacture of the carbon rods above described can be varied in detail, thus
instead of coking the carbonaceous mixture around rods, if desired, I coke them in
moulds fitted with spiral iron rods, in this case, the iron would be partly visible and
outside the bulk of the carbon, also if thought desirable, I can still further increase
the density of these rods by soaking in tar and coking, repeating these operations as
often as desired.
Instead of using fireclay cylinders or crucibles lined with basic materials, I may
use the ordinary iron cylinders, but in such case surround them with fireclay or other
refractory material and to increase the heat conductivity and to decrease oxidation of
the iron, I surround the iron inside the refractory material with a coating of a saline
or other suitable fusible material. When the apparatus is heated and employed for
the reduction of alkali, the fused salt will-lessen the oxidization of the iron.¨¨
בד
11
201
.
1
1000
W. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool,
Patent Agents for the Applicant.

page_text: COMPLETE SPECIFICATION.
Improvements in or relating to the Manufacture of Sodium or
Potassium.
I, GEORGE ARTHUR JARVIS of Eyton Cottage, St. George's near Wellington,
Salop, Metallurgical Chemist, 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 :-
The objects of my invention are to reduce the carbonates or other reducible
salts of sodium or potassiumi, without the expense and loss attendant on the .
use of iron crucibles or retorts, and also, avoiding the employment of a large
excess of carbon.
To avoid the expense and waste incurred by the employment of iron crucibles,
cylinders or retorts, I use crucibles, cylinders or retorts made of a refractory
basic material, which when fired shall produce a vessel or lining therefor, not
readily acted upon, and impervious to melted alkali and the vapour of sodium.
Among other materials which I have found useful, may mention magnesia as
having proved by my experiments very applicable. That made from very strongly
burnt magnesite being most suitable as being very dense
On the large scale, I prefer using double or compound crucibles, cylinders or
retorts; that is, crucibles, cylinders, or retorts made of fireclay, containing an
inner lining or cylinder composed of magnesian lime, or magnesia, or a mixture of
either of these with aluminate of soda, or other basic bodies or mixtures, and these
double or compound crucibles, or retorts, may also have sheet iron enclosed between
the outer case of clay and the inner of basic material.
The tubes or inner basic linings are made best with magnesia from hard burnt
magnesite, with an addition of about 10 per cent. of Fluor spar and to obtain this
mixture in the best possible form, moulded bricks of moistened mixture are made
and burnt. These when finely ground and moistened, ram up well into tubes or
linings and when burnt are similar in substance to Parian.
Instead of a 10 per cent. addition of Fluor spar to the hard burnt magnesite,
8 per cent. oxide of iron addition may be used, and for moistening the mixture
a 1 or 2 per cent. solution of sugar or aluminate of soda may be used to
facilitate the ramming or moulding of the mixture. It is essential that the
mixture should be of requisite fineness and smoothness, to produce when burnt, a
non-porous and non-absorptive tube or lining.
After burning there is a certain amount of shrinkage, so that the mixture.
should be rammed or moulded inside the fireclay crucible, cylinder or retort, they
being previously dried and, if of some size, slightly baked, so that when rammed
with the basic mixture and burnt, they should be practically one. If the fireclay
crucibles, cylinders or retorts be made very symmetrical, the basic tubes or linings may
be inserted after each has been burnt.
A series of such cylinders or retorts with suitable condensers may be used for
the reduction and distillation of sodium or potassium, arranged in a similar way,
as gas retorts for distillation of gas, and I recommend that regenerative furnaces
be employed in order to economise fuel.
To avoid using a large excess of carbon for. the reduction of the alkali, I make a
mixture of small charcoal, coke, coal, or other dense form of carbon with tar or pitch,

page_text: and I coke such mixture in suitable moulds around bars or tubes of iron. When
coked and stripped of moulds, 1 have then dense and heavy rods of carbon with
which to perform the reduction of the alkali, and these carbon rods are placed in the
basic retorts containing the alkali to be reduced. Similarly theso carbon rods can be
used for the reduction of the alkali in iron cylinders or retorts.
I find the carbonates of the alkalies are far more easily and quickly reduced than
the hydrates, and by using a series of basic cylinders or retorts, it can be so arranged
that they may be worked continuously.
The manufacture of the carbon rods above described, can be varied in details, thus
instead of coking the carbonaceous mixture around iron rods, if desired, I coke them
in moulds fitted with spiral iron rods, in this case the iron would be partly visible,
and outside the bulk of the carbon, and also if thought desirable, I can still further
increase the density of these rods by soaking in tar and coking, repeating these
operations as often as desired.
For the continuous reduction of the alkali, the cylinders must be curved or hent, so
that when the melted alkali reaches above a certain point in or about the middle of the
cylinder, it is so to speak, trapped, one end being left open for the introduction of
alkali and reducing agent, the other end being used for distillation, and connected
with the condensers. It is advisable to have the iron cores of carbon rods lengthened
and also bent to correspond with curve or bend, so that when introduced through the
open or charging end of cylinder the carbon is immersed in the farther portion of the
melted alkali, and the lengthened iron end projects beyond surface of melted alkali
contained in the nearer or charging end, and the iron rod is withdrawn when it is seen
that the carbon is consumed off the end.
When crucibles are used, the covers must be provided with tubes dipping a little
below the melted alkali to be reduced, such tubes being utilised for the addition of
alkali and for the insertion of the carbon rods, which, in this case, will be straight
ones, and may or may not have lengthened iron ends projecting above the tops of the
tubes, fitted into the covers of the crucibles.
The tubes and covers of such crucibles would be naturally made of iron, but
for continuous work as described, the bent cylinders and the crucibles may be of
wrought iron or steel.
Instead of using fireclay cylinders or crucibles lined with basic material, I may use
the ordinary iron cylinders, but in such case I surround them with salt or other
suitable fusible material, contained in fireclay vessels, loosely fitting the iron cylinders
or retorts. When the apparatus is heated, the fused salt will prevent the external
corrosion or oxidation of the iron almost entirely.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
1. In the manufacture of sodium or potassium by reducing the carbonate or hydrate
by means of carbon, the use or employment of basic, basic lined, or compound
cylinders, crucibles, or retorts, substantially as herein described.
2. In the manufacture of sodium or potassium, the use, as a reducing agent, of
carbon rods, tubes, or pieces constructed substantially as described.
3. In the manufacture of sodinm or potassium, the surrounding of the iron crucibles
or retorts with a fusible medium, such as salt, contained in fireclay vessels, substantially
as herein described.
Dated this 29th day of December 1888.