The Production or Obtainment of Metallic Beryllium from Minerals containing it.
Year: 1898

page_text: Date of Application, 11th Feb., 1898
Complete Specification Left, 10th Nov., 1898-Accepted, 4th Feb., 1899
PROVISIONAL SPECIFICATION.
The Production or Obtainment of Metallic Beryllium from Minerals
containing it.
I, LOUIS LIEBMANN, Ph. D. and Chemist, of Borkenheimer Anlage 1, Frankfurt-on-
Main, in the Empire of Germany, do hereby declare the nature of this invention to
be as follows:
For many years past I have been engaged with experiments having for their
object the industrial preparation of beryllium, a metal, which, for many technical
purposes, is of considerable value. Previous experiments have resulted in a process
for preparing the metal in the form of alloys, but my present invention has for its
object the industrial production of beryllium in the metallic state.
I have found that fluorine compounds are capable of eliminating silicic acid from
the beryllium minerals occurring in nature, thus exposing the beryllium to
reduction.
For this purpose the reduction of the mineral is carried out in the presence of a
recognised natural compound of fluorine.
The following method may be employed:
Beryllium minerals containing oxygen are reduced to powder, and intimately
mixed with calcium fluoride (fluor-spar) preferably with the addition of a halogen
derivative of an alkali or alkaline earth, to act as a flux, and the mixture is
subjected to electrolysis whilst in the fused state.
Carbon may be used for the electrodes, although under certain circumstances it is
advantageous to employ metals (copper iron &c. or even beryllium).
In the molten electrolyte the calcium fluoride dissolves out the silicic acid from
the beryllium minerals, forming calcium silicate or calcium aluminium silicate,
together with the intermediate product, calcium fluo-silicate, which immediately
undergoes further decomposition according to the equations
-
Al,U. 3 BеU. 4 div₂ + 0 CaFT — Alū¿. ɔ DEU †+ 4 Jak103 + 4 UHDIE 18
and
2 CaSiF=2 CaFl, + 2 SiFl.
The beryllium ore, freed from the silicic acid which it held in combination
undergoes further decomposition by the action of the electric current, the liberated
beryllium being deposited at the cathode, from which it is subsequently removed,
and remelted, whilst the alumina combines with the calcium silicate to form a
readily fusible calc-felspar according to the equation
No text detected.
AV + V&D]V3 — 4 Vav.AlgUg• # Ñ¡V₂
Or the following method may be employed:
To a mixture of fluorine compounds with beryllium minerals containing oxygen
coal (or other reducing agent) is added in sufficient quantity to combine with all
the oxygen and the mass is exposed to a white heat, or to the temperature of the
electric furnace.

page_text: It is advantageous to add halogen compounds of the alkalies or alkaline earths,
to the mixture.
All the silicon of the silicic acid escapes in the form of silicon fluoride. The
oxygen of both the silicic acid and the beryllium ore passes off in combination with
carbon whilst metallic beryllium accumulates in the molten state.
Fluorine compounds act on the alumina in the same way as on the silicon.
Consequently the method described may be applied also to those beryllium minerals,
(such as chrysoberyl) which contain alumina in place of silicon.
Dated this 11th day of Kohmua 1000
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.
The Production or Obtainment of Metallic Beryllium from Minerals
containing it.
I, LOUIS LIEBMANN, Ph. D. and Chemist, of Borkenheimer Anlage 1, Frankfurt-
on-Main, in the Empire of Germany, 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 :-
For many years past I have been engaged with experiments having for their
object the industrial preparation of beryllium, a metal which for many technical
purposes is of considerable value. Previous experiments have resulted in a process
for preparing the metal in the form of alloys but my present invention has for its
object the industrial production of beryllium in the metallic state.
I have found that fluorine compounds are capable of eliminating silicic acid from
the beryllium minerals occurring in nature, thus exposing the beryllium to
reduction.
For this purpose the, reduction of the mineral is carried out in the presence of a
recognised natural compound of fluorine.
The following method may be employed :-
Beryllium minerals containing oxygen are reduced to powder, and intimately
mixed with calcium fluoride (fluor-spar) in the proportion (by weight) of one part
of beryllium to four parts of fluor-spar preferably with the addition of a halogen
derivative of an alkali, or alkaline earth, (say, for instance, common salt, in the.
proportion of one-half part by weight) to act as a flux, and the mixture is subjected'
to electrolysis whilst in the fused state.
Carbon may be used for the electrodes, although it is advantageous to employ
metals (copper, iron, &c., or even beryllium).
In the latter case the beryllium alloy is first formed and this is subsequently
converted into metallic beryllium.
In the molten electrolyte the calcium fluoride dissolves out the silicic acid from
the beryllium minerals, forming calcium silicate, or calcium aluminium silicate,
together with the intermediate product, calcium fluo-silicate, which inmediately
undergoes further decomposition according to the equations.
Dec. 0
DIU₂+0 Carl₂
-
Al2O3. 3 Be0+4 CaSiO, +2 CaSiF!,
Dev. O
והייoc.o
==
Al2O3. 3 Be0+4 CaSiO, +2 CaSiFl。
TI
ורים

page_text: beryllium being deposited at the cathode, from which it is subsequently removed,
and remelted, whilst the alumina combines with the calcium silicate to form a
readily fusible calc-felspar according to the equation
A₁₂O₂+4 CaSiO₂ = 4 Ca0. Al,O,+4 SiO„.
3
Or the following method may be employed.
To a mixture of fluorine compounds with beryllium minerals, containing oxygen,
coal, (or other reducing agent), is added in sufficient quantity to combine with all
the oxygen, and the mass is exposed to a white heat, or to the temperature of the
electric furnace.
It is advantageous to add halogen compounds of the alkalies, or alkaline earths,
to the mixture.
All the silicon of the silicic acid escapes in the form of silicon fluoride. The
oxygen of both the silicic acid and the beryllium ore passes off in combination with
carbon whilst metallic beryllium accumulates in the molten state.
Fluorine compounds act on the alumina in the same way as on the silicon.
Consequently the method described may be applied also to those beryllium minerals
(such as chrysoberyl) which contain alumina in place of silicon.
It is evident that other fluorine compounds may be used instead of calcium
fluoride.
When carbon is employed as a reducing medium, beryllium carbide forms in the
first instance. A reaction of this is brought about by adding either pure beryllium
earth, or lime.
At this stage the beryllium earth gives up its oxygen to the car bon of the carbide
and liberates the metal.
Where lime is added calcium carbide will form besides the carbonic oxide gas in
accordance with the following equation.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
1. The obtainment or production of metallic beryllium from minerals containing
it, by reducing the said minerals in the presence of fluorine or a compound of
fluorine, the effect when the electrical current is employed, and metal electrodes are
used being that the beryllium alloy originally forming becomes converted into
metallic beryllium.
2. In a process for the purpose referred to in the first claim subjecting beryllium
mineral in conjunction with fluorine, or a compound of fluorine, and preferably
with the halogen compounds of alkalies and alkaline earths, to the action of
electrolysis.
3. In a process for the purpose referred to in the first claim subjecting a mixture
of beryllium mineral and fluorine compound in the presence of a reducing agent,
preferably with an addition of the halogen compounds of alkalies or alkaline earths,
to a white heat, or to the heat produced by the electrical current, the beryllium
carbide developing, being if necessary decomposed by suitable admixtures.
Dated this 10th day of November 1898.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.